WO2012167650A1 - Preparation method for non-silicon defoamer reagent used for solvent-type coating and ink - Google Patents

Preparation method for non-silicon defoamer reagent used for solvent-type coating and ink Download PDF

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WO2012167650A1
WO2012167650A1 PCT/CN2012/073155 CN2012073155W WO2012167650A1 WO 2012167650 A1 WO2012167650 A1 WO 2012167650A1 CN 2012073155 W CN2012073155 W CN 2012073155W WO 2012167650 A1 WO2012167650 A1 WO 2012167650A1
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solvent
weight
acrylate
based coating
initiator
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陈永康
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Chen Yongkang
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/02Foam dispersion or prevention
    • B01D19/04Foam dispersion or prevention by addition of chemical substances
    • B01D19/0404Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular

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  • the invention relates to a non-silicon type antifoaming agent for a solvent type coating ink and a production method thereof.
  • silicone defoaming agents are mostly used, and silicone oil and fumed silica are generally used for compounding.
  • silicone defoamers are generally not used in the primer coating of coating inks, which provides good market conditions for the development of non-silicone defoamers.
  • the invention provides a preparation method of a non-silicone antifoaming agent for solvent-based coating inks with good foam suppression and defoaming performance.
  • a non-silicone antifoaming agent for solvent-based coating inks which is characterized in that it is mainly made of the following raw materials by weight:
  • the fumed silica is 1-5%; and the fumed silica is selected from hydrophobic white carbon having a specific surface area of 200 m 2 /g or more.
  • the acrylate monomer is one or more of methyl acrylate, butyl acrylate, ethyl acrylate, isooctyl acrylate, lauryl acrylate, and octadecyl acrylate.
  • the functional acrylate monomer is one or more of hydroxypropyl methacrylate, hydroxypropyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid, methacrylic acid.
  • the initiator is azobisisobutyronitrile, benzoyl peroxide or tert-butyl peroxybenzoate.
  • the solvent is one or more of toluene, xylene, butyl acetate, propylene glycol methyl ether, and propylene glycol methyl ether acetate.
  • a preparation method of non-silicone antifoaming agent for solvent type coating ink which is characterized by: firstly, 0.5-45% The weight percentage of the solvent is poured into the reaction vessel and the temperature is raised to 80-145 ° C; while 40-90% by weight of the acrylate monomer, 0.0005-0.9% by weight of the initiator is at 3-5 Add to the reaction vessel within an hour, carry out polymerization, heat preservation for 2-3 hours; add 0.3-4% by weight of solvent and 0.0004% to 0.05% by weight of initiator; Incubate for 2-3 hours; add 0.0001-0.05% by weight of initiator and 0.2-1% by weight of solvent; keep warm for 1-2 hours; add at 80-145 °C 1-5% by weight of fumed silica, stirred for 2-5 hours, stirred for 2-5 hours; cooled to give the product.
  • the vacuum was vacuumed and the solvent in the reactor was purged.
  • a 1-5% by weight functional acrylate monomer is also added to the kettle along with the acrylic monomer and initiator.
  • the invention has excellent antifoaming and defoaming properties and can replace the use of silicone antifoaming agents in the system.
  • the invention relates to a non-silicone defoamer, a silicone defoamer and a blank antifoaming and defoaming application experiment:
  • 1 is a graph showing the experimental density of non-silicone defoaming agent, silicone antifoaming agent and blank antifoaming and defoaming application according to the present invention (non-silicone defoaming agent, silicone defoaming agent and blank of the present invention)
  • the density value changes with time after shaking for 15 minutes with hydroxy acrylate.
  • I-silicone defoamer II - non-silicone defoamer of the invention, III-blank.
  • a preparation method of a non-silicone antifoaming agent for a solvent-based coating ink firstly 5-60% (examples 5%, 35%, 60%)
  • the weight percentage of the solvent is poured into the reaction vessel, and the temperature is raised to 80-145 ° C (eg 80 ° C, 110 ° C, 145 ° C); at the same time will be 15-87% (example 15%, 45%, 87%) % by weight of acrylate monomer, 1-5% (Example 1%, 3%, 5%) by weight of functional acrylate monomer, 0.0005-4% (example 0.0005%, 2% 4%)
  • the weight percentage of the initiator is added to the reaction vessel within 3-5 hours, and the polymerization reaction is carried out for 2-3 hours; the addition is 3-10% (examples 3%, 7%, 10%) % by weight of solvent and 0.0004-0.
  • the acrylate monomer is one or more of methyl acrylate (or butyl acrylate, ethyl acrylate or isooctyl acrylate, lauryl acrylate, octadecyl acrylate).
  • the functional acrylate monomer is Hydroxypropyl methacrylate (or one or more of hydroxypropyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid or methacrylic acid).
  • the initiator is azobisisobutyronitrile (or benzoyl peroxide or tert-butyl peroxybenzoate).
  • the solvent is toluene (or one or more of xylene, butyl acetate, propylene glycol methyl ether, propylene glycol methyl ether acetate).
  • the fumed silica (also referred to as fumed silica) is selected to be a hydrophobic white carbon having a specific surface area of 200 m 2 /g (BET method) or more.
  • a vacuum is applied under a vacuum to clean the solvent in the reactor.
  • the present invention may further incorporate a fluorine monomer or no functional acrylate monomer.

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract

Disclosed are non-silicon defoamer reagent used for solvent-type coating and ink and preparation method thereof. The defoamer reagent is prepared from an acrylate monomer, a functional acrylate monomer, an initiator, a solvent and a fumed silica by adding the acrylate monomer, the functional acrylate monomer, the initiator and the solvent to a reaction kettle for polymerization reaction, then mixing the product and the fumed silica. The non-silicon defoamer reagent has excellent foam inhibiting and defoaming effects, and can replace organosilicone defoamers reagent to be used in a system.

Description

一种溶剂型涂料油墨用非硅类消泡剂的制备方法  Preparation method of non-silicon type antifoaming agent for solvent type coating ink
技术领域 Technical field
本发明涉及一种溶剂型涂料油墨用非硅类消泡剂及生产方法。 The invention relates to a non-silicon type antifoaming agent for a solvent type coating ink and a production method thereof.
背景技术 Background technique
在涂料油墨用消泡剂中,有机硅消泡剂居多,一般使用硅油和气相法二氧化硅进行复配使用。但是,在涂料油墨的底涂中一般不使用有机硅消泡剂,这就为非硅类消泡剂的开发提供了很好的市场条件。 Among the antifoaming agents for coating inks, silicone defoaming agents are mostly used, and silicone oil and fumed silica are generally used for compounding. However, silicone defoamers are generally not used in the primer coating of coating inks, which provides good market conditions for the development of non-silicone defoamers.
发明内容 Summary of the invention
本发明提供一种抑泡和脱泡性能好的溶剂型涂料油墨用非硅类消泡剂的制备方法。 The invention provides a preparation method of a non-silicone antifoaming agent for solvent-based coating inks with good foam suppression and defoaming performance.
本发明的技术解决方案是: The technical solution of the present invention is:
一种溶剂型涂料油墨用非硅类消泡剂,其特征是:主要由下列重量百分比的原料制成: A non-silicone antifoaming agent for solvent-based coating inks, which is characterized in that it is mainly made of the following raw materials by weight:
丙烯酸酯单体 15~87% Acrylate monomer 15~87%
引发剂 0.001~5% Initiator 0.001~5%
溶剂 10~80% Solvent 10~80%
气相法二氧化硅 1-5% ;所述气相法二氧化硅选用为比表面积 200m2 /g 以上的疏水型白炭黑。The fumed silica is 1-5%; and the fumed silica is selected from hydrophobic white carbon having a specific surface area of 200 m 2 /g or more.
还含有 1-5% 重量的功能性丙烯酸酯单体。 It also contains 1-5% by weight of functional acrylate monomer.
所述丙烯酸酯单体为丙烯酸甲酯、丙烯酸丁酯、丙烯酸乙酯、丙烯酸异辛酯、丙烯酸月桂酯、丙烯酸十八酯中的一种或几种。 The acrylate monomer is one or more of methyl acrylate, butyl acrylate, ethyl acrylate, isooctyl acrylate, lauryl acrylate, and octadecyl acrylate.
所述功能性丙烯酸酯单体为甲基丙烯酸羟丙酯、丙烯酸羟丙酯、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸、甲基丙烯酸中的一种或几种。 The functional acrylate monomer is one or more of hydroxypropyl methacrylate, hydroxypropyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid, methacrylic acid.
所述引发剂为偶氮二异丁腈、过氧化苯甲酰或 过氧化苯甲酸叔丁酯 。 The initiator is azobisisobutyronitrile, benzoyl peroxide or tert-butyl peroxybenzoate.
所述溶剂为甲苯、二甲苯、醋酸丁酯、丙二醇甲醚、丙二醇甲醚醋酸酯中的一种或几种。 The solvent is one or more of toluene, xylene, butyl acetate, propylene glycol methyl ether, and propylene glycol methyl ether acetate.
一种溶剂型涂料油墨用非硅类消泡剂的制备方法,其特征是:首先将 0.5-45% 重量百分比的溶剂倒入反应釜内 , 升温至 80-145℃;同时将40-90% 重量百分比的丙烯酸酯单体、 0.0005-0.9% 重量百分比的引发剂在 3-5 小时内加入到反应釜内,进行聚合反应,保温2-3小时;补加0.3-4% 重量百分比的溶剂 和 0.0004-0.05% 重量百分比的 引发剂 ; 保温2-3小时;加入 0.0001-0.05% 重量百分比 引发剂 和 0.2-1 % 重量百分比的溶剂; 保温1~2小时;在80-145℃条件下加入 1-5% 重量百分比的气相法二氧化硅,搅拌 2-5 小时,搅拌 2-5 小时 ;冷却后得 产品。 A preparation method of non-silicone antifoaming agent for solvent type coating ink, which is characterized by: firstly, 0.5-45% The weight percentage of the solvent is poured into the reaction vessel and the temperature is raised to 80-145 ° C; while 40-90% by weight of the acrylate monomer, 0.0005-0.9% by weight of the initiator is at 3-5 Add to the reaction vessel within an hour, carry out polymerization, heat preservation for 2-3 hours; add 0.3-4% by weight of solvent and 0.0004% to 0.05% by weight of initiator; Incubate for 2-3 hours; add 0.0001-0.05% by weight of initiator and 0.2-1% by weight of solvent; keep warm for 1-2 hours; add at 80-145 °C 1-5% by weight of fumed silica, stirred for 2-5 hours, stirred for 2-5 hours; cooled to give the product.
加入 气相法二氧化硅前,先负压抽真空,把反应釜中溶剂抽干净。 Before adding the fumed silica, the vacuum was vacuumed and the solvent in the reactor was purged.
还将 1-5% 重量百分比的功能性丙烯酸酯单体与丙烯酸单体、引发剂一起加入反应釜中。 A 1-5% by weight functional acrylate monomer is also added to the kettle along with the acrylic monomer and initiator.
本发明具有优异的 抑泡和脱泡性,可替代有机硅类消泡剂在体系中的使用。 The invention has excellent antifoaming and defoaming properties and can replace the use of silicone antifoaming agents in the system.
本发明非硅类消泡剂、有机硅类消泡剂及空白样抑泡和消泡性应用实验: The invention relates to a non-silicone defoamer, a silicone defoamer and a blank antifoaming and defoaming application experiment:
1 、 树脂液配制 1, resin liquid preparation
羟基丙烯酸树脂:混合溶剂 =70 : 30 Hydroxy Acrylic Resin: Mixed Solvent = 70 : 30
( 混合溶剂:二甲苯:醋酸丁酯:丙二醇甲醚醋酸酯 =2:1:1) (Mixed solvent: xylene: butyl acetate: propylene glycol methyl ether acetate = 2:1:1)
2 、 测试方法 2, test method
羟基丙烯酸树脂液中添加消泡剂 0.2% ,于振动机上振动 15 分钟,在不同时间点测定其密度值。(同时做空白实验) Add 0.2% defoamer to the hydroxy acrylic resin solution and vibrate on the vibrating machine. Minutes were measured for density values at different time points. (Doing a blank experiment at the same time)
3 、密度值测试数据( 25 ℃ g/ml) 3, density value test data (25 °C g / ml)
名称 name 开罐 Open can 5 分钟 5 minutes 10 分钟 10 minutes 15 分钟 15 minutes
有机硅类消泡剂 Silicone defoamer 0.982 0.982 0.984 0.984 0.988 0.988 0.990 0.990
非硅类消泡剂 Non-silicone defoamer 0.983 0.983 0.985 0.985 0.988 0.988 0.990 0.990
空白 blank 0.921 0.921 0.936 0.936 0.956 0.956 0.977 0.977
  1. 4、 密度测试图:见附图1。  4. Density test chart: See Figure 1.
5 、结果说明 5, the results of the description
从密度值的测试数据可较为直观地看出抑泡和脱泡的优异性,树脂液中气泡越多,则测得的密度越低,随着气泡的消失,密度值逐渐提高。空白样的抑泡和消泡性能最差。非硅类消泡剂具有优异的抑泡和脱泡性,可替代有机硅类消泡剂在体系中的使用。 From the test data of the density value, the superiority of the foam suppression and the defoaming can be visually seen. The more bubbles in the resin liquid, the lower the density measured, and the density value gradually increases as the bubbles disappear. The blank sample has the worst foaming and defoaming properties. Non-silicone defoamers have excellent antifoaming and defoaming properties and can replace the use of silicone defoamers in the system.
附图说明 DRAWINGS
下面结合附图和实施例对本发明作进一步说明。 The invention will now be further described with reference to the accompanying drawings and embodiments.
图1是本发明非硅类消泡剂、有机硅类消泡剂及空白样抑泡和消泡性应用实验密度测试图(本发明非硅类消泡剂、有机硅类消泡剂及空白样在羟基丙烯酸清振荡15分钟后密度值随时间变化比较图)。 1 is a graph showing the experimental density of non-silicone defoaming agent, silicone antifoaming agent and blank antifoaming and defoaming application according to the present invention (non-silicone defoaming agent, silicone defoaming agent and blank of the present invention) The density value changes with time after shaking for 15 minutes with hydroxy acrylate.
图中:Ⅰ-有机硅类消泡剂,Ⅱ-本发明非硅类消泡剂,Ⅲ-空白样。 In the figure: I-silicone defoamer, II - non-silicone defoamer of the invention, III-blank.
具体实施方式 detailed description
一种溶剂型涂料油墨用非硅类消泡剂的制备方法,首先将 5-60% (例 5% 、 35% 、 60% )重量百分比的溶剂倒入反应釜内 , 升温至 80-145℃(例80℃、110℃、145℃);同时将15-87% (例 15% 、 45% 、 87% )重量百分比的丙烯酸酯单体、 1-5% (例 1% 、 3% 、 5% )重量百分比的功能性丙烯酸酯单体、 0.0005-4% (例 0.0005% 、 2% 、 4% )重量百分比的引发剂在 3-5 小时内加入到反应釜内,进行聚合反应,保温2-3小时;补加3-10% (例 3% 、 7% 、 10% )重量百分比的溶剂 和 0.0004-0. 5% (例 0.0004% 、 0.03% 、 0.05% )重量百分比的 引发剂 ; 保温2-3小时;加入 0.0001-0.05% (例 0.0001% 、 0.02% 、 0.5% )重量百分比 引发剂 和 2-10 % (例 2% 、 6% 、 10% )重量百分比的溶剂; 保温1~2小时;在80-145℃(例80℃、110℃、145℃)条件下加入 1-5% (例 1% 、 3% 、 5% )重量百分比的气相法二氧化硅,搅拌 2-5 小时,搅拌 2-5 小时 ;冷却后得 产品。 A preparation method of a non-silicone antifoaming agent for a solvent-based coating ink, firstly 5-60% (examples 5%, 35%, 60%) The weight percentage of the solvent is poured into the reaction vessel, and the temperature is raised to 80-145 ° C (eg 80 ° C, 110 ° C, 145 ° C); at the same time will be 15-87% (example 15%, 45%, 87%) % by weight of acrylate monomer, 1-5% (Example 1%, 3%, 5%) by weight of functional acrylate monomer, 0.0005-4% (example 0.0005%, 2% 4%) The weight percentage of the initiator is added to the reaction vessel within 3-5 hours, and the polymerization reaction is carried out for 2-3 hours; the addition is 3-10% (examples 3%, 7%, 10%) % by weight of solvent and 0.0004-0. 5% (example 0.0004%, 0.03%, 0.05%) by weight of initiator; 2-3 hours of incubation; 0.0001-0.05% (example 0.0001%, 0.02%, 0.5%) weight percent initiator and 2-10% (example 2%, 6%, 10% ) a percentage by weight of solvent; 1 to 2 hours of incubation; 1-5% (eg 1%, 3%, 5%) at 80-145 ° C (eg 80 ° C, 110 ° C, 145 ° C) The weight percentage of fumed silica is stirred for 2-5 hours, stirred for 2-5 hours; and cooled to obtain the product.
所述丙烯酸酯单体为丙烯酸甲酯(或丙烯酸丁酯、丙烯酸乙酯或丙烯酸异辛酯、丙烯酸月桂酯、丙烯酸十八酯中的一种或几种。所述功能性丙烯酸酯单体为甲基丙烯酸羟丙酯(或丙烯酸羟丙酯、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸或甲基丙烯酸中的一种或几种)。所述引发剂为偶氮二异丁腈(或过氧化苯甲酰或 过氧化苯甲酸叔丁酯) 。所述溶剂为甲苯(或二甲苯、醋酸丁酯、丙二醇甲醚、丙二醇甲醚醋酸酯中的一种或几种)。所述气相法二氧化硅(或称为气相法白炭黑)选用为比表面积 200m2 /g ( BET 法)以上的疏水型白炭黑。The acrylate monomer is one or more of methyl acrylate (or butyl acrylate, ethyl acrylate or isooctyl acrylate, lauryl acrylate, octadecyl acrylate). The functional acrylate monomer is Hydroxypropyl methacrylate (or one or more of hydroxypropyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid or methacrylic acid). The initiator is azobisisobutyronitrile (or benzoyl peroxide or tert-butyl peroxybenzoate). The solvent is toluene (or one or more of xylene, butyl acetate, propylene glycol methyl ether, propylene glycol methyl ether acetate). The fumed silica (also referred to as fumed silica) is selected to be a hydrophobic white carbon having a specific surface area of 200 m 2 /g (BET method) or more.
本发明还可以在加入 气相法二氧化硅前,先负压抽真空,把反应釜中溶剂抽干净。 In the present invention, before the addition of the fumed silica, a vacuum is applied under a vacuum to clean the solvent in the reactor.
本发明还可以再加入氟单体或不加功能性丙烯酸酯单体。 The present invention may further incorporate a fluorine monomer or no functional acrylate monomer.

Claims (1)

1 、一种溶剂型涂料油墨用非硅类消泡剂,其特征是:主要由下列重量百分比的原料制成:1. A non-silicone defoamer for solvent-based coating inks, characterized in that it is mainly made of the following weight percentages of raw materials:
丙烯酸酯单体 15~87%Acrylate monomer 15~87%
引发剂 0.001~5%Initiator 0.001~5%
溶剂 10~80%Solvent 10~80%
气相法二氧化硅 1-5% ;所述气相法二氧化硅选用为比表面积 200m2 /g 以上的疏水型白炭黑。The fumed silica is 1-5%; and the fumed silica is selected from hydrophobic white carbon having a specific surface area of 200 m 2 /g or more.
2. 根据权利要求 1 所述的溶剂型涂料油墨用非硅类消泡剂,其特征是:还含有 1-5% 重量的功能性丙烯酸酯单体。2. The non-silicone antifoaming agent for solvent-based coating inks according to claim 1, further comprising 1-5% Weight of functional acrylate monomer.
3. 根据权利要求 1 或 2 所述的溶剂型涂料油墨用非硅类消泡剂,其特征是:所述丙烯酸酯单体为丙烯酸甲酯、丙烯酸丁酯、丙烯酸乙酯、丙烯酸异辛酯、丙烯酸月桂酯、丙烯酸十八酯中的一种或几种。3. According to claim 1 or 2 The non-silicone antifoaming agent for solvent-based coating inks is characterized in that: the acrylate monomer is methyl acrylate, butyl acrylate, ethyl acrylate, isooctyl acrylate, lauryl acrylate, acrylic acid One or more of the esters.
4. 根据权利要求 1 或 2 所述的溶剂型涂料油墨用非硅类消泡剂,其特征是:所述功能性丙烯酸酯单体为甲基丙烯酸羟丙酯、丙烯酸羟丙酯、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸、甲基丙烯酸中的一种或几种。4. According to claim 1 or 2 The non-silicone antifoaming agent for solvent-based coating inks is characterized in that: the functional acrylate monomer is hydroxypropyl methacrylate, hydroxypropyl acrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate One or more of ester, acrylic acid, methacrylic acid.
5. 根据权利要求 1 或 2 所述的溶剂型涂料油墨用非硅类消泡剂,其特征是:所述引发剂为偶氮二异丁腈、过氧化苯甲酰或 过氧化苯甲酸叔丁酯 。The non-silicone antifoaming agent for solvent-based coating inks according to claim 1 or 2, wherein the initiator is azobisisobutyronitrile, benzoyl peroxide or Tert-butyl peroxybenzoate.
6. 根据权利要求 1 或 2 所述的溶剂型涂料油墨用非硅类消泡剂,其特征是:所述溶剂为甲苯、二甲苯、醋酸丁酯、丙二醇甲醚、丙二醇甲醚醋酸酯中的一种或几种。6. According to claim 1 or 2 The non-silicone antifoaming agent for a solvent-based coating ink is characterized in that the solvent is one or more of toluene, xylene, butyl acetate, propylene glycol methyl ether, and propylene glycol methyl ether acetate.
7. 一种溶剂型涂料油墨用非硅类消泡剂的制备方法,其特征是:首先将 0.5-45% 重量百分比的溶剂倒入反应釜内 , 升温至 80-145℃;同时将40-90% 重量百分比的丙烯酸酯单体、 0.0005-0.9% 重量百分比的引发剂在 3-5 小时内加入到反应釜内,进行聚合反应,保温2-3小时;补加0.3-4% 重量百分比的溶剂 和 0.0004-0.05% 重量百分比的 引发剂 ; 保温2-3小时;加入 0.0001-0.05% 重量百分比 引发剂 和 0.2-1 % 重量百分比的溶剂; 保温1~2小时;在80-145℃条件下加入 1-5% 重量百分比的气相法二氧化硅,搅拌 2-5 小时,搅拌 2-5 小时 ;冷却后得 产品。7. A method for preparing a non-silicone antifoaming agent for a solvent-based coating ink, which is characterized in that: first, 0.5-45% by weight of a solvent is poured into the reaction vessel. Warm up to 80-145 ° C; at the same time 40-90% by weight of acrylate monomer, 0.0005-0.9% by weight of initiator in 3-5 Add to the reaction vessel within an hour, carry out polymerization, heat preservation for 2-3 hours; add 0.3-4% by weight of solvent and 0.0004% to 0.05% by weight of initiator; Incubate for 2-3 hours; add 0.0001-0.05% by weight of initiator and 0.2-1% by weight of solvent; keep warm for 1-2 hours; add at 80-145 °C 1-5% by weight of fumed silica, stirred for 2-5 hours, stirred for 2-5 hours; cooled to give the product.
8. 根据权利要求 7 所述的溶剂型涂料油墨用非硅类消泡剂的制备方法,其特征是: 加入 气相法二氧化硅前,先负压抽真空,把反应釜中溶剂抽干净。8. The method for preparing a non-silicone antifoaming agent for a solvent-based coating ink according to claim 7, wherein: Before the fumed silica, a vacuum is applied under a vacuum to clean the solvent in the reactor.
9. 根据权利要求 7 或 8 所述的溶剂型涂料油墨用非硅类消泡剂的制备方法,其特征是:还将 1-5% 重量百分比的功能性丙烯酸酯单体与丙烯酸单体、引发剂一起加入反应釜中。The method for preparing a non-silicone antifoaming agent for a solvent-based coating ink according to claim 7 or 8, characterized in that: 1-5% is further A percentage by weight of the functional acrylate monomer is added to the kettle along with the acrylic monomer and initiator.
PCT/CN2012/073155 2011-06-08 2012-03-27 Preparation method for non-silicon defoamer reagent used for solvent-type coating and ink WO2012167650A1 (en)

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