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WO1997024392A1 - Melange-mere contenant du dioxyde de titane - Google Patents

Melange-mere contenant du dioxyde de titane Download PDF

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Publication number
WO1997024392A1
WO1997024392A1 PCT/JP1996/003845 JP9603845W WO9724392A1 WO 1997024392 A1 WO1997024392 A1 WO 1997024392A1 JP 9603845 W JP9603845 W JP 9603845W WO 9724392 A1 WO9724392 A1 WO 9724392A1
Authority
WO
WIPO (PCT)
Prior art keywords
weight
treated
titanium oxide
terms
calcium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP1996/003845
Other languages
English (en)
Japanese (ja)
Inventor
Susumu Miyasita
Noburu Sakuma
Masaru Hosokawa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Artience Co Ltd
Original Assignee
Toyo Ink Mfg Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Toyo Ink Mfg Co Ltd filed Critical Toyo Ink Mfg Co Ltd
Priority to AU12093/97A priority Critical patent/AU1209397A/en
Priority to JP52419697A priority patent/JP3215979B2/ja
Publication of WO1997024392A1 publication Critical patent/WO1997024392A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • 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

Definitions

  • the present invention relates to a masterbatch used for coloring and processing a thermoplastic resin, and more particularly, to a masterpatch which is excellent in whiteness, heat-resistant, light-resistant, and weather-resistant.
  • the present invention relates to a resin molded product which is excellent in high-speed high-temperature workability, is uniform and has excellent concealing properties, and particularly relates to a master batch suitably used for a contact extrusion lamination film. Background technology
  • the coloring composition used for coloring and molding thermoplastic resin includes a powdery dry color in which a pigment and a dispersant are mixed, and a liquid in which the pigment is dispersed in a liquid at room temperature. Masterbatch in the form of pellets, flakes, or pellets by dispersing a pigment in a high concentration in a solid resin at room temperature, such as dyed color or pasted color. Above all, master batches are often used because they are easy to handle and preserve the working environment during use.
  • a thermoplastic resin containing titanium dioxide has been used as a master batch for white color. This titanium oxide is used in a large amount as a white pigment for resin coloring because of its excellent whiteness, high concealing property, and high coloring power. In terms of whiteness, the anatase type is excellent, and the rutile type has a yellow tint. Therefore, the anatase type is generally suitably used for applications requiring whiteness.
  • the whiteness of the molded product is impaired by heat during manufacturing, or the whiteness of the molded product is reduced by light after molding. There were problems such as deterioration over time.
  • titanium oxide is inherently hydrophilic, and is subjected to a surface treatment with an inorganic or organic substance to improve weather resistance, hydrophobicity, and dispersibility.
  • titanium oxide treated with a polyol-based or polysiloxane-based surface treatment agent there is titanium oxide treated with a polyol-based or polysiloxane-based surface treatment agent, but titanium oxide surface-treated with a polyol-based surface treatment agent has good dispersibility but a small effect of hydrophobization. Therefore, a large amount of water is adsorbed, and the master batch using the surface-treated titanium oxide and the thermoplastic resin also has a small hydrophobicity, and thus contains a large amount of water.
  • Titanium oxide that has been surface-treated with a polysiloxane-based treating agent has a favorable effect of beading, but because of the weak chemical bonding force between the titanium oxide surface and the treating agent, such surface treatment oxidation
  • the surface treatment agent is peeled off due to kneading conditions and extrusion conditions during manufacturing, resulting in uneven dispersion of titanium oxide in the master batch. Problems such as an increase in water content due to a decrease in hydrophobicity have occurred.
  • the present invention has solved the above-mentioned problems in the conventional masterbatch, and has higher whiteness than the conventional one, and is used for heat discoloration resistance, weather discoloration resistance, and light discoloration resistance, and is rich in dispersibility and hydrophobicity. It is intended to provide a titanium oxide-containing masterbatch containing less moisture generated during high-temperature processing. Disclosure of the invention
  • the present invention enhances high whiteness and color stability by containing 0.02 to 1.0% by weight of aluminum-aluminum (A1), and is excellent in heat discoloration resistance, weather discoloration resistance, and light discoloration resistance.
  • the present invention also relates to a masterbatch containing titanium dioxide and a thermoplastic resin, which have been improved in dispersibility and hydrophobicity by performing a surface treatment. Specifically, titanium dioxide treated by the following method is used.
  • Titanium oxide treated with 0.1 to 0.3% by weight of aluminate (5) Calcium oxide 0.01 to 0.5% by weight of calcium salt and silica equivalent of 0.01 to 0.3% by weight of calcium (6) 0.01 to 0.5% by weight of calcium salt in terms of calcium oxide and 0.05 to 3.0 weight Of the silane coupling agent and in terms of silica 0.0 1 to 0.3 wt% of the treated titanium oxide and Kei salt.
  • oxide mug Neshiumu terms 0.0 1 to 0.5 wt 0/6 magnesium salts may be used titanium oxide treated.
  • titanium oxide treated with 0.05 to 3.0% by weight of a silane coupling agent without using a calcium salt and magnesium, or 0.05 to 3.0% by weight of a silane coupling agent and 0 in terms of alumina titanium oxide treated with 0.05 to 3.0% by weight of a silane coupling agent without using a calcium salt and magnesium, or 0.05 to 3.0% by weight of a silane coupling agent and 0 in terms of alumina.
  • Titanium oxide treated with 0.1 to 0.3% by weight of aluminate clay, or 0.05 to 3.0% by weight of silane coupling agent and 0.01 to 0.3% by weight of silicic acid in terms of silicic acid Titanium oxide treated with a salt may be used.
  • the magnesium salt is used in place of the calcium salt, and the silicate is used in place of the aluminate clay.
  • the treatment is performed by adding a calcium salt / magnesium salt and then adding an aluminate or silicate. After that, it is preferable that the material is treated by adding a silane coupling agent.
  • the calcium salt calcium chloride, calcium bromide, calcium iodide or calcium nitrate can be used.
  • magnesium salt agglomerated magnesium, magnesium bromide, magnesium iodide or magnesium sulfate can be used.
  • silane coupling agent methyltrimethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, vinyltriethoxysilane, phenyltrialkoxysilane, or dialkyldialkoxysilane can be used.
  • the above-mentioned A1 contained in the titanium dioxide is contained in the crystal, and is preferably an anatase type titanium oxide.
  • the masterbatch of the present invention containing the above-mentioned titanium dioxide has a water content of 1200 ppm or less which can be volatilized in 280 to 35, and is suitable as a masterbatch for an extruded laminate film. It is. BEST MODE FOR CARRYING OUT THE INVENTION
  • the masterbatch of the present invention suppresses and prevents discoloration due to heat by using titanium oxide containing A1, increases whiteness, and specifies the titanium oxide containing A1! : Surface treatment using a silane rubbing agent or a specific amount of calcium salt to reduce the amount of volatile water and improve dispersibility, hydrophobicity, concealment, light discoloration resistance, weather discoloration resistance, etc. Things.
  • a master batch containing titanium oxide containing Nb, Ta, and W in the crystal is used in fields requiring high-temperature processing of 280 to 350 ⁇ , for example, in the field of melt extrusion lamination. At low temperature The blue and black of the colored molded product becomes remarkable as compared with the case where it is used.
  • the masterbatch containing titanium dioxide in which Nb, Ta, and W in this crystal were replaced with A1 prevents discoloration during high-temperature processing of 280 to 350, and is therefore melt-extruded.
  • a molded article such as a film
  • the amount of A 1 contained in the titanium dioxide crystal may be an amount capable of replacing the amount of the metal Nb, Ta, W present as an impurity taken into the titanium dioxide crystal as an ion.
  • the content is 0.02 to 1.0% by weight, and preferably 0.3% by weight or less. If the content is less than 0.02% by weight, no effect can be obtained in fast discoloration resistance, light discoloration resistance, and weather discoloration resistance. On the other hand, if the content exceeds 1.0% by weight, free A1 which does not enter the crystal is mixed in an oxide state, which is not preferable.
  • the titanium dioxide containing A 1 in the crystal is obtained by adding a water-soluble aluminum compound such as aluminum sulfate to a slurry of hydrated titanium dioxide obtained by the sulfuric acid method, drying the mixed slurry, and drying the mixed slurry at 850 to 110. Obtained by a wet process of firing at 0. Alternatively, it can also be manufactured by a dry manufacturing method in which alumina powder is added to titanium dioxide powder, and the mixed powder is fired at the above temperature.
  • the masterbatch of the present invention contains the above-mentioned A1-containing titanium dioxide which has been subjected to a surface treatment using a calcium clay or magnesium salt, a silane coupling agent, an aluminate clay or a silicate.
  • the silane coupling agent used in the present invention is used for hydrophobizing the A1-containing titanium oxide and improving dispersibility, and has a structure represented by the following general formulas (1) to (4).
  • R divalent aliphatic chain, divalent aromatic spear
  • organic functional groups of the above general formula those having a methyl group or an amino group are preferable, and in particular, dialkyl Dialkoxysilane is preferred, and dimethyldimethoxysilane is particularly preferred.
  • the use amount of the silane coupling agent is suitably 0.05 to 3.0% by weight, preferably 0.05 to: 1.0% by weight, more preferably 0.1 to 0.5% by weight, and most preferably 0.1. ⁇ 0.3% by weight.
  • the amount of the silane coupling agent exceeds 3.0% by weight, a slip occurs when the master batch is extruded, and the ejection of the material becomes unstable, so that the colorant composition cannot be manufactured stably.
  • the film thickness becomes non-uniform or the film breaks, making molding impossible.
  • the amount used is less than 0.05% by weight, the effect of water-hydrophobicity on the A1-containing titanium oxide is small, and water adsorption over time after the production of the master batch increases. Therefore, the same problem as the conventional one occurs.
  • the calcium salt or the magnesium salt used in the present invention reacts with the hydroxyl group on the surface of the A1-containing titanium oxide to fix the hydroxyl group and hydrophobize the A1-containing titanium oxide in the same manner as the silane coupling agent. It is used for
  • Examples of the calcium salt or magnesium salt include calcium chloride, calcium bromide, calcium iodide, calcium sulfate, magnesium chloride, magnesium bromide, magnesium iodide, magnesium sulfate and the like. These are used in an amount of 0.01 to 0.5% by weight in terms of calcium oxide or magnesium oxide. If the amount used is less than 0.01% by weight, the effect of sessification is insufficient, and if it is used in excess of 0.5% by weight, the effect of hydrophobization hardly changes.
  • a treatment with a silane coupling agent, a treatment with a calcium salt or the like, or a combination of a treatment with a silane coupling agent and a treatment with a calcium salt or the like, and further, an aluminate such as sodium aluminate or a silicate are used.
  • treatments such as alumina and sily can be applied together. That is, after treating the A1-containing titanium oxide with an aluminate, a silicate, or the like, it may be treated with a silane coupling agent, or after treating the A1-containing titanium oxide with a calcium salt or the like, and then treating the aluminum oxide with an aluminum salt.
  • A1 containing titanium oxide may be treated with a calcium salt, etc., then treated with an aluminate, a silicate, etc., and further treated with a silane coupling agent. May be.
  • Alumina, silica, and the like generally contain water of crystallization or are hydrated, and although it is preferable to reduce it as much as possible from the viewpoint of reducing water content, it has the effect of increasing the shielding power. Yes, in areas where concealment is strongly required.
  • the amount used is preferably as small as possible, and is suitably 0.3 wt.% Or less, and preferably 0.2 wt.% Or less based on titanium oxide. If the amount used exceeds 0.3% by weight, the water content is low and troubles during processing are likely to occur.
  • Alumina is preferred over silica in that it is easy to separate.
  • the AI-containing surface-treated titanium dioxide preferably has an average particle size of 0.01 to 1.0 ⁇ m.
  • the crystal type may be either rutile type or anatase type, but anatase type is particularly preferable from the viewpoint of whiteness.
  • the dispersion of the titanium oxide is extremely poor, and the coloring resin molded product has Agglomerates are generated and clogging of the screen mesh of the molding machine is caused.
  • thermoplastic resin used in the present invention examples include polyolefin resins, polyester resins, polystyrene resins, and nylon resins, which are common thermoplastic resins.
  • polyolefin resin and polyester resin are listed.
  • Polyolefin resin is particularly preferable for the melt extrusion lamination to the paper base, and polyethylene resin is particularly preferable.
  • a polyester resin is particularly preferable, and among them, polyethylene terephthalate is preferable.
  • the masterbatch of the present invention may contain the surface-treated titanium oxide and the thermoplastic resin in a ratio of 2-8 to 8-2, preferably 5Z5-7-7, more preferably 6-4. ⁇ 7 Z3.
  • the masterbatch of the present invention composed of the above components has a volatile water content of less than 120 O ppB at 280 to 350, preferably less than 80 O ppai, more preferably less than 300 O ppai. With a volatile water content of less than 60 O ppm.
  • the above-described various problems occur when an attempt is made to obtain a colored resin molded product using a master batch and a thermoplastic resin having a volatile water content of more than 1200 ⁇ within the above temperature range.
  • the moisture is the amount of moisture generated at a predetermined temperature under a nitrogen atmosphere using a Karl Fischer moisture system.
  • the masterbatch of the present invention may contain, if necessary, other known additives such as other pigments and ultraviolet absorbers, as long as the effect is not impaired, other than the above components.
  • other known additives such as other pigments and ultraviolet absorbers, as long as the effect is not impaired, other than the above components.
  • the configuration examples of the masterbatch of the present invention described above are shown in the following table.
  • the above master batch 67 weight ⁇ 1 ⁇ 2, low density polyethylene (specific gravity 0.918, MFR 4. Og / lOain.) 33 3% by weight is blended and molded using a T-die film molding machine (Toyo Seiki Co., Ltd.) At a temperature of 200 ° C, 280 °, 300 °, and 350 °, T-die films having a film thickness of 30 / iB were prepared, and the film forming properties (appearance), hue, etc. were evaluated. .
  • the whiteness and hue of a 30-a-thick T-die film extruded and prepared at each temperature by the above method were measured with a colorimeter (manufactured by Kurabo Industries, Ltd.).
  • Hue and whiteness are Industry standard (JIS Z-8715). The larger the whiteness W is, the whiter the color is, and the smaller the hue b is, the more bluish it is.
  • Thermally stable Specifically, 0.10 or less is appropriate, and 0.05 or less is preferable.
  • the masterbatch of the present invention using titanium dioxide containing A1 in the crystal has a hue difference ⁇ b of 0.05 or less in all cases, and the mature stability is extremely convenient. Have been.
  • the hue difference ⁇ b was at least significantly larger than 0.1 and the thermal stability was significantly low.
  • the masterbatch of the present invention using surface-treated titanium dioxide has good dispersibility and has a significantly small amount of volatile water.
  • the masterbatch of Comparative Example (No. 5) using titanium dioxide without surface treatment is inferior in dispersibility, has a remarkably large amount of volatile water, and is inferior in film formability.
  • a titanium oxide-containing masterbatch having a higher degree of whiteness, excellent heat discoloration resistance, light discoloration resistance, and weather discoloration resistance, rich in dispersibility and hydrophobicity, and low in moisture generated during high-temperature processing.
  • This masterbatch has a small amount of volatile moisture under high-temperature treatment, and does not cause inconveniences such as poor dispersion in an extruder and lacing, so that a high-quality colored resin product can be produced.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention porte sur un mélange-mère comprenant une résine thermoplastique contenant du dioxyde de titane. Ce dernier qui contient entre 0,02 et 1,00 % d'aluminium a subi un traitement de surface à l'aide d'un agent spécifique. Le mélange-mère présente de ce fait une blancheur élevée et une excellente stabilité thermique et une large réduction du contenu de vapeur s'évaporant lors du traitement à haute température.
PCT/JP1996/003845 1995-12-27 1996-12-27 Melange-mere contenant du dioxyde de titane Ceased WO1997024392A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU12093/97A AU1209397A (en) 1995-12-27 1996-12-27 Masterbatch containing titanium oxide
JP52419697A JP3215979B2 (ja) 1995-12-27 1996-12-27 酸化チタン含有マスターバッチ

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP34066095 1995-12-27
JP7/340660 1995-12-27
JP8/212281 1996-08-12
JP21228196 1996-08-12

Publications (1)

Publication Number Publication Date
WO1997024392A1 true WO1997024392A1 (fr) 1997-07-10

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Family Applications (1)

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PCT/JP1996/003845 Ceased WO1997024392A1 (fr) 1995-12-27 1996-12-27 Melange-mere contenant du dioxyde de titane

Country Status (3)

Country Link
JP (1) JP3215979B2 (fr)
AU (1) AU1209397A (fr)
WO (1) WO1997024392A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999044826A1 (fr) * 1998-03-03 1999-09-10 Qpf, Llc Film de polypropylene a orientation biaxiale contenant des particules de metal ou d'oxyde metallique
JP2007055875A (ja) * 2005-08-26 2007-03-08 Tayca Corp 酸化チタン水性スラリーの濾過速度を改善する方法およびこの方法から得られた酸化チタン粉体
JP2007224180A (ja) * 2006-02-24 2007-09-06 Toyo Ink Mfg Co Ltd 着色樹脂組成物
JP2009518329A (ja) * 2005-12-09 2009-05-07 ディーエスエム アイピー アセッツ ビー．ブイ． 改質された二酸化チタン粒子を含む新規な化粧料または皮膚科用組成物
CN106009470A (zh) * 2016-06-24 2016-10-12 深圳市同益实业股份有限公司 树脂材料及其制备方法
CN106633852A (zh) * 2016-12-02 2017-05-10 长兴天晟能源科技有限公司 一种提高尼龙66树脂湿稳定性的母粒

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54101795A (en) * 1978-01-30 1979-08-10 Toyo Soda Mfg Co Ltd Hydrophobic rendering method for oxide fine powder
JPS6243457A (ja) * 1985-06-13 1987-02-25 ロ−ヌ−プ−ラン　フイブル ポリアミド艶消し用マスタ−バツチ
JPH0350120A (ja) * 1989-07-18 1991-03-04 Ishihara Sangyo Kaisha Ltd 二酸化チタン顔料粉末の製造方法
JPH05221640A (ja) * 1992-02-17 1993-08-31 Shin Etsu Chem Co Ltd 疎水性酸化チタン微粒子の製造方法
JPH0753216A (ja) * 1993-08-17 1995-02-28 Titan Kogyo Kk 二酸化チタン微粉末およびその製造方法
JPH07138020A (ja) * 1993-11-12 1995-05-30 High Frequency Heattreat Co Ltd 超微粒子二酸化チタン複合化酸化物及びその製造方法
JPH07504932A (ja) * 1992-03-26 1995-06-01 メルク　パテント　ゲゼルシャフト　ミット　ベシュレンクテル　ハフトング 薄片状着色顔料およびその製造方法
JPH07315839A (ja) * 1993-11-24 1995-12-05 Kerr Mcgee Chem Corp 二酸化チタン生成物及びその製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54101795A (en) * 1978-01-30 1979-08-10 Toyo Soda Mfg Co Ltd Hydrophobic rendering method for oxide fine powder
JPS6243457A (ja) * 1985-06-13 1987-02-25 ロ−ヌ−プ−ラン　フイブル ポリアミド艶消し用マスタ−バツチ
JPH0350120A (ja) * 1989-07-18 1991-03-04 Ishihara Sangyo Kaisha Ltd 二酸化チタン顔料粉末の製造方法
JPH05221640A (ja) * 1992-02-17 1993-08-31 Shin Etsu Chem Co Ltd 疎水性酸化チタン微粒子の製造方法
JPH07504932A (ja) * 1992-03-26 1995-06-01 メルク　パテント　ゲゼルシャフト　ミット　ベシュレンクテル　ハフトング 薄片状着色顔料およびその製造方法
JPH0753216A (ja) * 1993-08-17 1995-02-28 Titan Kogyo Kk 二酸化チタン微粉末およびその製造方法
JPH07138020A (ja) * 1993-11-12 1995-05-30 High Frequency Heattreat Co Ltd 超微粒子二酸化チタン複合化酸化物及びその製造方法
JPH07315839A (ja) * 1993-11-24 1995-12-05 Kerr Mcgee Chem Corp 二酸化チタン生成物及びその製造方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999044826A1 (fr) * 1998-03-03 1999-09-10 Qpf, Llc Film de polypropylene a orientation biaxiale contenant des particules de metal ou d'oxyde metallique
JP2007055875A (ja) * 2005-08-26 2007-03-08 Tayca Corp 酸化チタン水性スラリーの濾過速度を改善する方法およびこの方法から得られた酸化チタン粉体
JP2009518329A (ja) * 2005-12-09 2009-05-07 ディーエスエム アイピー アセッツ ビー．ブイ． 改質された二酸化チタン粒子を含む新規な化粧料または皮膚科用組成物
JP2007224180A (ja) * 2006-02-24 2007-09-06 Toyo Ink Mfg Co Ltd 着色樹脂組成物
CN106009470A (zh) * 2016-06-24 2016-10-12 深圳市同益实业股份有限公司 树脂材料及其制备方法
CN106633852A (zh) * 2016-12-02 2017-05-10 长兴天晟能源科技有限公司 一种提高尼龙66树脂湿稳定性的母粒

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Publication number Publication date
JP3215979B2 (ja) 2001-10-09
AU1209397A (en) 1997-07-28

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