CN108997559A - 一种哑光型水性聚氨酯材料及其制备方法 - Google Patents
一种哑光型水性聚氨酯材料及其制备方法 Download PDFInfo
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- CN108997559A CN108997559A CN201810578170.6A CN201810578170A CN108997559A CN 108997559 A CN108997559 A CN 108997559A CN 201810578170 A CN201810578170 A CN 201810578170A CN 108997559 A CN108997559 A CN 108997559A
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- dumb light
- light type
- type water
- base polyurethane
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004970 Chain extender Substances 0.000 claims abstract description 20
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 20
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- 150000003077 polyols Chemical class 0.000 claims abstract description 17
- -1 small molecule hydrophilic compounds Chemical class 0.000 claims abstract description 16
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
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- 150000005215 alkyl ethers Chemical class 0.000 claims 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/6633—Compounds of group C08G18/42
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/72—Polyisocyanates or polyisothiocyanates
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
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- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
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Abstract
本发明公开了一种哑光型水性聚氨酯材料及制备方法，涉及水性聚氨酯材料技术领域，固含量30％‑40％，由如下重量份数的原料制成：二异氰酸酯20‑30份、大分子多元醇40‑50份、小分子扩链剂1.2‑3份、小分子亲水化合物1‑2.5份、催化剂0.2‑0.4份、阴离子乳化剂0.7‑1.4份、去离子水131‑170份、中和剂0.7‑2份、多元胺扩链剂3‑5份。本发明制备的哑光型水性聚氨酯材料不需要外加消光剂，避免“发白发黄”现象，安全环保，乳液性能稳定；并且具有优异的机械性能和耐摩擦、耐水性能，同时具备哑光性能，可广泛应用于水性涂料。
Description
技术领域：
本发明涉及水性聚氨酯材料技术领域，具体涉及一种哑光型水性聚氨酯材料及其制备方法。
背景技术：
水性涂料中最具代表性的是水性聚氨酯涂料，它不含或含很少量的有机溶剂，粒径小，具有较好的分散稳定性，不仅保留了传统的溶剂型聚氨酯涂料的一些优良性能，而且还具有成膜温度低、附着力强、耐磨性好、硬度大以及耐化学品、耐候性好等优越性能。
目前以哑光\消光为代表的水性哑光产品逐渐受到人们的欢迎，而制备水性哑光漆普遍采用物理添加消光剂的方法，制成的哑光涂层的脆性差，以及加入消光剂引起的涂料性能下降如沉淀，涂料的贮存稳定性差、涂层耐抛光性差、涂膜的透明性降低等。
为了克服数上述问题，通过不添加哑光\消光剂的方法，来合成具有哑光效果的水性聚氨酯材料。本体哑光聚氨酯材料，一方面可以保留聚氨酯的优良性能，另一方面通过对聚氨酯设计的改变，可以使合成材料更加均匀稳定，喷涂施工方便、涂层均匀，达到更加优异的哑光效果。
专利CN201510416194.8公开了一种哑光型水性聚氨酯树脂复合乳液的合成方法，在水性聚氨酯中通过化学键接入硅烷偶联剂改性气相二氧化硅，获得较强的稳定性和优良的哑光效果，在涂饰后成膜具有较好的通透度，在达到哑光效果的同时不会对皮胚颜色造成影响，避免了外加消光剂容易出现的“发白、发灰”现象。气相二氧化硅属于本领域常用消光剂，该专利通过硅烷偶联剂制得改性气相二氧化硅，并利用化学键将改性气相二氧化硅连接到聚氨酯分子结构上从而避免常规外加气相二氧化硅存在的技术问题。
发明内容：
本发明所要解决的技术问题在于提供一种作为涂料时贮存稳定性好且所形成涂层使用性能优异的哑光型水性聚氨酯材料及其制备方法。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种哑光型水性聚氨酯材料，固含量30％-40％，由如下重量份数的原料制成：
二异氰酸酯20-30份、大分子多元醇40-50份、小分子扩链剂1.2-3份、小分子亲水化合物1-2.5份、催化剂0.2-0.4份、阴离子乳化剂0.7-1.4份、去离子水131-170份、中和剂0.7-2份、多元胺扩链剂3-5份。
所述二异氰酸酯选自甲苯二异氰酸酯TDI、异佛尔酮二异氰酸酯IPDI、二苯基甲烷二异氰酸酯MDI、1,6-己二异氰酸酯HDI、苯二亚甲基二异氰酸酯XDI、萘-1,5-二异氰酸酯NDI、多亚甲基多苯基异氰酸酯PAPI中的一种或两种。
所述大分子多元醇选自聚己内酯多元醇PCL、聚碳酸酯多元醇PCD、聚四氢呋喃醚多元醇PTMG、聚乙二醇PEG、聚环氧丙烷多元醇PPG中的一种或几种。
所述小分子扩链剂选自乙二醇、一缩二乙二醇、1,4-丁二醇、2,3-丁二醇、2-甲基-1,3丙二醇、1,6-己二醇、新戊二醇、二甘醇、甘油、三羟甲基丙烷、二羟甲基环己烷中的一种或两种。
所述小分子亲水化合物选自二羟甲基丙酸、二羟甲基丁酸、二羟甲基戊酸、二羟甲基辛酸中的一种或几种。
所述催化剂选自二月桂酸二丁基锡、异辛酸铋、新癸酸铋、环烷酸铋、月桂酸铋中的一种。
所述阴离子乳化剂选自十二烷基磺酸钠、脂肪醇聚氧乙烯醚硫酸钠、脂肪醇聚氧乙烯醚磺酸钠、烯丙氧基羟丙基磺酸钠、乙烯基烷基酯磺酸钠中的一种或两种。
所述中和剂选自三乙胺、叔丁胺、三乙醇胺、二乙醇胺中的一种。
所述多元胺扩链剂选自二乙烯三胺、三乙烯四胺、四乙烯五胺、异氟尔酮二胺、水合肼中的一种或几种。
上述哑光型水性聚氨酯材料的制备方法包括以下步骤：
(1)预聚体制备：向四口烧瓶中加入大分子多元醇和小分子扩链剂，搅拌均匀，升温至90-100℃真空脱水1h，降温至60℃，一次性加入二异氰酸酯，再滴加2滴催化剂，搅拌，75℃保温反应2h，然后加入小分子亲水化合物，并滴加1滴催化剂，保温反应2h，降温到50℃以下缓慢滴加中和剂，搅拌均匀，即得水性聚氨酯预聚体；
(2)阴离子乳化剂水溶液制备：取阴离子乳化剂溶解于去离子水中，搅拌均匀，即得阴离子乳化剂水溶液；
(3)预聚体分散和扩链：将水性聚氨酯预聚体快速倒入阴离子乳化剂水溶液中，快速搅拌使预聚体均匀分散于水中，0.5h后加入多元胺扩链剂，搅拌均匀，得到均一、稳定、粒径分布宽的水性聚氨酯乳液。
本发明的有益效果是：
(1)本发明提供的哑光型水性聚氨酯材料通过自乳化和外加乳化剂的方式，使得乳液粒径分布宽，其中自乳化粒径分布在50-150nm，外乳化粒径分布在100-600nm；粒径不同对光的反射不一样，大小粒径均匀分布，乳液在作为水性涂料使用时，由于粒径的差异，成膜后对入射光的反射角度不同，形成光学的不平滑面，肉眼观看膜表面是哑光的。
(3)使用本发明制备的哑光型水性聚氨酯材料不需要外加消光剂，避免“发白发黄”现象，安全环保，乳液性能稳定；并且所制哑光型水性聚氨酯材料具有优异的机械性能和耐摩擦、耐水性能，同时具备哑光性能，可广泛应用于水性涂料。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例1
按照下表称取各原料。
哑光型水性聚氨酯材料的制备：
(1)预聚体制备：向四口烧瓶中加入大分子多元醇和小分子扩链剂，搅拌均匀，升温至90-100℃真空脱水1h，降温至60℃，一次性加入二异氰酸酯，再滴加2滴催化剂，搅拌，75℃保温反应2h，然后加入小分子亲水化合物，并滴加1滴催化剂，保温反应2h，降温到50℃以下缓慢滴加中和剂，搅拌均匀，即得水性聚氨酯预聚体；
(2)阴离子乳化剂水溶液制备：取阴离子乳化剂溶解于去离子水中，搅拌均匀，即得阴离子乳化剂水溶液；
(3)预聚体分散和扩链：将水性聚氨酯预聚体快速倒入阴离子乳化剂水溶液中，快速搅拌使预聚体均匀分散于水中，0.5h后加入多元胺扩链剂，搅拌均匀，得到均一、稳定、粒径分布宽的水性聚氨酯乳液。
实施例2
按照下表称取各原料。
本实施例哑光型水性聚氨酯材料的制备方法同实施例1。
实施例3
按照下表称取各原料。
| 原料 | 用量/份 |
| 二异氰酸酯IPDI | 28 |
| 聚碳酸酯多元醇PCD | 42 |
| 1,4丁二醇BDO | 1.5 |
| 三羟甲基丙烷TMP | 1 |
| 二羟甲基丙酸DMBA | 1.7 |
| 二月桂酸二丁基锡 | 0.3 |
| 乙烯基烷基酯磺酸钠JS-20 | 1.0 |
| 去离子水 | 144 |
| 三乙醇胺 | 1.7 |
| 水合肼 | 3 |
本实施例哑光型水性聚氨酯材料的制备方法同实施例1。
对照例1
以实施例1为基础，设置不外加阴离子乳化剂的对照例1。
按照下表称取各原料。
| 原料 | 用量/份 |
| 二异氰酸酯TDI | 25 |
| 聚四氢呋喃醚多元醇PTMG | 45 |
| 三羟甲基丙烷TMP | 1.4 |
| 二羟甲基丙酸DMPA | 2 |
| 二月桂酸二丁基锡 | 0.3 |
| 去离子水 | 166 |
| 三乙胺 | 1.5 |
| 二乙烯三胺DETA | 3 |
水性聚氨酯材料的制备：
(1)预聚体制备：向四口烧瓶中加入大分子多元醇和小分子扩链剂，搅拌均匀，升温至90-100℃真空脱水1h，降温至60℃，一次性加入二异氰酸酯，再滴加2滴催化剂，搅拌，75℃保温反应2h，然后加入小分子亲水化合物，并滴加1滴催化剂，保温反应2h，降温到50℃以下缓慢滴加中和剂，搅拌均匀，即得水性聚氨酯预聚体；
(2)预聚体分散和扩链：将水性聚氨酯预聚体快速倒入去离子水液中，快速搅拌使预聚体均匀分散于水中，0.5h后加入多元胺扩链剂，搅拌均匀，得到均一、稳定、粒径分布宽的水性聚氨酯乳液。
对照例2
以实施例1为基础，设置不外加阴离子乳化剂但添加消光剂气相二氧化硅的对照例2，消光剂添加量在5％。
按照下表称取除消光剂以外的原料，并计算消光剂用量。
| 原料 | 用量/份 |
| 二异氰酸酯TDI | 25 |
| 聚四氢呋喃醚多元醇PTMG | 45 |
| 三羟甲基丙烷TMP | 1.4 |
| 二羟甲基丙酸DMPA | 2 |
| 二月桂酸二丁基锡 | 0.3 |
| 去离子水 | 166 |
| 三乙胺 | 1.5 |
| 二乙烯三胺DETA | 3 |
哑光型水性聚氨酯材料的制备：
(1)预聚体制备：向四口烧瓶中加入大分子多元醇和小分子扩链剂，搅拌均匀，升温至90-100℃真空脱水1h，降温至60℃，一次性加入二异氰酸酯，再滴加2滴催化剂，搅拌，75℃保温反应2h，然后加入小分子亲水化合物，并滴加1滴催化剂，保温反应2h，降温到50℃以下缓慢滴加中和剂，搅拌均匀，即得水性聚氨酯预聚体；
(2)消光剂水溶液制备：取消光剂分散于去离子水中，搅拌均匀，即得消光剂水溶液；
(3)预聚体分散和扩链：将水性聚氨酯预聚体快速倒入消光剂水溶液中，快速搅拌使预聚体均匀分散于水中，0.5h后加入多元胺扩链剂，搅拌均匀，得到均一、稳定、粒径分布宽的水性聚氨酯乳液。
对照例3
以对照例2为基础，将消光剂添加量设为4％，其余条件不变。
实施例4
分别利用实施例1、实施例2、实施例3、对照例1、对照例2制备水性聚氨酯乳液，测定所制水性聚氨酯乳液的贮存稳定性；并将所制水性聚氨酯乳液通过相同喷涂工艺喷涂于相同材质的同批工件上，涂层厚度5μm，测定所形成涂层的使用性能指标，如表1所示。
表1本发明所制水性聚氨酯乳液的使用性能
| 组别 | 18℃贮存稳定性 | 60°光泽度 | 附着力 | 铅笔硬度 | 25℃耐水性 |
| 实施例1 | ＞12个月 | 11 | 0级 | 2H | ＞7d |
| 实施例2 | ＞12个月 | 11 | 0级 | 2H | ＞7d |
| 实施例3 | ＞12个月 | 10 | 0级 | 2H | ＞7d |
| 对照例1 | 6-12个月 | 15 | 1级 | 1H | ＞7d |
| 对照例2 | ＜6个月 | 19 | 2级 | HB | ＜7d |
| 对照例3 | ＜6个月 | 32 | 2级 | HB | ＜7d |
由表1可知，当消光剂气相二氧化硅的添加量为5％时所制水性聚氨酯乳液形成的涂层才具有哑光效果，但其哑光效果仍不如实施例1-3，并且其涂层的附着力、硬度和耐水性以及乳液的贮存稳定性都不如实施例1-3。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (10)
1.一种哑光型水性聚氨酯材料，其特征在于：固含量30％-40％，由如下重量份数的原料制成：
二异氰酸酯20-30份、大分子多元醇40-50份、小分子扩链剂1.2-3份、小分子亲水化合物1-2.5份、催化剂0.2-0.4份、阴离子乳化剂0.7-1.4份、去离子水131-170份、中和剂0.7-2份、多元胺扩链剂3-5份。
2.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述二异氰酸酯选自甲苯二异氰酸酯TDI、异佛尔酮二异氰酸酯IPDI、二苯基甲烷二异氰酸酯MDI、1,6-己二异氰酸酯HDI、苯二亚甲基二异氰酸酯XDI、萘-1,5-二异氰酸酯NDI、多亚甲基多苯基异氰酸酯PAPI中的一种或两种。
3.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述大分子多元醇选自聚己内酯多元醇PCL、聚碳酸酯多元醇PCD、聚四氢呋喃醚多元醇PTMG、聚乙二醇PEG、聚环氧丙烷多元醇PPG中的一种或几种。
4.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述小分子扩链剂选自乙二醇、一缩二乙二醇、1,4-丁二醇、2,3-丁二醇、2-甲基-1,3丙二醇、1,6-己二醇、新戊二醇、二甘醇、甘油、三羟甲基丙烷、二羟甲基环己烷中的一种或两种。
5.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述小分子亲水化合物选自二羟甲基丙酸、二羟甲基丁酸、二羟甲基戊酸、二羟甲基辛酸中的一种或几种。
6.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述催化剂选自二月桂酸二丁基锡、异辛酸铋、新癸酸铋、环烷酸铋、月桂酸铋中的一种。
7.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述阴离子乳化剂选自十二烷基磺酸钠、脂肪醇聚氧乙烯醚硫酸钠、脂肪醇聚氧乙烯醚磺酸钠、烯丙氧基羟丙基磺酸钠、乙烯基烷基酯磺酸钠中的一种或两种。
8.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述中和剂选自三乙胺、叔丁胺、三乙醇胺、二乙醇胺中的一种。
9.根据权利要求1所述的哑光型水性聚氨酯材料，其特征在于：所述多元胺扩链剂选自二乙烯三胺、三乙烯四胺、四乙烯五胺、异氟尔酮二胺、水合肼中的一种或几种。
10.根据权利要求1-9中任一项哑光型水性聚氨酯材料的制备方法，其特征在于，包括以下步骤：
(1)预聚体制备：向四口烧瓶中加入大分子多元醇和小分子扩链剂，搅拌均匀，升温至90-100℃真空脱水1h，降温至60℃，一次性加入二异氰酸酯，再滴加2滴催化剂，搅拌，75℃保温反应2h，然后加入小分子亲水化合物，并滴加1滴催化剂，保温反应2h，降温到50℃以下缓慢滴加中和剂，搅拌均匀，即得水性聚氨酯预聚体；
(2)阴离子乳化剂水溶液制备：取阴离子乳化剂溶解于去离子水中，搅拌均匀，即得阴离子乳化剂水溶液；
(3)预聚体分散和扩链：将水性聚氨酯预聚体快速倒入阴离子乳化剂水溶液中，快速搅拌使预聚体均匀分散于水中，0.5h后加入多元胺扩链剂，搅拌均匀，得到均一、稳定、粒径分布宽的水性聚氨酯乳液。
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