CN107151475A - A kind of powdery paints dry-mixed additive and its powdery paints of offer grain effect - Google Patents
A kind of powdery paints dry-mixed additive and its powdery paints of offer grain effect Download PDFInfo
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- CN107151475A CN107151475A CN201710461439.8A CN201710461439A CN107151475A CN 107151475 A CN107151475 A CN 107151475A CN 201710461439 A CN201710461439 A CN 201710461439A CN 107151475 A CN107151475 A CN 107151475A
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- resin
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- acid
- sulfonic acid
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- 239000000654 additive Substances 0.000 title claims abstract description 63
- 230000000996 additive effect Effects 0.000 title claims abstract description 32
- 230000000694 effects Effects 0.000 title claims abstract description 20
- 239000003973 paint Substances 0.000 title claims description 15
- 239000000843 powder Substances 0.000 claims abstract description 112
- 238000000576 coating method Methods 0.000 claims abstract description 78
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 73
- 239000011248 coating agent Substances 0.000 claims abstract description 56
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 45
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- 229920003180 amino resin Polymers 0.000 claims abstract description 24
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 241000270295 Serpentes Species 0.000 claims abstract description 11
- -1 sulfonic acid imide Chemical class 0.000 claims abstract description 11
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- 239000011347 resin Substances 0.000 claims description 47
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- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 15
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- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 6
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- 125000000217 alkyl group Chemical group 0.000 claims description 3
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- 239000012972 dimethylethanolamine Substances 0.000 claims description 2
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 2
- CJMZLCRLBNZJQR-UHFFFAOYSA-N ethyl 2-amino-4-(4-fluorophenyl)thiophene-3-carboxylate Chemical compound CCOC(=O)C1=C(N)SC=C1C1=CC=C(F)C=C1 CJMZLCRLBNZJQR-UHFFFAOYSA-N 0.000 claims description 2
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 claims description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N mono-methylamine Natural products NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 claims 1
- OVOJUAKDTOOXRF-UHFFFAOYSA-N 2,4-dinitrobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O OVOJUAKDTOOXRF-UHFFFAOYSA-N 0.000 claims 1
- YCPXWRQRBFJBPZ-UHFFFAOYSA-N 5-sulfosalicylic acid Chemical compound OC(=O)C1=CC(S(O)(=O)=O)=CC=C1O YCPXWRQRBFJBPZ-UHFFFAOYSA-N 0.000 claims 1
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- MWVFCEVNXHTDNF-UHFFFAOYSA-N hexane-2,3-dione Chemical group CCCC(=O)C(C)=O MWVFCEVNXHTDNF-UHFFFAOYSA-N 0.000 claims 1
- UDGSVBYJWHOHNN-UHFFFAOYSA-N n',n'-diethylethane-1,2-diamine Chemical compound CCN(CC)CCN UDGSVBYJWHOHNN-UHFFFAOYSA-N 0.000 claims 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/28—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for wrinkle, crackle, orange-peel, or similar decorative effects
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
- C08K5/3447—Five-membered rings condensed with carbocyclic rings
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L33/04—Homopolymers or copolymers of esters
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- C08L33/08—Homopolymers or copolymers of acrylic acid esters
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Abstract
本发明公开了一种可作为干混用途的添加剂，以及由它和另一种具有纹理特征的底粉构成的具有蛇纹或龟纹效果的粉末涂料组成。干混添加剂本身也是一种粉末涂料组成物并具有平面高光泽，基本构成为一种或多种羟基聚酯树脂、氨基树脂交联剂、磺酸酰亚胺型催化剂、流平剂/除气剂和颜填料。具有蛇纹或龟纹效果的粉末涂料由上述干混添加剂和底粉组成，二者通过干混合构成本发明的龟纹和蛇纹粉末涂料，底粉与干混添加剂的重量比为1：0.0001‑1，优选为1：0.01‑0.1，更优选为1：0.02‑0.05。本发明与现有技术相比，改进了冲击性能和图案的稳定性，涂层的装饰效果也更佳。
The invention discloses an additive which can be used as dry mixing, and a powder coating composition with serpentine or moiré effect which is composed of it and another base powder with texture characteristics. The dry blend additive itself is also a powder coating composition with flat and high gloss. It is basically composed of one or more hydroxyl polyester resins, amino resin crosslinking agents, sulfonic acid imide catalysts, leveling agents/degassers agents and pigments. The powder coating with snake pattern or moiré effect is composed of the above-mentioned dry blend additive and primer, the two are dry mixed to form the moiré and snake pattern powder coating of the present invention, and the weight ratio of primer to dry blend additive is 1:0.0001 -1, preferably 1:0.01-0.1, more preferably 1:0.02-0.05. Compared with the prior art, the invention improves the impact performance and the stability of the pattern, and the decorative effect of the coating is also better.
Description
技术领域technical field
本发明涉及粉末涂料技术领域，尤其涉及一种粉末涂料用干混添加剂及其提供纹理效果的粉末涂料。The invention relates to the technical field of powder coatings, in particular to a dry mixing additive for powder coatings and a powder coating for providing texture effects.
背景技术Background technique
热固性粉末涂料是一种溶剂和挥发物排放量没有或者极少的环保型涂料，特别是在以VOC(Volatile Organic Compounds，挥发性有机化合物)排放标准日益严格的今天，其意义十分重大，市场份额正逐年增加。Thermosetting powder coating is an environmentally friendly coating with no or very little solvent and volatile emissions, especially in today's increasingly stringent VOC (Volatile Organic Compounds, volatile organic compounds) emission standards, it is of great significance and market share is increasing year by year.
热固性粉末涂料主要由官能性成膜树脂、固化剂、流平剂、颜/填料、一种或多种添加剂(助剂)、表面风格剂和其他性能改进剂等构成。制备过程通常包含将所有的组分一起置于高速混合机中干混合，然后通过合适的挤出机热熔融混炼、压片、粉碎和过筛等步骤。这样制成的粉末涂料可以通过粉末静电枪、摩擦枪喷涂或流化床浸涂使其粘附在底材上，通常是金属的表面，然后加热或辐射固化形成涂膜。Thermosetting powder coatings are mainly composed of functional film-forming resins, curing agents, leveling agents, pigments/fillers, one or more additives (auxiliaries), surface style agents and other performance improvers. The preparation process usually includes the steps of dry mixing all the components together in a high-speed mixer, followed by hot melt mixing through a suitable extruder, tableting, crushing and sieving. The powder coating produced in this way can be adhered to the substrate, usually the surface of the metal, by powder electrostatic gun, friction gun spraying or fluidized bed dipping, and then heated or radiated to form a coating film.
一般情况下通过以上步骤所得到的涂层具有高光泽和平面的装饰效果。但是，在一些特殊的应用领域倾向于使用具有纹理装饰效果的特殊涂层，例如金属防撬门、保险柜、五金工具和办公用品等。之所以作这样的要求，一方面是出于美学上的观赏需要，另一方面也是由于纹理粉末涂料本身通常比平面高光型粉末具有更好的瑕疵耐受性。也就是说对于要大表面涂装的被涂物，纹理能够很好地掩盖其表面缺陷从而避免喷涂失败。如果没有特殊的要求，在一些特殊的应用领域纹理型粉末涂料，尤其是皱纹、龟纹和蛇皮纹是优选的目标。事实也正是这样，近年来在这方面的需求正与日俱增。因此，设法提供成型稳定、易于制备和机械性能优越的上述特殊纹理粉末涂料是非常必要的。Generally, the coating obtained through the above steps has a high gloss and a flat decorative effect. However, special coatings with textured decorative effects tend to be used in some special applications, such as metal tamper-resistant doors, safes, hardware tools and office supplies. This requirement is partly due to aesthetics and partly because textured powder coatings are inherently more resistant to imperfections than flat high-gloss powders. That is to say, for the coated object to be painted on a large surface, the texture can well cover up its surface defects so as to avoid spraying failure. If there are no special requirements, textured powder coatings, especially wrinkles, moiré and snakeskin, are the preferred targets in some special application areas. This is also the case, and the demand in this area is increasing day by day in recent years. Therefore, it is very necessary to try to provide the above-mentioned special texture powder coatings with stable molding, easy preparation and superior mechanical properties.
对于一般的诸如橘纹、锤纹、砂纹、皱纹、仿古纹等粉末涂料系统，目前的技术措施是使用各种类型的纹理剂，例如聚四氟乙烯微粉、尼龙微粉、改性的聚丙烯/聚乙烯蜡、硅酮树脂、乙酸丁酸纤维素(CAB，Cellulose acetate butyrate)、聚乙烯醇缩丁醛(PVB，Polyvinyl butyral)和基于液体表面活性剂作为活性物成分的母体混合物(Masterbatch)等，其最典型的是业界十分熟悉的所谓“浮花剂”，其优选的活性成分为液体聚丙烯酸酯流平剂。For general powder coating systems such as orange grain, hammer grain, sand grain, wrinkle, and antique grain, the current technical measures are to use various types of texturing agents, such as polytetrafluoroethylene micropowder, nylon micropowder, modified polypropylene / Polyethylene wax, silicone resin, cellulose acetate butyrate (CAB, Cellulose acetate butyrate), polyvinyl butyral (PVB, Polyvinyl butyral) and liquid surfactant-based masterbatch as active ingredient (Masterbatch) etc., the most typical of which is the so-called "floating agent" that is very familiar in the industry, and its preferred active ingredient is a liquid polyacrylate leveling agent.
纹理粉末涂料的制备方法众所周知。其一是同于现行的平面高光泽粉，采用挤出机进行热熔融加工，即①所谓的一步挤出(one shot)工艺；另一种就是所谓的②“后添加(post addition)”混合技术。Methods of preparing textured powder coatings are well known. One is the same as the current flat high-gloss powder, using an extruder for hot-melt processing, that is, ① the so-called one-shot extrusion process; the other is the so-called ② "post addition" mixing technology.
①法典型的步骤包括将所有的组分一起置于高速混合机中干混合，然后用挤出机挤出均化。挤出后的物料经粉碎、过筛和包装制成最终的粉末涂料。但是对于大多数纹理粉末涂料来说，采用这种工艺往往只能得到少数几种典型的结构，例如砂纹和用CAB、PVB作为纹理剂的锤纹等。The typical steps of the ① method include putting all the components together in a high-speed mixer for dry mixing, and then extruding and homogenizing with an extruder. The extruded material is crushed, screened and packaged to make the final powder coating. But for most textured powder coatings, only a few typical structures can be obtained by using this process, such as sand grains and hammer grains using CAB and PVB as texture agents.
②法的制备步骤包括：(a)，预先制备一符合性能要求的底粉，该底粉可含有或不含有流平剂；(b)通过干混合向(a)组分中添加干混添加剂。所述的干混合方式可以是手动也可以是机械作用，例如使用V型结构的慢速混合器。②是现行应用最为广泛的技术方案，其优势在于纹理效果明显。因此它也成为本技术领域的优选，其延伸的技术优势是已经发展出了许多适合此种加工方式的干混添加剂。2. The preparation steps of the method include: (a), pre-preparing a base powder meeting the performance requirements, which may or may not contain a leveling agent; (b) adding dry blending additives to (a) component by dry mixing . The dry mixing method can be manual or mechanical, for example, using a slow mixer with a V-shaped structure. ② is currently the most widely used technical solution, and its advantage is that the texture effect is obvious. Therefore, it has also become the first choice in this technical field, and its extended technical advantage is that many dry blend additives suitable for this processing method have been developed.
众所周知，对于特殊的纹理，尤其是本发明所界定的龟纹、网纹、蛇皮纹等，由于其他大多数粉末涂料系统例如纯环氧、环氧/聚酯混合、聚酯/TGIC和羟烷基酰胺(HAA)并不太容易实现，因此习惯上采用羟基聚酯+氨基树脂(Aminoplast)交联剂和特殊催化剂的固化系统。这也是本技术领域优选的方案，构成本发明技术的一部分，适用于户内或户外的用途。It is well known that for special textures, especially moire, net, snakeskin, etc. as defined by the present invention, due to most other powder coating systems such as pure epoxy, epoxy/polyester hybrid, polyester/TGIC and hydroxyl Alkylamide (HAA) is not easy to realize, so it is customary to use a curing system of hydroxyl polyester + amino resin (Aminoplast) crosslinking agent and special catalyst. This is also a preferred solution in this technical field, which constitutes a part of the technology of the present invention and is suitable for indoor or outdoor use.
所述的羟基聚酯可以很方便地通过商购的途径获得；氨基树脂交联剂，典型的为甘脲类型，优选自四(甲氧基甲基)甘脲(缩写作TMMGU，n,n’,n”,n”’-tetramethoxymethylglycoluril)，化学结构：Described hydroxyl polyester can be obtained through commercially available way very conveniently; Amino resin cross-linking agent, is typically glycoluril type, is preferably from tetrakis (methoxymethyl) glycoluril (abbreviated as TMMGU, n,n ',n”,n”'-tetramethoxymethylglycoluril), chemical structure:
例如，取自美国Cytec公司的产品Powderlink 1174。For example, Powderlink 1174, a product from Cytec, USA.
US5447751，Morton International，Inc，发表于1995年9月5日，现全文引证作为参考。公开了使用一种环拉酸(cyclamic acid)作为催化剂的羟基聚酯/甘脲树脂的粉末涂料系统，其特征的纹理为皱纹(wrinkled finish)。但记载中没有使用干混添加剂。US5447751, Morton International, Inc, published September 5, 1995, which is hereby incorporated by reference in its entirety. A powder coating system of hydroxylated polyester/glycoluril resin using a cyclic acid as catalyst is disclosed, characterized by a wrinkled finish. However, no dry blend additive is used in the record.
另一授权专利US5695852，Morton International，Inc，发表于1997年12月9日，现全文引证作为参考。公开了使用一种三氟甲磺酸二乙胺盐作为催化剂、向羟基聚酯/甘脲树脂固化系统中添加少量的环氧化合物，通过一步挤出工艺实现龟纹(alligator)粉末涂料的技术方案。但记载中同样也没有使用干混添加剂。Another authorized patent US5695852, Morton International, Inc, published on December 9, 1997, is hereby incorporated by reference in its entirety. Disclosed is the technology of using a trifluoromethanesulfonate diethylamine salt as a catalyst, adding a small amount of epoxy compound to the hydroxyl polyester/glycoluril resin curing system, and realizing moire (alligator) powder coatings through a one-step extrusion process plan. However, there is also no dry blending additive used in the record.
作为这两篇授权专利的衍生，现行所发展出的改进技术是分别使用按US5447751和US5695852所述制成的标准粉末涂料作为底粉，然后向这样的底粉中通过干混合添加一种干混添加剂，例如浮花剂，实现所需要的纹理。具体地说，向专利5447751所述的底粉中一般得到的是蛇皮纹，而后者则为龟纹。As a derivative of these two authorized patents, the current improved technology is to use the standard powder coatings made as described in US5447751 and US5695852 respectively as the base powder, and then add a dry-blended powder to such a base powder by dry mixing Additives, such as embossing agents, achieve the desired texture. Specifically, what generally obtain in the bottom powder described in the patent 5447751 is a snakeskin pattern, while the latter is a moiré pattern.
众所周知，可以用作上述浮花剂的替代物还有许多种，例如经粉碎的固体双酚A环氧树脂、CAB、PVB和醛酮树脂等。As everyone knows, there are many alternatives that can be used as the above-mentioned floating agent, such as pulverized solid bisphenol A epoxy resin, CAB, PVB and aldehyde and ketone resins.
经验知道，使用这样的后混干混添加剂技术和原先采用的如US5447751和US5695852所述的技术相比所形成的纹理更加明显和稳定；另一个优势是可以不用或减少如US5695852所要求使用的环氧化合物，这是有利的一面因为已经发现配方中的环氧化合物会极大地影响机械性能。但另一方面，经验也知道，由于采用的干混添加剂大都为热塑性化合物或聚合物，在涂膜的交联过程中很难参与反应的进程，因此它们的存在将对连续涂膜的力学性能产生影响，结果导致差的机械性能，这是不期望的。因此努力发展一种干混添加剂，一方面它们能有效地提供所要求的纹理另一方面又不影响最终涂膜的机械性能是极端需要的。进而基于这样的干混添加剂而努力发展出一类新型的成型稳定、改进现行技术缺陷的纹理粉末涂料也是极端需要的。It is known from experience that the use of such a post-blending dry-blending additive technique results in a more pronounced and stable texture than previously employed techniques such as those described in US5447751 and US5695852; Oxygen compounds, this is an advantage as epoxies in the formulation have been found to greatly affect mechanical properties. But on the other hand, experience also knows that since most of the dry blending additives used are thermoplastic compounds or polymers, it is difficult to participate in the reaction process during the crosslinking process of the coating film, so their existence will affect the mechanical properties of the continuous coating film. have an effect, resulting in poor mechanical properties, which is undesirable. Efforts to develop dry blend additives which are effective in providing the desired texture on the one hand without affecting the mechanical properties of the final coating film on the other hand are therefore extremely desirable. Furthermore, based on such dry-blended additives, it is also extremely desirable to develop a new class of textured powder coatings with stable molding and improved existing technical defects.
发明内容Contents of the invention
本申请人通过种种努力发现一类新型的干混添加剂而完成了本发明。其特点是本发明的干混添加剂本身也是一种粉末涂料的组成物，因此可以参与后续的交联过程而成为交联结构的一部分，从而消除了以往的缺陷，即不会导致涂膜的机械性能变差。The present applicant has accomplished the present invention through various efforts to discover a new class of dry blend additives. Its characteristic is that the dry blend additive of the present invention is also a composition of powder coating itself, so it can participate in the subsequent cross-linking process and become a part of the cross-linking structure, thereby eliminating the previous defect, that is, it will not cause mechanical damage to the coating film. Performance deteriorates.
本发明的目的是提供一种作为干混用途的纹理添加剂，其本身也是一种粉末涂料组成物，但若单独喷涂则显示出平面和高光泽，无法单独形成纹理。The object of the present invention is to provide a texture additive for dry mixing, which itself is also a powder coating composition, but if it is sprayed alone, it will show plane and high gloss, and cannot form texture alone.
本发明的另一目的是向业界提供一种有效的干混添加剂及其由它构成的热固性纹理粉末涂料。所述的粉末涂料固化后纹理为龟纹、网纹和蛇皮纹等。Another object of the present invention is to provide the industry with an effective dry blend additive and a thermosetting textured powder coating composed of it. The cured texture of the powder coating is moiré, net and snakeskin.
本发明的进一步目的是提供一种具有上述纹理技术特征的热固性粉末涂料。其构成基础的底粉可以来源于任何现成的粉末涂料；再干混入本发明的特征添加剂后其纹理成型更加明显和稳定，尤其是明显地改进了机械性能。A further object of the present invention is to provide a thermosetting powder coating having the above texture technical features. The base powder that forms the basis can be derived from any ready-made powder coating; after dry mixing the characteristic additives of the present invention, its texture formation is more obvious and stable, especially the mechanical properties are obviously improved.
本发明提出的一种粉末涂料用干混添加剂，其原料包括：羟基树脂、氨基树脂交联剂、催化剂、助剂、颜填料。The invention proposes a dry blend additive for powder coatings, the raw materials of which include: hydroxyl resin, amino resin crosslinking agent, catalyst, auxiliary agent, pigment and filler.
优选地，助剂包括流平剂和/或除气剂。Preferably, the auxiliaries include leveling and/or degassing agents.
上述粉末涂料用干混添加剂和本发明所界定的底粉组成物基于相同的交联化学，即同源于羟基聚酯树脂和氨基树脂交联剂。采用干混添加剂进行单独喷涂，显示出平面和高光泽，不能单独形成纹理。The above-mentioned dry blending additives for powder coatings and the base powder composition defined by the present invention are based on the same crosslinking chemistry, that is, homogeneously derived from hydroxyl polyester resin and amino resin crosslinking agent. Sprayed alone with dry blend additives, it shows flat and high gloss and cannot be textured by itself.
上述粉末涂料用干混添加剂的原料按重量份包括：羟基树脂50-100份，氨基树脂交联剂1-10份，催化剂0.1-1份，流平剂0.5-1.5份，除气剂0.5-1.5份，颜填料0-50份，其余助剂0-2份。The raw materials of the above-mentioned dry blend additives for powder coatings include by weight: 50-100 parts of hydroxyl resin, 1-10 parts of amino resin crosslinking agent, 0.1-1 part of catalyst, 0.5-1.5 parts of leveling agent, and 0.5-10 parts of degassing agent. 1.5 parts, 0-50 parts of pigments and fillers, and 0-2 parts of other additives.
上述粉末涂料用干混添加剂的原料按重量份包括：羟基聚酯树脂50-100份，四甲氧基甲基甘脲1-10份，N-(甲磺酰基)-对-甲苯基磺酰胺0.1-1份，聚丙烯酸酯0.5-1.5份，安息香0.5-1.5份，颜填料0-50份，其余助剂0-2份。The raw materials of the above-mentioned dry blending additives for powder coatings include by weight: 50-100 parts of hydroxyl polyester resin, 1-10 parts of tetramethoxymethyl glycoluril, N-(methylsulfonyl)-p-tolylsulfonamide 0.1-1 part, polyacrylate 0.5-1.5 part, benzoin 0.5-1.5 part, pigment and filler 0-50 part, other additives 0-2 part.
上述组成物必需加工成可利用的粉末涂料型式才能构成本发明的干混添加剂。因此经挤出机挤出均化、冷却、粉碎和过筛这样加工步骤是必不可少的。粉碎是一个十分重要的过程，其粒度范围通常要求控制在通过80-200目筛(中国标准筛)。优选100-180目，更优选的为120-140目。The above composition must be processed into a usable powder coating form to constitute the dry blend additive of the present invention. Therefore, processing steps such as extruding through an extruder, homogenizing, cooling, crushing and sieving are essential. Crushing is a very important process, and its particle size range is usually required to be controlled to pass through a 80-200 mesh sieve (Chinese standard sieve). Preferably 100-180 mesh, more preferably 120-140 mesh.
已经观察到，本发明作为干混添加剂一个明显的技术优势不影响涂层的力学性能如抗冲击，这一点非常出乎意料。其可能的原因是它们本身也是成膜树脂的一部分而参与了化学反应进程，因而不像其他热塑性的干混添加剂损坏了涂膜的连续性。这是非常有意义的。It has been observed, quite unexpectedly, that the present invention, a clear technical advantage as a dry blend additive, does not affect the mechanical properties of the coating, such as impact resistance. The possible reason is that they themselves are also part of the film-forming resin and participate in the chemical reaction process, so unlike other thermoplastic dry-blended additives, they damage the continuity of the film. This is very meaningful.
另一个特殊的技术优势是，一般生产基于本发明的羟基聚酯树脂+氨基树脂交联化学的纹理粉末涂料的生产者也同时生产具有相同交联化学的平面高光泽涂料粉，因此本发明所界定的干粉添加剂事实上无需特别制备，它可以取自现行的涂料粉，这一点意义非常巨大，可以减少生产周期和降低生产成本。Another special technical advantage is that the producers who typically produce textured powder coatings based on the hydroxyl polyester resin + amino resin crosslinking chemistry of the present invention are also simultaneously producing flat high gloss coating powders with the same crosslinking chemistry, so the present invention In fact, the defined dry powder additive does not need to be specially prepared, and it can be obtained from the existing paint powder, which is of great significance, which can reduce the production cycle and reduce the production cost.
根据本发明，上述配方组成物可以通过调整上述配方的参数得到进一步优化，例如改变颜填料份额、使用和/或不使用流平剂和其他助剂和/或改变它们的用量等。一般来说，减少配方中填料的份额可以增大纹理；添加某些色料可以给图案带来令人愉悦的外观；某些任选的助剂将主要影响图案的风格。原则上说使用不加颜填料的配方更有利于干混纹理的形成、图案也更佳清晰稳定，这是所期望的。According to the present invention, the above formula composition can be further optimized by adjusting the parameters of the above formula, such as changing the proportion of pigments and fillers, using or not using leveling agents and other additives and/or changing their dosage, etc. Generally speaking, reducing the proportion of fillers in the formula can increase the texture; adding some colorants can bring a pleasing appearance to the pattern; some optional additives will mainly affect the style of the pattern. In principle, the use of a formula without pigments and fillers is more conducive to the formation of dry-mixed textures, and the patterns are clearer and more stable, which is expected.
优选地，羟基树脂为含羟基官能度的聚酯树脂和/或含羟基官能度的聚(甲基)丙烯酸树脂。这些树脂可以在催化剂存在下和甘脲型氨基树脂交联剂产生化学交联，具体如下：Preferably, the hydroxyl resin is a hydroxyl-functional polyester resin and/or a hydroxyl-functional poly(meth)acrylic resin. These resins can be chemically crosslinked with glycoluril type amino resin crosslinking agents in the presence of catalysts, as follows:
优选地，含羟基官能度的聚酯树脂的数均分子量为1000-40000，优选为1500-10000。Preferably, the hydroxyl functionality-containing polyester resin has a number average molecular weight of 1,000-40,000, preferably 1,500-10,000.
优选地，为保证产生有效的化学交联，含羟基官能度的聚酯树脂的官能度大于2，优选为2.2-3.5。一般认为，高官能度将有利于纹理的充分形成，而低官能度更倾向于形成平整光泽的表面，因此具有高官能度的树脂为本发明的优选。Preferably, the hydroxyl functionality-containing polyester resin has a functionality greater than 2, preferably 2.2 to 3.5, in order to ensure effective chemical crosslinking. It is generally believed that high functionality will be conducive to the full formation of texture, while low functionality tends to form a smooth and glossy surface, so resins with high functionality are preferred in the present invention.
优选地，含羟基官能度的聚酯树脂的羟值为10-100mgKOH/g，优选为20-80mgKOH/g，更优选为25-50mgKOH/g。Preferably, the hydroxyl value of the polyester resin containing hydroxyl functionality is 10-100 mgKOH/g, preferably 20-80 mgKOH/g, more preferably 25-50 mgKOH/g.
优选地，含羟基官能度的聚酯树脂的玻璃态转化温度Tg为40-80℃，优选为45-65℃，更优选为50-65℃。Preferably, the hydroxyl functionality-containing polyester resin has a glass transition temperature Tg of 40-80°C, preferably 45-65°C, more preferably 50-65°C.
上述含羟基官能度的聚酯树脂通常由相应的多元酸和多元醇缩合而成。所述多元酸的例子有对苯二甲酸、间苯二甲酸、1，4-环己基二甲酸、己二酸、马来酸、琥珀酸和偏苯三甲酸等；所述多元醇的例子有乙二醇、二甘醇、丙二醇、己二醇、新戊二醇、环己基二甲醇和三羟甲基丙烷等。The above-mentioned hydroxyl-functional polyester resins are generally formed by condensation of the corresponding polyacids and polyols. Examples of the polybasic acid include terephthalic acid, isophthalic acid, 1,4-cyclohexanedicarboxylic acid, adipic acid, maleic acid, succinic acid, and trimellitic acid, etc.; examples of the polyhydric alcohol include Ethylene glycol, diethylene glycol, propylene glycol, hexanediol, neopentyl glycol, cyclohexyldimethanol, and trimethylolpropane, etc.
这些树脂可以通过商购的途径得到，例如：These resins are available commercially, for example:
更具体地，可以浏览：www.cytec.com；www.dsmcoatingresins.com和www.nanfangresin.com中关于聚酯树脂(polyester resin)的描述，现全文引证作为参考。对本技术领域的相关技术人员来说这是公知的。More specifically, you can browse: www.cytec.com; www.dsmcoatingresins.com and www.nanfanggresin.com about polyester resin (polyester resin) description, the full text is hereby cited as a reference. This is well known to those skilled in the art.
同时，聚(甲基)丙烯酸树脂也可以作为成膜树脂，它们可以单独或和上述含羟基官能度的聚酯树脂结合作为成膜树脂的一部分。At the same time, poly(meth)acrylic resins can also be used as film-forming resins, which can be used alone or in combination with the above-mentioned polyester resins containing hydroxyl functionality as part of the film-forming resins.
化学上，聚(甲基)丙烯酸树脂可以通过聚合得到，其制备方法无特别的限制，只要能满足本发明限定的要求即可。习惯上，常使用的共聚方法包括本体聚合、游离基溶液聚合、乳液聚合和悬浮聚合等，其中游离基溶液聚合为优选。这样的技术对本技术领域的相关技术人员来说是公知的。Chemically, poly(meth)acrylic resin can be obtained by polymerization, and its preparation method is not particularly limited, as long as it can meet the requirements defined in the present invention. Conventionally, commonly used copolymerization methods include bulk polymerization, free radical solution polymerization, emulsion polymerization and suspension polymerization, among which free radical solution polymerization is preferred. Such techniques are well known to those skilled in the art.
根据本发明，所述的聚(甲基)丙烯酸树脂是含羟基官能度的。可以通过选择下列结构单体向组成中引入羟基官能团：According to the invention, said poly(meth)acrylic resin is hydroxyl-functional. Hydroxyl functionality can be introduced into the composition by selecting the following structural monomers:
其中：R1为H或C1-C4的烷基，优选为H或C1-C2的烷基，更优选的为甲基；R2为羟甲基或羟乙基，优选为羟甲基。Wherein: R 1 is H or C 1 -C 4 alkyl, preferably H or C 1 -C 2 alkyl, more preferably methyl; R 2 is hydroxymethyl or hydroxyethyl, preferably hydroxy methyl.
这些官能团单体，可以单独、也可以结合加入到共聚物的组成中。根据本发明，其用量为聚(甲基)丙烯酸树脂总重量的1-60wt％，优选5-50wt％，更加优选的是10-30wt％。These functional group monomers can be added alone or in combination to the composition of the copolymer. According to the present invention, the amount used is 1-60 wt%, preferably 5-50 wt%, more preferably 10-30 wt%, based on the total weight of the poly(meth)acrylic resin.
根据本发明，所述的聚(甲基)丙烯酸树脂还可能包括(甲基)丙烯酸酯，具体是(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸十二烷基酯和(甲基)丙烯酸苄基酯等。According to the present invention, the poly(meth)acrylic resin may also include (meth)acrylates, specifically methyl (meth)acrylate, ethyl (meth)acrylate, n-propyl (meth)acrylate , isopropyl (meth)acrylate, n-butyl (meth)acrylate, isobutyl (meth)acrylate, tert-butyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, ( Octyl methacrylate, dodecyl (meth)acrylate, benzyl (meth)acrylate, etc.
此外，本发明的共聚单体中还可能包括其他乙烯基单体，例如苯乙烯或甲基苯乙烯。根据本发明，其用量为聚(甲基)丙烯酸树脂总重量的10-70％，优选为35-50％。In addition, it is also possible to include other vinyl monomers, such as styrene or methylstyrene, in the comonomers of the present invention. According to the present invention, its dosage is 10-70% of the total weight of the poly(meth)acrylic resin, preferably 35-50%.
聚(甲基)丙烯酸树脂的聚合过程中还需要加入引发剂，所列举的包括偶氮二异丁腈(AIBN)、过氧化二苯甲酰(BPO)、叔丁基过氧化氢和过氧化二异丙苯等，其中以BPO和过氧化二异丙苯为优选。In the polymerization process of poly(meth)acrylic resin, initiators also need to be added, such as azobisisobutyronitrile (AIBN), dibenzoyl peroxide (BPO), tert-butyl hydroperoxide and peroxide Dicumyl, etc., wherein BPO and dicumyl peroxide are preferred.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的数均分子量为1000-20000，优选为2000-10000，更优选为2000-5000。Preferably, the poly(meth)acrylic resin containing hydroxyl functionality has a number average molecular weight of 1,000-20,000, preferably 2,000-10,000, more preferably 2,000-5,000.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的羟值为10-100mgKOH/g，优选为20-80mgKOH/g，更优选为25-50mgKOH/g。Preferably, the hydroxyl value of the poly(meth)acrylic resin containing hydroxyl functionality is 10-100 mgKOH/g, preferably 20-80 mgKOH/g, more preferably 25-50 mgKOH/g.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的玻璃态转化温度Tg为30-110℃，优选为45-70℃。Preferably, the poly(meth)acrylic resin containing hydroxyl functionality has a glass transition temperature Tg of 30-110°C, preferably 45-70°C.
优选地，氨基树脂交联剂为是三聚氰胺/甲醛树脂、烷氧基化的甘脲树脂，尤其是六甲氧基甲基三聚氰胺和四甲氧基甲基甘脲；优选为四甲氧基甲基甘脲，因为它在室温状态下为固体，特别适用于粉末涂料的用途。Preferably, the amino resin crosslinking agent is melamine/formaldehyde resin, alkoxylated glycoluril resin, especially hexamethoxymethyl melamine and tetramethoxymethyl glycoluril; preferably tetramethoxymethyl Glycoluril, because it is solid at room temperature, is particularly suitable for powder coating applications.
上述交联剂可以很方便地通过商业的途径购得，例如购自美国Cytec公司的Powderlink 1174，其主要的技术特征如下：The above-mentioned crosslinking agent can be purchased through commercial channels very conveniently, such as Powderlink 1174 purchased from U.S. Cytec Company, and its main technical characteristics are as follows:
此外，这样的交联剂也可以是购自山西太原科源化学有限公司，这些对本技术领域的相关技术人员来说是公知的。In addition, such crosslinking agents can also be purchased from Shanxi Taiyuan Keyuan Chemical Co., Ltd., which are well known to those skilled in the art.
根据本发明，氨基树脂交联剂与羟基树脂的重量比为4-20：100，优选为5-7：100，主要取决于树脂的羟值。According to the present invention, the weight ratio of the amino resin crosslinking agent to the hydroxyl resin is 4-20:100, preferably 5-7:100, mainly depending on the hydroxyl value of the resin.
优选地，催化剂为有机磺酸和/或磺酰亚胺类化合物，可提供光洁的表面。Preferably, the catalyst is an organic sulfonic acid and/or sulfonimide compound, which can provide a smooth surface.
优选地，有机磺酸和/或磺酰亚胺类化合物在本发明粉末涂料中所占重量百分比为0.05-3％，优选为0.1-1％，更优选为0.2-0.5％。Preferably, the weight percentage of the organic sulfonic acid and/or sulfonimide compound in the powder coating of the present invention is 0.05-3%, preferably 0.1-1%, more preferably 0.2-0.5%.
优选的，催化剂为对甲苯磺酸、二壬基萘磺酸、十二烷基苯磺酸、二苯磺酰亚胺和/或N-(甲磺酰基)-对-甲苯基磺酰胺，优选为N-(甲磺酰基)-对-甲苯基磺酰胺。Preferably, the catalyst is p-toluenesulfonic acid, dinonylnaphthalenesulfonic acid, dodecylbenzenesulfonic acid, diphenylsulfonimide and/or N-(methylsulfonyl)-p-tolylsulfonamide, preferably For N-(methylsulfonyl)-p-toluenesulfonamide.
本发明还提出的一种可提供蛇纹或龟纹效果的粉末涂料，其原料包括：上述粉末涂料用干混添加剂，和底粉。The present invention also proposes a powder coating that can provide snake pattern or moiré effect, and its raw materials include: the above-mentioned dry blend additive for powder coating, and primer.
优选地，底粉与上述粉末涂料用干混添加剂的重量比为1：0.0001-1，优选为1：0.01-0.1，更优选为1：0.02-0.05。Preferably, the weight ratio of the base powder to the above-mentioned dry blend additive for powder coating is 1:0.0001-1, preferably 1:0.01-0.1, more preferably 1:0.02-0.05.
优选地，底粉的原料包括：羟基树脂、氨基树脂交联剂、氨或胺封闭的磺酸型催化剂、助剂、颜填料。Preferably, the raw materials of the primer include: hydroxyl resin, amino resin crosslinking agent, ammonia or amine-blocked sulfonic acid catalyst, additives, pigments and fillers.
优选地，助剂包括流平剂和/或除气剂。Preferably, the auxiliaries include leveling and/or degassing agents.
根据本发明，作为本发明粉末涂料系统的底粉由羟基聚酯、氨基树脂交联剂和特殊催化剂等所构成，其典型特征是：若不使用干混添加剂，其单独固化后也可以实现皱纹和浅度龟纹中的任何一种，因此其本身也是一类纹理型粉末涂料，但所形成的稳定稳定性极差，对于工厂生产而言废品率过高。According to the present invention, the base powder as the powder coating system of the present invention is composed of hydroxyl polyester, amino resin crosslinking agent and special catalyst, etc. Its typical characteristics are: if no dry blend additives are used, it can also achieve wrinkles after curing alone And shallow moiré, so it is also a kind of textured powder coating itself, but the stability formed is extremely poor, and the reject rate is too high for factory production.
这样的粉末涂料组成物对本技术领域的相关技术人员来说是公知的。例如由上文所列的US5447751和US5695852所披露的那些，现全文引证作为参考。本发明对这样的系统底粉没有特别的限定，只要不影响本发明的实施即可。但是要作为恰当的底粉，对US5447751和US5695852所披露的内容做些局部的改进和衍生也是容许的。Such powder coating compositions are well known to those skilled in the art. For example those disclosed in US5447751 and US5695852 listed above, which are hereby incorporated by reference in their entirety. The present invention has no special limitation on such a system primer, as long as it does not affect the implementation of the present invention. But to be used as a proper primer, some local improvements and derivatives are also allowed to the contents disclosed in US5447751 and US5695852.
上述底粉的原料按重量份包括：羟基树脂50-100份，氨基树脂交联剂1-10份，氨或胺封闭的磺酸型催化剂0.1-1份，流平剂0.5-1.5份，除气剂0.5-1.5份，颜填料0-50份，其余助剂0-2份。The raw materials of the above-mentioned base powder include by weight: 50-100 parts of hydroxyl resin, 1-10 parts of amino resin crosslinking agent, 0.1-1 part of ammonia or amine-blocked sulfonic acid catalyst, 0.5-1.5 parts of leveling agent, except 0.5-1.5 parts of air agent, 0-50 parts of pigment and filler, and 0-2 parts of other additives.
上述底粉的原料按重量份包括：羟基树脂50-100份，固体环氧树脂1-5份，氨基树脂交联剂1-10份，氨或胺封闭的磺酸型催化剂0.1-1份，流平剂0.5-1.5份，除气剂0.5-1.5份，颜填料0-50份，其余助剂0-2份。The raw materials of the above-mentioned base powder include by weight: 50-100 parts of hydroxyl resin, 1-5 parts of solid epoxy resin, 1-10 parts of amino resin crosslinking agent, 0.1-1 part of ammonia or amine-blocked sulfonic acid catalyst, 0.5-1.5 parts of leveling agent, 0.5-1.5 parts of degassing agent, 0-50 parts of pigment and filler, and 0-2 parts of other additives.
上述底粉的原料按重量份包括：羟基聚酯树脂50-100份，固体环氧树脂1-5份，四甲氧基甲基甘脲1-10份，胺封闭磺酸0.1-1份，聚丙烯酸酯0.5-1.5份，安息香0.5-1.5份，颜填料0-50份，其余助剂0-2份。The raw materials of the above-mentioned base powder include by weight: 50-100 parts of hydroxyl polyester resin, 1-5 parts of solid epoxy resin, 1-10 parts of tetramethoxymethyl glycoluril, 0.1-1 part of amine blocked sulfonic acid, 0.5-1.5 parts of polyacrylate, 0.5-1.5 parts of benzoin, 0-50 parts of pigments and fillers, and 0-2 parts of other additives.
根据本发明，作为底粉仍需要单独制成粉末涂料。其特征是预先经历挤出机挤出均化、冷却、粉碎和过筛等这样的加工步骤。粉碎的粒度范围通常要求控制在通过80-200目筛(中国标准筛)。优选100-180目，更优选的为120-140目。According to the present invention, still need to make powder coating separately as primer. It is characterized in that it has gone through such processing steps as extruder homogenization, cooling, crushing and sieving in advance. The particle size range of crushing is usually required to be controlled to pass through a 80-200 mesh sieve (Chinese standard sieve). Preferably 100-180 mesh, more preferably 120-140 mesh.
根据本发明，上述底粉配方组成物可以通过调整上述配方的参数得到进一步优化，例如改变颜填料份额、使用和/或不使用流平剂和其他助剂和/或改变它们的用量等。According to the present invention, the formula composition of the above-mentioned foundation powder can be further optimized by adjusting the parameters of the formula, such as changing the proportion of pigments and fillers, using or not using leveling agents and other additives and/or changing their dosage.
除此之外，本发明之底粉粉末涂料还可以任意地加入着色剂，通常为一种或多种的颜料或染料。也可能进一步含有一种或多种的性能助剂，例如流平剂、增塑剂、稳定剂如防止UV降解的稳定剂、除气剂如安息香、一种到多种的填料。颜料的例子有无机的TiO2、氧化铁红和黄、铬颜料和碳黑；有机的包括酞青蓝、偶氮、蒽醌、硫靛、苯并蒽酮、三苯二烷和喹吖(二)酮颜料，还原染料、莱克氏酸、碱以及媒染料。染料可被颜料所取代。In addition, the base powder coating of the present invention can also optionally add a colorant, usually one or more pigments or dyes. It is also possible to further contain one or more performance aids, such as leveling agents, plasticizers, stabilizers such as stabilizers for preventing UV degradation, degassing agents such as benzoin, and one or more fillers. Examples of pigments are inorganic TiO 2 , iron oxide red and yellow, chromium pigments, and carbon black; organic ones include phthalocyanine blue, azo, anthraquinone, thioindigo, benzoanthrone, triphenyldioxane, and quinacridine ( 2) Ketone pigments, vat dyes, Reich's acid, alkali and mordant dyes. Dyes can be replaced by pigments.
优选地，羟基树脂为含羟基官能度的聚酯树脂和/或含羟基官能度的聚(甲基)丙烯酸树脂，同上述干混添加剂中关于含羟基官能度的聚酯树脂和含羟基官能度的聚(甲基)丙烯酸树脂的解释。Preferably, the hydroxyl resin is a hydroxyl-functional polyester resin and/or a hydroxyl-functional poly(meth)acrylic resin, as described above for the hydroxyl-functional polyester resin and hydroxyl-functional poly(meth)acrylic resin. Poly(meth)acrylic resins explained.
优选地，含羟基官能度的聚酯树脂的数均分子量为1000-40000，优选为1500-10000。Preferably, the hydroxyl functionality-containing polyester resin has a number average molecular weight of 1,000-40,000, preferably 1,500-10,000.
优选地，含羟基官能度的聚酯树脂的官能度大于2，优选为2.2-3.5。Preferably, the hydroxyl functionality-containing polyester resin has a functionality greater than 2, preferably from 2.2 to 3.5.
优选地，含羟基官能度的聚酯树脂的羟值为10-100mgKOH/g，优选为20-80mgKOH/g，更优选为25-50mgKOH/g。Preferably, the hydroxyl value of the polyester resin containing hydroxyl functionality is 10-100 mgKOH/g, preferably 20-80 mgKOH/g, more preferably 25-50 mgKOH/g.
优选地，含羟基官能度的聚酯树脂的玻璃态转化温度Tg为40-80℃，优选为45-65℃，更优选为50-65℃。Preferably, the hydroxyl functionality-containing polyester resin has a glass transition temperature Tg of 40-80°C, preferably 45-65°C, more preferably 50-65°C.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的数均分子量为1000-20000，优选为2000-10000，更优选为2000-5000。Preferably, the poly(meth)acrylic resin containing hydroxyl functionality has a number average molecular weight of 1,000-20,000, preferably 2,000-10,000, more preferably 2,000-5,000.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的羟值为10-100mgKOH/g，优选为20-80mgKOH/g，更优选为25-50mgKOH/g。Preferably, the hydroxyl value of the poly(meth)acrylic resin containing hydroxyl functionality is 10-100 mgKOH/g, preferably 20-80 mgKOH/g, more preferably 25-50 mgKOH/g.
优选地，含羟基官能度的聚(甲基)丙烯酸树脂的玻璃态转化温度Tg为30-110℃，优选为45-70℃。Preferably, the poly(meth)acrylic resin containing hydroxyl functionality has a glass transition temperature Tg of 30-110°C, preferably 45-70°C.
优选地，氨基树脂交联剂为甘脲型氨基树脂，同上述干混添加剂中关于氨基树脂交联剂的解释；优选为四甲氧基甲基甘脲。Preferably, the amino resin cross-linking agent is a glycoluril type amino resin, the same as the explanation about the amino resin cross-linking agent in the above-mentioned dry blend additive; preferably tetramethoxymethyl glycoluril.
优选地，氨或胺封闭的磺酸型催化剂为由氨或胺与磺酸反应所形成的盐，可提供纹理；胺的结构为：RxNH3-x，其中R为C1-4的烷基，0＜x≤3。Preferably, the ammonia or amine-blocked sulfonic acid catalyst is a salt formed by the reaction of ammonia or amine and sulfonic acid, which can provide texture; the structure of the amine is: R x NH 3-x , wherein R is C 1-4 Alkyl, 0<x≤3.
优选地，氨或胺封闭的磺酸型催化剂在本发明粉末涂料中所占重量百分比为0.05-3％，优选为0.1-1％，更优选为0.2-0.5％。Preferably, the ammonia or amine-blocked sulfonic acid catalyst accounts for 0.05-3% by weight in the powder coating of the present invention, preferably 0.1-1%, more preferably 0.2-0.5%.
优选地，胺为甲基胺、二甲基胺、三甲基胺、乙胺、丙胺、二丙胺、丁基胺、三乙胺、二丁基胺、苄基胺、乙醇胺、二甲基乙醇胺、N,N-二乙基乙醇胺和/或二异丙醇胺，优选为二乙胺和/或N,N-二乙基乙醇胺。Preferably, the amine is methylamine, dimethylamine, trimethylamine, ethylamine, propylamine, dipropylamine, butylamine, triethylamine, dibutylamine, benzylamine, ethanolamine, dimethylethanolamine , N,N-diethylethanolamine and/or diisopropanolamine, preferably diethylamine and/or N,N-diethylethanolamine.
优选地，磺酸为对甲苯磺酸、邻硝基苯磺酸、间硝基苯磺酸、对硝基苯磺酸、硝基苯-2,4-二磺酸、2-硝基甲苯基-3-磺酸、邻位磺基苯甲酸、磺基水杨酸、磺基邻苯二甲酸、2,4-二硝基苯磺酸、3,5-二硝基苯磺酸和/或环拉酸，优选为对甲苯磺酸、邻硝基苯磺酸、间硝基苯磺酸、对硝基苯磺酸、硝基苯-2,4-二磺酸、邻位磺基苯甲酸、磺基水杨酸和/或环拉酸，更优选为对甲苯磺酸和/或环拉酸。Preferably, the sulfonic acid is p-toluenesulfonic acid, o-nitrobenzenesulfonic acid, m-nitrobenzenesulfonic acid, p-nitrobenzenesulfonic acid, nitrobenzene-2,4-disulfonic acid, 2-nitrotolyl -3-sulfonic acid, o-sulfobenzoic acid, sulfosalicylic acid, sulfophthalic acid, 2,4-dinitrobenzenesulfonic acid, 3,5-dinitrobenzenesulfonic acid and/or Cyclonic acid, preferably p-toluenesulfonic acid, o-nitrobenzenesulfonic acid, m-nitrobenzenesulfonic acid, p-nitrobenzenesulfonic acid, nitrobenzene-2,4-disulfonic acid, ortho-sulfobenzoic acid , sulfosalicylic acid and/or cyclamic acid, more preferably p-toluenesulfonic acid and/or cyclamic acid.
优选地，底粉的原料还包括：环氧树脂。Preferably, the raw material of the primer further includes: epoxy resin.
根据本发明，固体环氧树脂也可以存在于本发明粉末涂料的组成中，尽管其用量很少。如果在底粉的配方组成中使用环氧树脂，它将通过组成中的仲羟基和甘脲固化剂发生作用，因此它也构成为本发明成膜树脂的一部分。According to the invention, solid epoxy resins may also be present in the composition of the powder coatings according to the invention, albeit in small amounts. If epoxy resin is used in the formula composition of primer, it will act through the secondary hydroxyl group and glycoluril curing agent in the composition, so it also constitutes a part of the film-forming resin of the present invention.
根据本发明，所述的环氧树脂可以是任选的双酚A型、双酚F型、双酚S型、EPN型(线性酚醛环氧树脂)、ECN型(邻甲酚线性酚醛环氧树脂)、三羟苯基甲烷型、四酚基乙烷型和其他杂环型以及它们的改性型产品；根据本发明，由所列举的环氧树脂的含卤素产品也是适合的，它们通常能提供更好的耐热和电绝缘性能。According to the present invention, the epoxy resin can be optional bisphenol A type, bisphenol F type, bisphenol S type, EPN type (novolac epoxy resin), ECN type (o-cresol novolac epoxy resin) Resin), trishydroxyphenylmethane type, tetraphenol ethane type and other heterocyclic types and their modified products; according to the present invention, the halogen-containing products of the epoxy resins listed are also suitable, and they are usually Can provide better heat resistance and electrical insulation properties.
优选地，环氧树脂为双酚A型环氧树脂或双酚F型环氧树脂，优选为双酚A型环氧树脂，更优选为1-9型双酚A型环氧树脂固体产品，更更优选为2-7型双酚A型环氧树脂固体产品，特别优选为3-4型双酚A型环氧树脂固体产品。Preferably, the epoxy resin is a bisphenol A type epoxy resin or a bisphenol F type epoxy resin, preferably a bisphenol A type epoxy resin, more preferably a 1-9 type bisphenol A type epoxy resin solid product, It is more preferably a 2-7 type bisphenol A type epoxy resin solid product, especially preferably a 3-4 type bisphenol A type epoxy resin solid product.
优选地，环氧树脂在本发明粉末涂料中所占重量百分比为0.01-1％，优选0.1-0.5％，更优选的0.2-0.4％。Preferably, the weight percentage of epoxy resin in the powder coating of the present invention is 0.01-1%, preferably 0.1-0.5%, more preferably 0.2-0.4%.
根据本发明尽管使用上述固体环氧树脂可以实现所要求的纹理，但是其效果同样相当有限，纹理偏小或不充分，此外也具有差的机械性能，因此并不是本发明所特别期望的。Although the desired texture can be achieved according to the invention with the above-mentioned solid epoxy resin, the effect is also quite limited, the texture is small or insufficient, and also has poor mechanical properties, so it is not particularly desirable in the present invention.
优选地，粉末涂料的原料还包括：乙酰丁酰基纤维素(CAB)、聚乙烯醇缩丁醛(PVB)和/或醛酮树脂。Preferably, the raw materials of the powder coating also include: cellulose acetobutyryl (CAB), polyvinyl butyral (PVB) and/or aldehyde and ketone resins.
根据本发明，需要向本发明的底粉中添加干混添加剂。According to the invention, it is necessary to add dry blend additives to the primer of the invention.
向底粉中添加干混添加剂来实现所期望的纹理技术在本行业是众所周知的。业界已有多种类型可供选择的添加剂，例如CAB、PVB、醛酮树脂和浮花剂等，其中应最广的为浮花剂。某些经粉碎的固体双酚A环氧树脂和醛酮树脂也特别适合本发明的用途，因此它们也是一种有效的干混添加剂。The addition of dry blend additives to foundation powders to achieve a desired texture technique is well known in the industry. There are many types of additives available in the industry, such as CAB, PVB, aldehydes and ketone resins, and embossing agents, among which embossing agents should be the most widely used. Certain comminuted solid bisphenol A epoxy resins and aldehyde and ketone resins are also particularly suitable for use in the present invention and are therefore also effective dry blend additives.
CAB为热塑性树脂，其分子式可以表达为：CAB is a thermoplastic resin, and its molecular formula can be expressed as:
[C6H7O2(OCOCH3)x(OCOC3H7)y(OH)3-x-y]n [C 6 H 7 O 2 (OCOCH 3 ) x (OCOC 3 H 7 ) y (OH) 3-xy ] n
CAS号：9004-36-8CAS number: 9004-36-8
理想的化学结构式为：The ideal chemical structural formula is:
其中：R为 Where: R is
工业上最重要的CAB提供者为美国Eastman Kodak公司，它拥有一族乙酰基(acetyl)和丁酰基(butyryl)含量不同的产品。The most important CAB provider in the industry is Eastman Kodak Company of the United States, which has a family of products with different acetyl and butyryl contents.
三种典型的产品可作为粉末涂料纹理剂的用途，其主要的技术特性概括见下表：Three typical products can be used as texture agents for powder coatings, and their main technical characteristics are summarized in the table below:
US5321063，Nippon Oil and Fats，发表于1994年6月14日，现全文引证作为参考。另一篇授权专利US5498663，Nippon Oil and Fats，发表于1996年3月12日，现也全文引证作为参考。公开了使用含上述CAB的环氧和/或环氧/聚酯混合型粉末涂料作为干混添加剂实现所期望纹理的技术方案，但是所得到纹理为锤纹，并非为本发明所界定的纹理类型，因此也不属于本发明的技术范畴。US5321063, Nippon Oil and Fats, published June 14, 1994, is hereby incorporated by reference in its entirety. Another authorized patent US5498663, Nippon Oil and Fats, was published on March 12, 1996, which is also cited in its entirety as a reference. Disclosed is the use of epoxy and/or epoxy/polyester hybrid powder coatings containing the above CAB as a dry blend additive to achieve the desired texture, but the resulting texture is hammered and not the type of texture defined in the present invention , and therefore do not belong to the technical scope of the present invention.
另一种可作为干混添加剂使用的是PVB树脂。PVB可以通过聚乙烯醇(PVA)和丁醛在酸性条件下缩合而成，其CAS号：63148-65-2。Another available dry blend additive is PVB resin. PVB can be formed by condensation of polyvinyl alcohol (PVA) and butyraldehyde under acidic conditions, its CAS number: 63148-65-2.
由于羟醛缩合总是不能进行完全，因此在所形成的树脂结构中将残存一定量的-OH。羟基含量的多少取决于乙酰化程度，基本规则是乙酰化程度愈高其残存的-OH数就愈少，反之亦然。Since the aldol condensation cannot always be completed completely, a certain amount of -OH will remain in the formed resin structure. The amount of hydroxyl group depends on the degree of acetylation. The basic rule is that the higher the degree of acetylation, the less the number of remaining -OH, and vice versa.
适合作为粉末涂料干混添加剂用途的是它的低分子量产品，这些树脂对本技术领域的相关技术人员来说是公知的。例如商购自日本可乐丽(Kuraray)公司的B20H和30T或者60H等，优选自B20H和30T。但是使用这样的树脂所得的纹理为浅平的锤纹，并非为本发明所界定的纹理类型，因此同样也不属于本发明的技术范畴。Suitable for use as dry blend additives for powder coatings are its low molecular weight products, and these resins are well known to those skilled in the art. For example, B20H and 30T or 60H commercially available from Japan Kuraray (Kuraray) Co., Ltd., preferably B20H and 30T. However, the texture obtained by using such resin is shallow and flat hammer pattern, which is not the type of texture defined by the present invention, and thus also does not belong to the technical scope of the present invention.
更进一步地，某些醛酮树脂适合作为本发明的干混添加剂提供所期望的纹理。酮醛树脂是一类由酮和/或醛经缩聚反应得到的聚合物，也称为酮醛树脂或者聚酮树脂。其化学结构可以描述为：Still further, certain aldehyde and ketone resins are suitable as dry blend additives of the present invention to provide the desired texture. Keto-aldehyde resins are a class of polymers obtained by polycondensation of ketones and/or aldehydes, also known as ketone-aldehyde resins or polyketone resins. Its chemical structure can be described as:
一般来说，未经改性的醛酮树脂分子结构中含有羰基，端基为羟基，在涂料、油墨和其他领域有着广泛地用途。Generally speaking, unmodified aldehyde and ketone resins contain carbonyl groups in their molecular structure, and the terminal groups are hydroxyl groups. They are widely used in coatings, inks and other fields.
我们已经发现，某些含有伯/仲羟基的化合物和树脂适合作为本发明的干混添加剂。We have found that certain compounds and resins containing primary/secondary hydroxyl groups are suitable as dry blend additives in the present invention.
酮醛树脂在涂料和油墨行业是众所周知的，这样的树脂可以商购自山东圣马生物科技有限公司。更具体地，可以浏览：www.smabio.com关于AK酮醛树脂的描述，现全文引证作为参考。Keto-formaldehyde resins are well known in the coating and ink industry, and such resins are commercially available from Shandong Shengma Biotechnology Co., Ltd. More specifically, you can browse: www.smabio.com for a description of AK ketone-aldehyde resin, which is hereby cited in its entirety as a reference.
合适的醛酮树脂没有特别限定，只要它们符合要求即可。一般来说，根据本发明选择低分子量、具有合适软化点，例如50-150℃，优选80-120℃的产品为佳。例如典型的为酮醛树脂AK120和醛树脂HS-A81，优选为HS-A81。Suitable aldehyde and ketone resins are not particularly limited as long as they meet the requirements. Generally speaking, according to the present invention, it is better to choose a product with a low molecular weight and a suitable softening point, such as 50-150°C, preferably 80-120°C. Typical examples are ketone-aldehyde resin AK120 and aldehyde resin HS-A81, preferably HS-A81.
优选地，醛酮树脂在本发明粉末涂料中所占重量百分比为0.01-1％，优选0.1-0.5％，更优选的0.2-0.4％。Preferably, the weight percentage of the aldehyde and ketone resin in the powder coating of the present invention is 0.01-1%, preferably 0.1-0.5%, more preferably 0.2-0.4%.
尽管使用上述的醛酮树脂可以实现本发明所要求的纹理，但是其效果相当有限，纹理偏小或不充分，此外也具有差的机械性能。尽管这样的应用可看做本发明的一部分，但不是本发明所特别期望的。Although the texture required by the present invention can be achieved by using the above-mentioned aldehyde and ketone resins, the effect is rather limited, the texture is small or insufficient, and it also has poor mechanical properties. While such use is considered part of the present invention, it is not specifically contemplated by the present invention.
所谓的浮花剂在本行业是众所周知的。它可以是丙烯酸树脂(俗称光亮剂)和/或聚醚型液体流平剂吸附在固体丙烯酸树脂中的复合产品。也可以是用环氧/聚酯混合型粉末涂料作为吸附材料的上述液体流平剂的复合产品。优选的可以是“95％光亮剂+5％丙烯酸丁酯液体流平剂”的复合。So-called floating agents are well known in the art. It can be a composite product of acrylic resin (commonly known as brightener) and/or polyether liquid leveling agent adsorbed in solid acrylic resin. It can also be a composite product of the above-mentioned liquid leveling agent using epoxy/polyester mixed powder coating as the adsorption material. The preferred compound can be "95% brightener + 5% butyl acrylate liquid leveling agent".
根据本发明，这类浮花剂可以很方便地通过商购的途径从市场上获得。一种优选的产品是黄山惠久粉末材料有限公司的WHCC。According to the present invention, this type of floating agent can be obtained from the market through commercial channels very conveniently. A preferred product is WHCC from Huangshan Huijiu Powder Materials Co., Ltd.
优选地，浮花剂在本发明粉末涂料中所占重量百分比为0.01-1％，优选0.1-0.5％，更优选的0.2-0.4％。Preferably, the weight percentage of the embossing agent in the powder coating of the present invention is 0.01-1%, preferably 0.1-0.5%, more preferably 0.2-0.4%.
根据本发明尽管使用上述浮花剂可以实现所要求的纹理且成型稳定，但是其效果同样相当有限，纹理偏小。此外也具有相对差的机械性能，因此并不是本发明所特别期望的。According to the present invention, although the required texture can be achieved and the shape is stable by using the above-mentioned embossing agent, its effect is also quite limited, and the texture is relatively small. It also has relatively poor mechanical properties and is therefore not particularly desirable in the present invention.
本发明采用上述干混剂和上述底粉进行配合，使涂膜呈现蛇纹或龟纹，纹理清晰，大小适中，而且成型稳定，废品率低，同时机械性能十分优秀The present invention adopts the above-mentioned dry mixture and the above-mentioned primer to make the coating film present serpentine or moiré patterns, with clear texture, moderate size, stable molding, low reject rate and excellent mechanical properties.
附图说明Description of drawings
图1为本发明所得典型皱纹图案的涂膜。Fig. 1 is the coating film of the typical wrinkle pattern obtained in the present invention.
图2为本发明所得典型龟纹图案的涂膜。Fig. 2 is the coating film of the typical moiré pattern obtained in the present invention.
图3为本发明所得典型莽蛇纹图案的涂膜。Fig. 3 is the coating film of the typical wild snake pattern obtained in the present invention.
图4为本发明所得典型蛇皮纹图案的涂膜。Fig. 4 is the coating film of the typical snakeskin pattern obtained in the present invention.
具体实施方式detailed description
下面，通过具体实施例对本发明的技术方案进行详细说明。Below, the technical solution of the present invention will be described in detail through specific examples.
实施例1制备基础底粉1-1，记为D1-1(皱纹，黑)Example 1 prepares foundation powder 1-1, denoted as D1-1 (wrinkle, black)
按重量份将300份羟基聚酯树脂YE-2080、19份四甲氧基甲基甘脲、1.5份胺封闭的对甲苯磺酸催化剂AHA6319、6份聚丙烯酸酯流平剂AHA1088P、170份硫酸钡、1.5份安息香和3.0份炭黑混合3-5min，然后加入到双螺杆试验用挤出机中熔融均化，压片、冷却和碾磨成细粉，过筛通过140目得到基础底粉(D1-1)。By weight, 300 parts of hydroxyl polyester resin YE-2080, 19 parts of tetramethoxymethyl glycoluril, 1.5 parts of amine-blocked p-toluenesulfonic acid catalyst AHA6319, 6 parts of polyacrylate leveling agent AHA1088P, 170 parts of sulfuric acid Barium, 1.5 parts of benzoin and 3.0 parts of carbon black were mixed for 3-5 minutes, then added to a twin-screw extruder for testing, melted and homogenized, pressed into tablets, cooled and ground into a fine powder, and sieved through a 140 mesh to obtain the base powder (D1-1).
实施例2制备基础底粉1-2，记为D1-2(龟纹，白)Example 2 prepares the base powder 1-2, denoted as D1-2 (moiré, white)
按重量份将300份羟基聚酯树脂YE-2080、15份固体双酚A型环氧树脂KD213、19份四甲氧基甲基甘脲、3.0份胺封闭的对甲苯磺酸催化剂AHA6319、6份聚丙烯酸酯流平剂AHA1088P、75份TiO2和1.5份安息香混合3-5min，然后加入到双螺杆试验用挤出机中熔融均化，压片、冷却和碾磨成细粉，过筛通过140目得到基础底粉(D1-2)。By weight, 300 parts of hydroxyl polyester resin YE-2080, 15 parts of solid bisphenol A type epoxy resin KD213, 19 parts of tetramethoxymethyl glycoluril, 3.0 parts of amine-blocked p-toluenesulfonic acid catalyst AHA6319, 6 1 part of polyacrylate leveling agent AHA1088P, 75 parts of TiO 2 and 1.5 parts of benzoin were mixed for 3-5 minutes, then added to a twin-screw test extruder for melting and homogenization, tableted, cooled and ground into fine powder, and sieved A base powder (D1-2) was obtained through 140 mesh.
实施例3制备基础底粉1-3，记为D1-3(龟纹，黑)Embodiment 3 prepares base powder 1-3, denoted as D1-3 (moiré, black)
按重量份将300份羟基聚酯树脂YE-2080、10份固体双酚A型环氧树脂KD213、19份固化剂四甲氧基甲基甘脲、2.0份胺封闭的对甲苯磺酸催化剂AHA6319、6份聚丙烯酸酯流平剂AHA1088P、30份硫酸钡、3.0份炭黑和1.5份安息香混合3-5min，然后加入到双螺杆试验用挤出机中熔融均化，压片、冷却和碾磨成细粉，过筛通过140目得到基础底粉(D1-3)。By weight, 300 parts of hydroxyl polyester resin YE-2080, 10 parts of solid bisphenol A type epoxy resin KD213, 19 parts of curing agent tetramethoxymethyl glycoluril, 2.0 parts of amine-blocked p-toluenesulfonic acid catalyst AHA6319 , 6 parts of polyacrylate leveling agent AHA1088P, 30 parts of barium sulfate, 3.0 parts of carbon black and 1.5 parts of benzoin were mixed for 3-5 minutes, then added to a twin-screw test extruder for melting and homogenization, tableting, cooling and grinding Grind into a fine powder, and sieve through a 140 mesh to obtain a base powder (D1-3).
实施例4制备干粉添加剂1-1，记为A1-1(高光平面)Example 4 Preparation of dry powder additive 1-1, denoted as A1-1 (high-gloss plane)
按重量份将300份羟基聚酯树脂P550、19份四甲氧基甲基甘脲、1.5份N-(甲磺酰基)-对-甲苯基磺酰胺RD1218、6份聚丙烯酸酯流平剂AHA1088P、100份TiO2、75份硫酸钡、1.5份安息香和1.0份表面性能改性剂WH999混合3-5min，然后加入到双螺杆试验用挤出机中熔融均化，压片、冷却和碾磨成细粉，过筛通过160目得到干混添加剂(A1-1)。By weight, 300 parts of hydroxyl polyester resin P550, 19 parts of tetramethoxymethyl glycoluril, 1.5 parts of N-(methylsulfonyl)-p-tolylsulfonamide RD1218, 6 parts of polyacrylate leveling agent AHA1088P , 100 parts of TiO 2 , 75 parts of barium sulfate, 1.5 parts of benzoin and 1.0 part of surface property modifier WH999 were mixed for 3-5 minutes, then added to a twin-screw test extruder for melting and homogenization, tableting, cooling and milling into a fine powder, and sieved through a 160 mesh to obtain a dry blend additive (A1-1).
作为对比验证，将干混添加剂(A1-1)静电喷涂在脱脂冷轧钢板上，200℃/15min固化。显示出平整高光泽的表面，PCI流平6级，光泽97.8％，正冲50Kgcm。As a comparative verification, the dry-blended additive (A1-1) was electrostatically sprayed on a degreased cold-rolled steel plate, and cured at 200°C/15min. It shows a smooth and high-gloss surface, PCI level 6, gloss 97.8%, and positive impact 50Kgcm.
实施例5制备粉末涂料1-1，记为例1-1Embodiment 5 prepares powder coating 1-1, record example 1-1
向100g基础底粉(D1-1)中加入2g的干混添加剂(A1-1)混合均匀得到粉末涂料(例1-1)。Add 2g of dry blend additive (A1-1) to 100g of base powder (D1-1) and mix evenly to obtain a powder coating (Example 1-1).
静电喷涂在脱脂冷轧钢板上，200℃/15min固化。然后按如下试验方法进行测试，具体结果如下表所示。Electrostatic spraying on degreased cold-rolled steel plate, curing at 200℃/15min. Then test according to the following test method, the specific results are shown in the table below.
实施例6制备粉末涂料2-1，记为例2-1Embodiment 6 prepares powder coating 2-1, record example 2-1
操作与实施例6相同，其中基础底粉为(D1-2)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-2). The specific mixing ratio and test results are shown in the table below.
实施例7制备粉末涂料3-1，记为例3-1Embodiment 7 prepares powder coating 3-1, writes down as example 3-1
操作与实施例6相同，其中基础底粉为(D1-3)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-3). The specific mixing ratio and test results are shown in the table below.
实施例8制备粉末涂料3-2，记为例3-2Embodiment 8 prepares powder coating 3-2, writes down as example 3-2
操作与实施例6相同，其中基础底粉为(D1-3)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-3). The specific mixing ratio and test results are shown in the table below.
实施例9制备粉末涂料3-3，记为例3-3Embodiment 9 prepares powder coating 3-3, writes down as example 3-3
操作与实施例6相同，其中基础底粉为(D1-3)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-3). The specific mixing ratio and test results are shown in the table below.
实施例10制备粉末涂料3-4，记为例3-4Embodiment 10 prepares powder coating 3-4, writes down as example 3-4
操作与实施例6相同，其中基础底粉为(D1-3)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-3). The specific mixing ratio and test results are shown in the table below.
比较例3-0制备粉末涂料3-0，记为例3-0Comparative example 3-0 prepares powder coating 3-0, writes down as example 3-0
操作与实施例6相同，其中基础底粉为(D1-3)。其具体的混合比例和测试结果如下表所示。The operation is the same as in Example 6, wherein the base powder is (D1-3). The specific mixing ratio and test results are shown in the table below.
由上表可见：采用本发明所得干混添加剂可以稳定地实现所期望得到纹理，其机械性能不会下降。一般来说，随着干混添加剂用量的提高，纹理会向小的方向转变。而作为对比，其比较例3-0采用类似于US5447751所公开的实例，结果龟纹非常小，而且纹路出现不连续的断头，其机械性能也完全不能接受。It can be seen from the above table that the desired texture can be stably achieved by using the dry blend additive obtained in the present invention, and its mechanical properties will not decrease. In general, as the level of dry blend additive increases, the texture will shift to a smaller direction. As a comparison, its comparative example 3-0 adopts an example similar to that disclosed in US5447751. As a result, the moiré is very small, and discontinuous broken ends appear in the lines, and its mechanical properties are completely unacceptable.
比较例4-1Comparative example 4-1
向100g基础底粉(D1-1)中加入0.5g浮花剂WHCC(黄山惠久粉末材料有限公司)混合均匀得到比较例4-1。Add 0.5 g of floating agent WHCC (Huangshan Huijiu Powder Material Co., Ltd.) to 100 g of foundation powder (D1-1) and mix evenly to obtain Comparative Example 4-1.
静电喷涂在脱脂冷轧钢板上，200℃/15min固化。然后按如上试验方法进行测试，具体结果如下表所示。Electrostatic spraying on degreased cold-rolled steel plate, curing at 200℃/15min. Then test according to the above test method, the specific results are shown in the table below.
比较例4-2Comparative example 4-2
操作与比较例4-1相同，其中基础底粉改为(D1-3)。具体结果如下表所示。The operation is the same as that of Comparative Example 4-1, wherein the base powder is changed to (D1-3). The specific results are shown in the table below.
比较例5-1Comparative example 5-1
向100g基础底粉(D1-1)中加入0.5g醛酮树脂HS-A81(长沙倡泰实业有限公司)混合均匀得到比较例5-1。Add 0.5 g of aldehyde and ketone resin HS-A81 (Changsha Changtai Industrial Co., Ltd.) to 100 g of foundation powder (D1-1) and mix evenly to obtain Comparative Example 5-1.
静电喷涂在脱脂冷轧钢板上，200℃/15min固化。然后按如上试验方法进行测试，具体结果如下表所示。Electrostatic spraying on degreased cold-rolled steel plate, curing at 200℃/15min. Then test according to the above test method, the specific results are shown in the table below.
比较例5-2Comparative example 5-2
操作与比较例5-1相同，其中基础底粉改为(D1-3)。具体结果如下表所示。The operation is the same as that of Comparative Example 5-1, wherein the base powder is changed to (D1-3). The specific results are shown in the table below.
比较例4-1中，向基础底粉D1-1中添加浮花剂WHCC后图案变得相对油润和稳定，图案没有发生明显的改变，也不能得到所期望的蛇皮纹；比较例4-2中，向基础底粉D1-3中添加浮花剂WHCC，得到的是非常细小的龟纹；而比较例5-1和5-2中，通过添加醛酮树脂HS-A81，会改变原配方的纹理图案，其龟纹甚至还原成标准的皱纹，这是出乎意料的。In Comparative Example 4-1, after adding the embossing agent WHCC to the base powder D1-1, the pattern became relatively oily and stable, and the pattern did not change significantly, and the desired snakeskin pattern could not be obtained; Comparative Example 4 In -2, the embossing agent WHCC is added to the base powder D1-3, and very fine moiré is obtained; while in comparative examples 5-1 and 5-2, by adding aldehyde and ketone resin HS-A81, it will change The texture pattern of the original formula, its moiré even reverts to standard wrinkles, which is unexpected.
本发明试样按如下方法测定：Sample of the present invention is measured as follows:
1.涂膜厚度1. Coating thickness
用磁性厚度测定仪(度测定仪德国Automation Dr.Nix GmbH公司的QNix4500)直接测得。It is directly measured with a magnetic thickness measuring instrument (QNix4500 from Automation Dr. Nix GmbH, Germany).
2.外观2. Appearance
用肉眼观察：表面平整无明显缺陷的记为○，有轻微缺陷记为△，有明显缺陷计为×。Observe with naked eyes: the surface is smooth without obvious defects, marked as ○, with slight defects, marked as △, and with obvious defects, marked as ×.
3.光泽3. Gloss
按GB/T1743-89标准进行，60°的反射率，采用德国BYK公司的Micro-gloss60°4442直接测得。According to GB/T1743-89 standard, the reflectivity of 60° is directly measured by Micro-gloss60°4442 of BYK Company in Germany.
4.冲击强度4. Impact strength
按GB/T1732-88标准进行，用锤式耐冲击测定仪进行。其中50Kgcm正反冲通过标为50+，正冲通过标为50，依此类推。According to the GB/T1732-88 standard, it is carried out with a hammer impact resistance tester. Among them, the pass of 50Kgcm forward and recoil is marked as 50+, the pass of forward recoil is marked as 50, and so on.
5.流平5. Leveling
用肉眼观察进行PCI分级，其中10为最好，0为最差。PCI was graded visually, with 10 being the best and 0 being the worst.
6.附着力6. Adhesion
按GB/T9286-1998标准进行，级别划分6个等级，0为最好，5最差。According to the GB/T9286-1998 standard, the grade is divided into 6 grades, 0 is the best and 5 is the worst.
7.色差7. Chromatic aberration
用BGD-551型色差仪直接测得，用△E表示。△E＜5的表示好，记为○，5＜△E＜10之间表示一般，记为△，△E＞10的表示差，计为×。Measured directly with BGD-551 colorimeter, represented by △E. △E<5 means good, marked as ○, 5<△E<10 means fair, marked as △, △E>10 means poor, scored as ×.
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any person familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.
Claims (10)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154305A (en) * | 2019-12-24 | 2020-05-15 | 广东合邦新型粉末涂料科技股份有限公司 | Base powder and external texture agent wrinkle powder and preparation and spraying method thereof |
| CN112745709A (en) * | 2020-01-13 | 2021-05-04 | 万辉(广州)高新材料有限公司 | Art powder coating with snakeskin effect and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1079763A (en) * | 1992-04-10 | 1993-12-22 | 莫顿国际股份有限公司 | Form the powder coating of wrinkle surface layer |
| US5573828A (en) * | 1994-03-08 | 1996-11-12 | Morton International, Inc. | Wrinkle finish powder coating |
| CN106519924A (en) * | 2016-10-28 | 2017-03-22 | 福建万安实业集团有限公司 | Turtle shell appearance imitated type powder paint |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079763A (en) * | 1992-04-10 | 1993-12-22 | 莫顿国际股份有限公司 | Form the powder coating of wrinkle surface layer |
| US5573828A (en) * | 1994-03-08 | 1996-11-12 | Morton International, Inc. | Wrinkle finish powder coating |
| CN106519924A (en) * | 2016-10-28 | 2017-03-22 | 福建万安实业集团有限公司 | Turtle shell appearance imitated type powder paint |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154305A (en) * | 2019-12-24 | 2020-05-15 | 广东合邦新型粉末涂料科技股份有限公司 | Base powder and external texture agent wrinkle powder and preparation and spraying method thereof |
| CN112745709A (en) * | 2020-01-13 | 2021-05-04 | 万辉(广州)高新材料有限公司 | Art powder coating with snakeskin effect and preparation method thereof |
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