CN110128585A - 一种多用途甲基丙烯酸异冰片酯的配方及其制备方法 - Google Patents

一种多用途甲基丙烯酸异冰片酯的配方及其制备方法 Download PDF

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CN110128585A
CN110128585A CN201810127513.7A CN201810127513A CN110128585A CN 110128585 A CN110128585 A CN 110128585A CN 201810127513 A CN201810127513 A CN 201810127513A CN 110128585 A CN110128585 A CN 110128585A
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isobornyl methacrylate
methacrylate
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崔继元
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Handan Ruista Chemical Technology Co Ltd
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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
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    • C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/08—Homopolymers or copolymers of acrylic acid esters
    • 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
    • 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

Abstract

本发明提供了一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，其配方如下：甲基丙烯酸异冰片酯0.36mol/L、丙烯酸丁酯1.75mol/L、甲基丙烯酸羟乙酯0.85mol/L、丙烯酸0.22mol/L、甲基丙烯酸甲酯A 0.60mol/L、正十二烷基硫醇0.03mol/L、过硫酸钾0.03mol/L、MIXSTAR6550可聚合乳化剂0.29mol/L、去离子水占整体的44％、丙二醇甲醚醋酸酯5％、氨水1％。本发明所述的一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，具有甲基丙烯酸异冰片酯所拥有的高硬度、高光泽、韧性强和强疏水性能等方面的优点，与其它成膜物质组成的水性树脂制备水性木器漆、水性工业漆等，对降低施工场所VOC，改善大气环境具有显著效果。

Description

一种多用途甲基丙烯酸异冰片酯的配方及其制备方法
技术领域
本发明涉及甲基丙烯酸异冰片酯制备技术领域，尤其是一种具有高硬度、高光泽、韧性强和强疏水性能等方面的优点的多用途甲基丙烯酸异冰片酯的配方及其制备方法。
背景技术
甲基丙烯酸异冰片酯由于其特殊的结构和性质近年来作为一种新颖的丙烯酸单体在研究和应用方面引起人们的兴趣和重视，其酯烷基部分为巨大的非极性二环烷基，具有很强的体积位阻效应，使之具有优异的耐UV性、耐水性和耐化学性。聚合物链上巨大的非极性基团，弱化了分子链间的作用力，相对应力及体积收缩均要小得多，提高了与其它树脂的相容性。另外甲基丙烯酸异冰片酯沸点高，玻璃化温度TgIBOMA＝170℃、TgIBOA＝100℃，具有低挥发性、减少VOC的排放、改善环境等作用。正是这些优异的性能使其应用范围不断扩大，但是其目前主要用于溶剂型高固体份涂料、汽车涂料、光固化涂料、光纤涂料、粉末涂料等，在水性漆方面的应用很少。
发明内容
为解决上述问题，本发明提供了一种具有高硬度、高光泽、韧性强和强疏水性能等方面的优点的多用途甲基丙烯酸异冰片酯的配方及其制备方法。
实现本发明目的的一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，调节体系的pH，使得pH＜2，激发甲基丙烯酸异冰片酯聚合端的活性，使其与其它单体共聚后，按如下配方配置：甲基丙烯酸异冰片酯0.36mol/L、丙烯酸丁酯1.75mol/L、甲基丙烯酸羟乙酯0.85mol/L、丙烯酸0.22mol/L、甲基丙烯酸甲酯A 0.60mol/L、正十二烷基硫醇0.03mol/L、过硫酸钾0.03mol/L、MIXSTAR6550可聚合乳化剂0.29mol/L、去离子水占整体的44％、丙二醇甲醚醋酸酯5％、氨水1％。
其制备方法如下：按配方量，在反应釜中加入乳化剂和去离子水，搅拌升温至80℃，保温0.5h，加入单体量5％的单体及35％的引发剂，升温至85-90℃，反应0.5h左右，然后滴加剩余的单体及剩余的过硫酸钾，2h内滴毕，保温2h，得到半透明的水性树脂。降温至50℃以下，过滤，出料即可。
进一步的：水性树脂(-OH 2.95％)/Bayer 305(-NCO 16％)＝-OH/-NCO＝1/1.5，其中Bayer 305需要用丙二醇甲醚醋酸酯稀释成80％。
本专利的该实施例的特点如下：光泽(60°)90％、附着力1级、硬度2H、耐52％的乙醇1h无变化。
进一步的：水性树脂(-OH 2.95％)50％、甲醚化氨基树脂8-10％、钛白粉20％、助剂3％、助溶剂15％，余量为水。
本专利的该实施例的特点如下：光泽(60°)80％、附着力1级、硬度2H、耐水168h无变化、耐盐水(5％)120h无变化、耐盐雾96h无变化。
本专利技术克服了甲基丙烯酸异冰片酯烷基部分巨大的非极性二环基团具有的很强体积位阻效应、造成得(甲基)丙烯酸异冰片酯与其它单体共聚上的困难的问题，通过调整体系pH＜2，激发(甲基)丙烯酸异冰片酯聚合端的活性，达到与其它单体共聚的目的。
本专利所述的一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，具有甲基丙烯酸异冰片酯所拥有的高硬度、高光泽、韧性强和强疏水性能等方面的优点，与其它成膜物质组成的水性树脂制备水性木器漆、水性工业漆等，对降低施工场所VOC，改善大气环境具有显著效果。
具体实施方式
本发明的一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，调节体系的pH，使得pH＜2，激发甲基丙烯酸异冰片酯聚合端的活性，使其与其它单体共聚后，按如下配方配置：甲基丙烯酸异冰片酯0.36mol/L、丙烯酸丁酯1.75mol/L、甲基丙烯酸羟乙酯0.85mol/L、丙烯酸0.22mol/L、甲基丙烯酸甲酯A 0.60mol/L、正十二烷基硫醇0.03mol/L、过硫酸钾0.03mol/L、MIXSTAR6550可聚合乳化剂0.29mol/L、去离子水占整体的44％、丙二醇甲醚醋酸酯5％、氨水1％。
其制备方法如下：按配方量，在反应釜中加入乳化剂和去离子水，搅拌升温至80℃，保温0.5h，加入单体量5％的单体及35％的引发剂，升温至85-90℃，反应0.5h左右，然后滴加剩余的单体及剩余的过硫酸钾，2h内滴毕，保温2h，得到半透明的水性树脂。降温至50℃以下，过滤，出料即可。
进一步的：水性树脂(-OH 2.95％)/Bayer 305(-NCO 16％)＝-OH/-NCO＝1/1.5，其中Bayer 305需要用丙二醇甲醚醋酸酯稀释成80％。
本专利的该实施例的特点如下：光泽(60°)90％、附着力1级、硬度2H、耐52％的乙醇1h无变化。
进一步的：水性树脂(-OH 2.95％)50％、甲醚化氨基树脂8-10％、钛白粉20％、助剂3％、助溶剂15％，余量为水。
本专利的该实施例的特点如下：光泽(60°)80％、附着力1级、硬度2H、耐水168h无变化、耐盐水(5％)120h无变化、耐盐雾96h无变化。
本专利技术克服了甲基丙烯酸异冰片酯烷基部分巨大的非极性二环基团具有的很强体积位阻效应、造成得(甲基)丙烯酸异冰片酯与其它单体共聚上的困难的问题，通过调整体系pH＜3，激发(甲基)丙烯酸异冰片酯聚合端的活性，达到与其它单体共聚的目的。
本专利所述的一种多用途甲基丙烯酸异冰片酯的配方及其制备方法，具有甲基丙烯酸异冰片酯所拥有的高硬度、高光泽、韧性强和强疏水性能等方面的优点，与其它成膜物质组成的水性树脂制备水性木器漆、水性工业漆等，对降低施工场所VOC，改善大气环境具有显著效果。
上面所述的实施例仅仅是对本发明的优选实施方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神前提下，本领域普通工程技术人员对本发明技术方案做出的各种变形和改进，均应落入本发明的权利要求书确定的保护范围内。

Claims (2)

1.一种多用途甲基丙烯酸异冰片酯的配方，其特征在于，调节体系的pH，使得pH＜2，激发甲基丙烯酸异冰片酯聚合端的活性，使其与其它单体共聚后，按如下配方配置：甲基丙烯酸异冰片酯0.36mol/L、丙烯酸丁酯1.75mol/L、甲基丙烯酸羟乙酯0.85mol/L、丙烯酸0.22mol/L、甲基丙烯酸甲酯A 0.60mol/L、正十二烷基硫醇0.03mol/L、过硫酸钾0.03mol/L、MIXSTAR6550可聚合乳化剂0.29mol/L、去离子水占整体的44％、丙二醇甲醚醋酸酯5％、氨水1％。
2.一种多用途甲基丙烯酸异冰片酯的制备方法，其特征在于，其制备方法如下：按配方量，在反应釜中加入乳化剂和去离子水，搅拌升温至80℃，保温0.5h，加入单体量5％的单体及35％的引发剂，升温至85-90℃，反应0.5h左右，然后滴加剩余的单体及剩余的过硫酸钾，2h内滴毕，保温2h，得到半透明的水性树脂，降温至50℃以下，过滤，出料即可。
CN201810127513.7A 2018-02-08 2018-02-08 一种多用途甲基丙烯酸异冰片酯的配方及其制备方法 Pending CN110128585A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111763280A (zh) * 2020-07-02 2020-10-13 安徽罗斯夫新材料科技有限公司 一种自清洁丙烯酸乳液及其制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061665A (zh) * 2015-07-31 2015-11-18 华南理工大学 一种羟基聚丙烯酸酯乳液及其制备方法与应用
CN105949378A (zh) * 2016-05-17 2016-09-21 佛山市加恩新材料有限公司 一种水性丙烯酸乳液树脂和水性涂层乳液及制备方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061665A (zh) * 2015-07-31 2015-11-18 华南理工大学 一种羟基聚丙烯酸酯乳液及其制备方法与应用
CN105949378A (zh) * 2016-05-17 2016-09-21 佛山市加恩新材料有限公司 一种水性丙烯酸乳液树脂和水性涂层乳液及制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111763280A (zh) * 2020-07-02 2020-10-13 安徽罗斯夫新材料科技有限公司 一种自清洁丙烯酸乳液及其制备方法

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