WO2019127442A1 - 一种水性涂料及其制备方法 - Google Patents

一种水性涂料及其制备方法 Download PDF

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WO2019127442A1
WO2019127442A1 PCT/CN2017/120047 CN2017120047W WO2019127442A1 WO 2019127442 A1 WO2019127442 A1 WO 2019127442A1 CN 2017120047 W CN2017120047 W CN 2017120047W WO 2019127442 A1 WO2019127442 A1 WO 2019127442A1
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water
acrylic resin
butyl
aqueous
raw materials
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PCT/CN2017/120047
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French (fr)
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张继华
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张继华
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • 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
    • C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
    • C09D125/02—Homopolymers or copolymers of hydrocarbons
    • C09D125/04—Homopolymers or copolymers of styrene
    • C09D125/08—Copolymers of styrene
    • C09D125/14—Copolymers of styrene with unsaturated esters

Definitions

  • the invention relates to the field of waterborne coatings, in particular to an aqueous coating and a preparation method thereof.
  • Water-based paints are widely used because they are harmless to the human body, have low pollution and save resources.
  • Existing water-based paints contain synthetic resins, but existing water-based resins are not highly transparent, affecting gloss and water resistance. Therefore, in order to avoid the disadvantages existing in the prior art, it is necessary to make improvements to the prior art.
  • the object of the present invention is to overcome the shortcomings and deficiencies of the prior art and to provide an aqueous coating which can improve the gloss and ease of use.
  • Another object of the present invention is to provide a method for preparing an aqueous coating.
  • a water-based paint comprising the following raw materials in a percentage by mass: 70% to 85% of water-based acrylic resin, 5% to 10% of ethanol, 5% to 10% of water, and 5% to 10% of silane coupling agent, said water-based
  • the acrylic resin includes the following raw materials in mass ratio: 20% to 25% of styrene, 10% to 15% of butyl acrylate, 15% to 20% of methyl methacrylate, 5% to 10% of acrylic acid, and isooctanoic acid peroxide.
  • Tertiary ester 1% to 5%, tert-butyl peroxybenzoate 0.1% to 1%, propylene glycol methyl ether 30% to 40%, and ammonia water 5% to 10%.
  • the following raw materials are included in the mass ratio: 73% aqueous acrylic resin, 9% ethanol, 9% water, and 9% silane coupling agent.
  • the aqueous acrylic resin comprises the following raw materials in a mass ratio: styrene 20%, butyl acrylate 10%, methyl methacrylate 15%, acrylic acid 10%, tert-butyl peroxyoctanoate 1%, Oxidation of tert-butyl benzoate 1%, propylene glycol methyl ether 35% and ammonia water 8%.
  • a method for preparing an aqueous coating comprising the following steps:
  • Step (1) preparing raw materials according to mass ratio, and passing nitrogen in the high tank and the reaction kettle;
  • Step (2) adding styrene, butyl acrylate, methyl methacrylate, acrylic acid, t-butyl peroxyisophthalate and t-butyl peroxybenzoate to a high-level tank for mixing and standby;
  • Step (3) propylene glycol methyl ether was added to the reaction vessel and the reactor was heated to 110 ° C ⁇ 130 ° C, the mixed solution in step (1) was added dropwise into the reaction kettle, the addition time was 4h;
  • Step (4) the mixed solution in the step (3) is kept for 6 hours, then cooled to 10 ° C to 40 ° C, added with ammonia water, stirred for 30 min, and the viscosity is detected to obtain a finished aqueous acrylic resin, which is sealed and stored;
  • Step (5) adding ethanol, water and a silane coupling agent to the finished product of the aqueous acrylic resin, stirring uniformly, adjusting the viscosity, and performing the construction.
  • the reactor was heated to 120 °C.
  • the cooling temperature of the step (4) is 30 °C.
  • the water-based acrylic resin of the invention is beneficial to improve the gloss of the water-based paint, and the two-component room temperature curing is carried out by the silane coupling agent, the curing mode is simple, the construction is convenient, the activation period is long, and the use is more stable.
  • the present invention is a transparent water-soluble acrylic resin which has a better gloss and a longer activation period than an emulsion cured with isocyanate.
  • a water-based paint comprising the following raw materials in a percentage by mass: 70% to 85% of water-based acrylic resin, 5% to 10% of ethanol, 5% to 10% of water, and 5% to 10% of silane coupling agent, said water-based
  • the acrylic resin includes the following raw materials in mass ratio: 20% to 25% of styrene, 10% to 15% of butyl acrylate, 15% to 20% of methyl methacrylate, 5% to 10% of acrylic acid, and isooctanoic acid peroxide.
  • Tertiary ester 1% to 5%, tert-butyl peroxybenzoate 0.1% to 1%, propylene glycol methyl ether 30% to 40%, and ammonia water 5% to 10%.
  • the following raw materials are included in the mass ratio: 73% aqueous acrylic resin, 9% ethanol, 9% water, and 9% silane coupling agent.
  • the waterborne acrylic resin comprises the following raw materials in mass ratio: styrene 20%, butyl acrylate 10%, methyl methacrylate 15%, acrylic acid 10%, tert-butyl peroxyoctanoate 1%, benzoic acid benzoic acid 1% butyl ester, 35% propylene glycol methyl ether and 8% ammonia water.
  • a method for preparing an aqueous coating comprising the following steps:
  • Step (1) Prepare the raw materials according to the mass ratio, and pass nitrogen gas in the high tank and the reaction vessel to avoid coloring.
  • Step (2) adding styrene, butyl acrylate, methyl methacrylate, acrylic acid, tert-butyl peroxyisophthalate and t-butyl peroxybenzoate to a high-position tank for uniform use.
  • Step (3) adding propylene glycol methyl ether to the reaction vessel and raising the reaction vessel to 110 ° C to 130 ° C, the mixed solution in the step (1) is added dropwise to the reaction vessel, and the dropping time is 4 hours;
  • the reaction vessel can be heated to 120 ° C, and the reaction effect is better.
  • Propylene glycol methyl ether is used to adjust the viscosity of the aqueous coating and can be adjusted as needed.
  • Step (4) the mixed solution in the step (3) is kept for 6 hours, then cooled to 10 ° C to 40 ° C, added with ammonia water, stirred for 30 min; cooled at a temperature of 30 ° C, the viscosity is measured, and the finished aqueous acrylic resin is obtained, and sealed and stored. Ammonia water is used as a diluent and can be added slowly to adjust to the proper viscosity.
  • Step (5) adding ethanol, water and a silane coupling agent to the finished product of the aqueous acrylic resin, stirring uniformly, adjusting the viscosity, and performing the construction. Step (5) can be carried out before the construction and adjusted to the appropriate application viscosity.
  • the activation period is relatively long, greater than 6h.
  • the waterborne acrylic resin comprises the following raw materials in mass ratio: styrene 20%, butyl acrylate 10%, methyl methacrylate 15%, acrylic acid 10%, tert-butyl peroxyoctanoate 1%, benzoic acid benzoic acid 1% butyl ester, 35% propylene glycol methyl ether and 8% ammonia water.
  • the water-based paint naturally dried after 72h test performance obtained the following data: 1, using the gloss meter (60 °) test, gloss > 93 °; 2, after 24 hours of normal temperature blisters, no whitening, no blistering phenomenon.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Paints Or Removers (AREA)

Abstract

一种水性涂料及其制备方法，按质量百份比包括以下原材料：水性丙烯酸树脂70％～85％、乙醇5％～10％、水5％～10％及硅烷偶联剂5％～10％，所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％～25％、丙烯酸丁酯10％～15％、甲基丙烯酸甲酯15％～20％、丙烯酸5％～10％、过氧化异辛酸叔丁酯1％～5％、过氧化苯甲酸叔丁酯0.1％～1％、丙二醇甲醚30％～40％及氨水5％～10％。该材料耐水性好，光泽度高，施工环境要求低，降低了施工成本，提高了防腐效果和使用稳定性。

Description

一种水性涂料及其制备方法 技术领域
本发明涉及水性涂料领域，具体涉及一种水性涂料及其制备方法。
背景技术
水性涂料对人体无害，污染低及节省资源而得到广泛应用。现有的水性涂料含有人工合成树脂，但现有的水性树脂透明度不高，影响光泽度和耐水性。因此，为了避免现有技术中存在的缺点，有必要对现有技术做出改进。
发明内容
本发明的目的在于克服现有技术中的缺点与不足，提供一种能提高使用光泽度和使用方便性的水性涂料。
本发明的另一个目的在于提供一种水性涂料制备方法。
本发明是通过以下的技术方案实现的：
一种水性涂料，按质量百份比包括以下原材料：水性丙烯酸树脂70％～85％、乙醇5％～10％、水5％～10％及硅烷偶联剂5％～10％，所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％～25％、丙烯酸丁酯10％～15％、甲基丙烯酸甲酯15％～20％、丙烯酸5％～10％、过氧化异辛酸叔丁酯1％～5％、过氧化苯甲酸叔丁酯0.1％～1％、丙二醇甲醚30％～40％及氨水5％～10％。
进一步，按质量百份比包括以下原材料：水性丙烯酸树脂73％、乙醇9％、水9％及硅烷偶联剂9％。
进一步，所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％、丙烯酸丁酯10％、甲基丙烯酸甲酯15％、丙烯酸10％、过氧化异辛酸叔丁酯1％、过氧化苯甲酸叔丁酯1％、丙二醇甲醚35％及氨水8％。
一种水性涂料制备方法，包括以下步骤：
步骤(1)：按质量配比准备原材料，并在高位槽和反应釜内通过氮气；
步骤(2)：将苯乙烯、丙烯酸丁酯、甲基丙烯酸甲酯、丙烯酸、过氧化异辛酸叔丁酯及 过氧化苯甲酸叔丁酯加入高位槽内混合均匀备用；
步骤(3)：将丙二醇甲醚加入反应釜内并将反应釜升温至110℃～130℃，将步骤(1)中的混合溶液滴加入反应釜内，滴加时间为4h；
步骤(4)：将步骤(3)中的混合溶液保温6h后冷却至10℃～40℃，加入氨水，搅拌30min，检测粘度，得到水性丙烯酸树脂成品，密封保存；
步骤(5)：将乙醇、水及硅烷偶联剂加入水性丙烯酸树脂成品中，搅拌均匀，调节粘度，进行施工。
进一步，所述步骤(3)将反应釜升温至120℃。
进一步，所述步骤(4)的冷却温度为30℃。
相对于现有技术，本发明的水性丙烯酸树脂有利于提高水性涂料的光泽度，通过硅烷偶联剂进行双组份常温固化，固化方式简单，施工方便，活化期长，使用更稳定。本发明是一种透明的水溶性丙烯酸树脂，相对于采用异氰酸酯固化的乳液，有着更好的光泽，更长的活化期。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
一种水性涂料，按质量百份比包括以下原材料：水性丙烯酸树脂70％～85％、乙醇5％～10％、水5％～10％及硅烷偶联剂5％～10％，所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％～25％、丙烯酸丁酯10％～15％、甲基丙烯酸甲酯15％～20％、丙烯酸5％～10％、过氧化异辛酸叔丁酯1％～5％、过氧化苯甲酸叔丁酯0.1％～1％、丙二醇甲醚30％～40％及氨水5％～10％。
作为一种具体实施方式，按质量百份比包括以下原材料：水性丙烯酸树脂73％、乙醇9％、水9％及硅烷偶联剂9％。水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％、丙烯酸丁酯10％、甲基丙烯酸甲酯15％、丙烯酸10％、过氧化异辛酸叔丁酯1％、过氧化苯甲酸叔丁酯1％、丙二醇甲醚35％及氨水8％。
一种水性涂料制备方法，包括以下步骤：
步骤(1)：按质量配比准备原材料，并在高位槽和反应釜内通过氮气，以免着色。
步骤(2)：将苯乙烯、丙烯酸丁酯、甲基丙烯酸甲酯、丙烯酸、过氧化异辛酸叔丁酯及 过氧化苯甲酸叔丁酯加入高位槽内混合均匀备用。
步骤(3)：将丙二醇甲醚加入反应釜内并将反应釜升温至110℃～130℃，将步骤(1)中的混合溶液滴加入反应釜内，滴加时间为4h；作为一种具体实施方式，可将反应釜升温至120℃，反应效果较佳。丙二醇甲醚用于调整水性涂料的粘度，可根据需要进行调整。
步骤(4)：将步骤(3)中的混合溶液保温6h后冷却至10℃～40℃，加入氨水，搅拌30min；冷却可以温度为30℃，检测粘度，得到水性丙烯酸树脂成品，密封保存。氨水作为稀释剂，可缓慢加入以调整到合适粘度。
步骤(5)：将乙醇、水及硅烷偶联剂加入水性丙烯酸树脂成品中，搅拌均匀，调节粘度，进行施工。步骤(5)可在施工前操作，并调节到合适的施工粘度后进行施工。活化期比较长，大于6h。
测试数据：
一、采用以下配比得到水性涂料：水性丙烯酸树脂73％、乙醇9％、水9％及硅烷偶联剂9％。水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％、丙烯酸丁酯10％、甲基丙烯酸甲酯15％、丙烯酸10％、过氧化异辛酸叔丁酯1％、过氧化苯甲酸叔丁酯1％、丙二醇甲醚35％及氨水8％。
二、水性涂料自然干燥72h后测试性能得到以下数据：1、采用光泽度仪(60°)测试，光泽度>93°；2、常温水泡24h后，无发白，无起泡现象。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

  1. 一种水性涂料，其特征在于：按质量百份比包括以下原材料：水性丙烯酸树脂70％～85％、乙醇5％～10％、水5％～10％及硅烷偶联剂5％～10％，所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％～25％、丙烯酸丁酯10％～15％、甲基丙烯酸甲酯15％～20％、丙烯酸5％～10％、过氧化异辛酸叔丁酯1％～5％、过氧化苯甲酸叔丁酯0.1％～1％、丙二醇甲醚30％～40％及氨水5％～10％。
  2. 根据权利要求1所述的水性涂料，其特征在于：按质量百份比包括以下原材料：水性丙烯酸树脂73％、乙醇9％、水9％及硅烷偶联剂9％。
  3. 根据权利要求1所述的水性涂料，其特征在于：所述水性丙烯酸树脂按质量百份比包括以下原材料：苯乙烯20％、丙烯酸丁酯10％、甲基丙烯酸甲酯15％、丙烯酸10％、过氧化异辛酸叔丁酯1％、过氧化苯甲酸叔丁酯1％、丙二醇甲醚35％及氨水8％。
  4. 一种水性涂料制备方法，其特征在于：包括以下步骤：
    步骤(1)：按质量配比准备原材料，并在高位槽和反应釜内通过氮气；
    步骤(2)：将苯乙烯、丙烯酸丁酯、甲基丙烯酸甲酯、丙烯酸、过氧化异辛酸叔丁酯及过氧化苯甲酸叔丁酯加入高位槽内混合均匀备用；
    步骤(3)：将丙二醇甲醚加入反应釜内并将反应釜升温至110℃～130℃，将步骤(2)中的混合溶液滴加入反应釜内，滴加时间为4h；
    步骤(4)：将步骤(3)中的混合溶液保温6h后冷却至10℃～40℃，加入氨水，搅拌30min，检测粘度，得到水性丙烯酸树脂成品，密封保存；
    步骤(5)：将乙醇、水及硅烷偶联剂加入水性丙烯酸树脂成品中，搅拌均匀，调节粘度，进行施工。
  5. 根据权利要求4所述的水性涂料制备方法，其特征在于：所述步骤(3)将反应釜升温至120℃。
  6. 根据权利要求4所述的水性涂料制备方法，其特征在于：所述步骤(4)的冷却温度为30℃。
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