CN107446472A - 一种水性聚酯涂料用改性不饱和聚酯乳液及其制备方法 - Google Patents
一种水性聚酯涂料用改性不饱和聚酯乳液及其制备方法 Download PDFInfo
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- CN107446472A CN107446472A CN201710659850.6A CN201710659850A CN107446472A CN 107446472 A CN107446472 A CN 107446472A CN 201710659850 A CN201710659850 A CN 201710659850A CN 107446472 A CN107446472 A CN 107446472A
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Classifications
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- 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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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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- C08G18/67—Unsaturated compounds having active hydrogen
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- C08G18/683—Unsaturated polyesters containing cyclic groups
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/64—Polyesters containing both carboxylic ester groups and carbonate groups
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- 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
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
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- 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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
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Abstract
本发明涉及一种水性聚酯涂料用改性不饱和聚酯乳液，是在传统的聚酯分子链上引入不饱和单体进行改性制得改性不饱和聚酯，达到规定的酸值20～80mgKOH/g后，真空脱除溶剂，再通过反相乳化法制备改性不饱和聚酯乳液；所述的改性不饱和聚酯乳液为半透明的微乳液，粒径在60～100nm。本发明还提供水性聚酯涂料用改性不饱和聚酯乳液的制备方法；本发明制得的改性不饱和聚酯乳液可配制成纯聚酯水性木器涂料，其附着力、耐沾污性、耐水性、耐碱性优于水性聚氨酯涂料、水性丙烯酸涂实、水性硅丙涂料。本发明所述的改性不饱和聚酯乳液还可与氨基树脂配制成双组分水性烤漆，也可与聚氨酯固化剂配制成双组分水性聚氨酯涂料。
Description
技术领域
本发明涉及一种水性聚酯乳液，尤其涉及到一种水性聚酯涂料用改性不饱和聚酯乳液及其制备方法，属于水性树脂技术领域。
技术背景
国内外相继制定了严厉的环保法规来限制挥发性有机化合物(VOC)向大气排放，高性能、环保化已成为涂料发展的方向。水性木器涂料以水为分散介质，生产和使用过程中污染最小，是木器涂料的发展趋势。随着人们环保意识的不断增强，水性木器漆越来越受到市场的欢迎和消费者的青睐。
目前，水性木器涂料的主要种类有水性醇酸、聚氨酯水分散体、丙烯酸乳液、聚氨酯-丙烯酸杂化乳液等。醇酸类水性木器涂料虽然成膜性好、光泽度高、装饰性好，但涂膜干性慢、硬度低、耐黄变性差，且涂料在储存过程中容易发生水解，储存稳定性差；聚氨酯水分散体类木器涂料虽然丰满度高、韧性好、装饰性好，但涂膜硬度低、耐水性差，且价格昂贵；丙烯酸乳液类木器涂料具有硬度好、价格较为低廉等优点，但丙烯酸乳液类木器涂料还存在涂膜偏软、打磨性较差、涂料对底材的渗透性差、涂膜的耐水性和耐溶剂性较差、涂膜光泽度低、丰满度较差等缺点。因此市场上大量使用丙烯酸杂化聚氨酯乳液或聚氨酯化学改性丙烯酸乳液，但其硬度、丰满度等性能较溶剂型木器漆相差较大，因此市场上水性木器漆市场占有率较小，在政府政策环保化、涂料水性化的大背景下，市场上对高硬度、高丰满度水性木器漆的要求越来越迫切。
中国专利CN105669939A公开一种改性不饱和聚酯乳液的制备方法，其特征是在双酚A与顺酐形成的不饱和聚酯分子链上引入聚氨酯链段，再反相乳化制得聚氨酯改性的不饱和聚酯乳液；该乳液与碳纤维的相容性好，可作为碳纤维上浆剂的主材使用，使碳纤维集束性能优良，耐磨性好，柔韧性较好。该乳液仅作为上浆剂使用，起到润湿胶粘作用。
溶剂型不饱和聚酯树脂(PE)木器漆因高丰满度、高硬度等特点在木器涂料领域具有较高市场占有率，由于环保的原因，水性聚酯树脂应运而生，作为含有羟基的水性聚酯都是与氨基树脂配制成烤漆，或与聚氨酯固化剂配制成双组分涂料。目前没有公开资料报导纯聚酯水性木器涂料，因此开发一种用于纯聚酯水性木器涂料的改性聚酯乳液很有必要。
发明内容
为克服现有技术的缺点和不足，本发明的目的旨在提供一种水性聚酯涂料用改性不饱和聚酯乳液。
本发明的另一目的提供一种水性聚酯涂料用改性不饱和聚酯乳液的制备方法。
本发明所述的水性聚酯涂料用改性不饱和聚酯乳液，在传统的聚酯分子链上引入不饱和单体进行改性制得改性不饱和聚酯，达到规定的酸值20～80mgKOH/g后，真空脱除溶剂，再通过反相乳化法制备改性不饱和聚酯乳液。
本发明所述的水性聚酯涂料用改性不饱和聚酯乳液的制备方法，步骤如下：
a)、在装有搅拌器、冷凝管、恒压加料装置和温度计的反应釜中，将30～40份多元醇、20～40份有机酸酐加入到反应器中，添加10～15份二甲苯，在160～200℃反应4～6h；然后降温到120℃加入10～12份改性多元醇与5～10份不饱和反应型单体、0.5份对苯二酚，在温度120～180℃下继续反应3～5h至酸值为20～80mgKOH/g，在真空下脱除溶剂，得到亲水型改性不饱和聚酯树脂；
b)、反相乳化：将所述的亲水型改性不饱和聚酯树脂降温至反相乳化转变温度30～60℃，加入三乙胺-二氯甲烷络合物进行中和反应；然后加入0.5～5份不饱和反应型乳化剂或常规乳化剂、去离子水80～125份，转相后，继续滴加去离子水40～160份，最终得到固含30％～40％的所述改性不饱和聚酯乳液。
其中，所述的多元醇为丙二醇、丁二醇、新戊二醇、乙基丁基丙二醇、甘油、三羟甲基丙烷、季戊四醇和双三羟甲基丙烷的一种或两种。
所述的有机酸酐为间苯二甲酸、对苯二甲酸、四氯邻苯二甲酸酐、四氢化邻苯二甲酸酐、邻苯二甲酸酐、己二酸、壬二酸、癸二酸、马来酸酐、富马酸中的一种或两种以上。
所述的改性多元醇为相对分子质量为1000～20000的聚醚多元醇或聚酯多元醇；所述的聚酯多元醇为聚己二酸丁二醇酯二元醇、聚碳酸酯二元醇、聚己内酯二元醇中的一种或两种以上；所述的聚醚多元醇为聚四氢呋喃醚二醇、聚四亚甲基醚二醇、聚环氧丙烷醚二醇中的一种或两种以上。
所述的不饱和反应型单体为甲基丙烯酰氧基丙二醇、对苯乙烯基磺酸、邻苯乙烯基磺酸、α-对苯乙烯基乙酸、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、甲基丙烯酸羟丁酯、三羟甲基丙烷三甲基丙烯酸酯、富马酸、衣康酸、马来酸酐中的一种或两种以上。
所述的不饱和反应型乳化剂为2-丙烯酰胺-2,2-二甲基乙磺酸钠、乙烯基聚乙二醇、烯丙基磺基烷氧基琥珀酸双酯钠盐、烯丙基-2丙基乙磺酸钠、乙烯基-2-丙基乙磺酸钠、聚氧化乙烯壬酚醚丙烯酸酯、十八烷基二甲基乙烯苯基氯化铵中的一种或两种以上。
所述的常规乳化剂为OP类、苯乙基酚聚氧乙烯醚类、吐温类、脂肪醇聚氧乙烯醚类的一种或两种以上。
本发明的一种水性聚酯涂料用改性不饱和聚酯乳液，通过不饱和酸酐或不饱和羧酸类单体将碳碳双键接枝于聚酯树脂上，且由于不饱和羧酸(酐)类单体位于或接近于聚酯树脂端基，因此碳碳双键活性较大，易于进行自由基聚合反应而交联固化。本发明制得的乳液亲水性好，为半透明的纳米微乳液，其粒径为60～100nm。
本发明所述的改性不饱和聚酯乳液可配制成纯聚酯水性木器涂料，其附着力、耐沾污性、耐水性、耐碱性优于水性聚氨酯涂料、水性丙烯酸涂实、水性硅丙涂料。本发明所述的改性不饱和聚酯乳液还可与氨基树脂配制成双组分水性烤漆，也可与聚氨酯固化剂配制成双组分水性聚氨酯涂料。
本发明所述的改性不饱和聚酯树脂分子结构式如下所示：
其中，分子结构式中1-表示R1-COO-R2-OCOR3，R1、R2、R3分别代表不同碳链长度的烷基。
具体实施方式
下面结合实施例对本发明的一种水性聚酯涂料用改性不饱和聚酯乳液做进一步的描述。可以理解的是，此处所描述的具体实施例仅仅用于解释相关发明，而非对该发明的限定。
实施例1
一种水性聚酯涂料用改性不饱和聚酯乳液，制备步骤如下：
a)、在装有搅拌器、冷凝管、恒压加料装置和温度计的反应釜中，将5份季戊四醇、18份乙二醇、新戊二醇10份、12份己二酸、25份苯酐加入到反应器中，添加10份二甲苯，在120～200℃反应4h；然后加入10份聚己二酸丁二醇酯二元醇与8份甲基丙烯酸羟丙酯、0.5份对苯二酚，在温度120～200℃下继续反应3h至酸值为70～75mgKOH/g，在真空下脱除溶剂二甲苯，得到亲水不饱和聚酯树脂；
b)、反相乳化：将所述的亲水型改性不饱和聚酯树脂降温至反相乳化转变温度40℃，加入加入三乙胺-二氯甲烷络合物进行中和反应，然后加入2份2-丙烯酰胺-2,2-二甲基乙磺酸钠乳化剂、去离子水85份，转相后，继续滴加去离子水110份，最终得固含30％的所述改性不饱和聚酯乳液。
实施例2
一种水性聚酯涂料用改性不饱和聚酯乳液，制备步骤如下：
a)、在装有搅拌器、冷凝管、恒压加料装置和温度计的反应釜中，将5份三羟甲基丙烷、新戊二醇20份、10份对苯二甲酸、5份马来酸酐、25份苯酐加入到反应器中，添加10份二甲苯，在120～200℃反应4h；然后加入10份聚碳酸酯二元醇与12份甲基丙烯酸羟丁酯、0.5份对苯二酚，在温度120～200℃下继续反应3h至酸值为70～80mgKOH/g，在真空下脱除溶剂二甲苯，得到亲水不饱和聚酯树脂；
b)、反相乳化：将所述的亲水型改性不饱和聚酯树脂降温至反相乳化转变温度50℃，加入加入三乙胺-二氯甲烷络合物进行中和反应，然后加入2.5份烯丙基-2丙基乙磺酸钠乳化剂、去离子水95份，转相后，继续滴加去离子水120份，最终得固含30％的所述改性不饱和聚酯乳液。
实施例3
一种水性聚酯涂料用改性不饱和聚酯乳液，制备步骤如下：
a)、在装有搅拌器、冷凝管、恒压加料装置和温度计的反应釜中，将2份季戊四醇、2份三羟甲基丙烷、新戊二醇25份、10份己二酸、5份马来酸酐、15份苯酐加入到反应器中，添加10份二甲苯，在120～200℃反应4h；然后加入8份聚碳酸酯二元醇与10份甲基丙烯酸羟丁酯、0.5份对苯二酚，在温度120～200℃下继续反应3h至酸值在40～50mgKOH/g，在真空下脱除溶剂二甲苯，得到亲水不饱和聚酯树脂；
b)、反相乳化：将所述的亲水型改性不饱和聚酯树脂降温至反相乳化转变温度50℃，加入加入三乙胺-二氯甲烷络合物进行中和反应，然后加入2份烯丙基磺基烷氧基琥珀酸双酯钠乳化剂、去离子水100份，转相后，继续滴加去离子水125，最终得固含30％的所述改性不饱和聚酯乳液。
实施例1-3中所述的改性不饱和聚酯乳液技术指标如表1所示：
表1改性不饱和聚酯乳液技术指标
| 实施例 | 粘度 | 玻璃化温度Tg | 粒径 |
| 实施例1 | 320～350mPa·s | 45℃ | 70nm±5nm |
| 实施例2 | 260～300mPa·s | 35℃ | 60nm±5nm |
| 实施例3 | 400～430mPa·s | 50℃ | 90nm±5nm |
实施例1-3所述的改性不饱和聚酯乳液按相同配方配成水性双组分聚酯木器清漆，与水性双组份聚氨酯亮光清面漆性能进行对比(实干24h)，其技术数据如表2所示：
表2对比技术数据
| 实施例 | 硬度 | 60光泽 | 耐水性，48h | 耐碱性 |
| 实施例1 | 1H | 82～86％ | 不起泡不发白 | 不起泡不起皱 |
| 实施例2 | 1H | 80～85％ | 不起泡不发白 | 不起泡不起皱 |
| 实施例3 | 1H | 78～84％ | 不起泡不发白 | 不起泡不起皱 |
| 聚氨酯 | 1H | 76～82％ | 不起泡不发白 | 不起泡不起皱 |
尽管本发明已作了详细说明并引证了实施例，但对于本领域的普通技术人员，显然可以按照上述说明而做出的各种方案、修改和改动，都应该包括在权利要求的范围之内。
Claims (7)
1.一种水性聚酯涂料用改性不饱和聚酯乳液，其特征在于，所述的水性聚酯涂料用改性不饱和聚酯乳液，是在传统的聚酯分子链上引入不饱和单体进行改性制得改性不饱和聚酯，达到规定的酸值20～80mgKOH/g后，真空脱除溶剂，再通过反相乳化法制得；
所述的改性不饱和聚酯树脂分子结构式如下所示：
其中，分子结构式中1-表示R1-COO-R2-OCOR3，R1、R2、R3分别代表不同碳链长度的烷基；
所述的水性聚酯涂料用改性不饱和聚酯乳液，其制备步骤如下：
a)、在装有搅拌器、冷凝管、恒压加料装置和温度计的反应釜中，将30～40份多元醇、20～40份有机酸酐加入到反应器中，添加10～15份二甲苯，在160～200℃反应4～6h；然后降温到120℃加入10～12份改性多元醇与5～10份不饱和反应型单体、0.5份对苯二酚，在温度120～180℃下继续反应3～5h至酸值为20～80mgKOH/g，在真空下脱除溶剂，得到亲水型改性不饱和聚酯树脂；
b)、反相乳化：将所述的亲水型改性不饱和聚酯树脂降温至反相乳化转变温度30～60℃，加入三乙胺-二氯甲烷络合物进行中和反应；然后加入0.5～5份不饱和反应型乳化剂或常规乳化剂、去离子水80～125份，转相后，继续滴加去离子水40～160份，最终得到固含30％～40％的所述改性不饱和聚酯乳液。
2.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的多元醇为丙二醇、丁二醇、新戊二醇、乙基丁基丙二醇、甘油、三羟甲基丙烷、季戊四醇和双三羟甲基丙烷的一种或两种。
3.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的有机酸酐为间苯二甲酸、对苯二甲酸、四氯邻苯二甲酸酐、四氢化邻苯二甲酸酐、邻苯二甲酸酐、己二酸、壬二酸、癸二酸、马来酸酐、富马酸中的一种或两种以上。
4.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的改性多元醇为相对分子质量为1000～20000的聚醚多元醇或聚酯多元醇；所述的聚酯多元醇为聚己二酸丁二醇酯二元醇、聚碳酸酯二元醇、聚己内酯二元醇中的一种或两种以上；所述的聚醚多元醇为聚四氢呋喃醚二醇、聚四亚甲基醚二醇、聚环氧丙烷醚二醇中的一种或两种以上。
5.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的不饱和反应型单体为甲基丙烯酰氧基丙二醇、对苯乙烯基磺酸、邻苯乙烯基磺酸、α-对苯乙烯基乙酸、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、甲基丙烯酸羟丁酯、三羟甲基丙烷三甲基丙烯酸酯、富马酸、衣康酸、马来酸酐中的一种或两种以上。
6.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的不饱和反应型乳化剂为2-丙烯酰胺-2,2-二甲基乙磺酸钠、乙烯基聚乙二醇、烯丙基磺基烷氧基琥珀酸双酯钠盐、烯丙基-2丙基乙磺酸钠、乙烯基-2-丙基乙磺酸钠、聚氧化乙烯壬酚醚丙烯酸酯、十八烷基二甲基乙烯苯基氯化铵中的一种或两种以上；所述的常规乳化剂为OP类、苯乙基酚聚氧乙烯醚类、吐温类、脂肪醇聚氧乙烯醚类的一种或两种以上。
7.根据权利要求1所述的改性不饱和聚酯乳液，其特征在于，所述的改性不饱和聚酯乳液为半透明的纳米微乳液，其粒径为60～100nm。
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| CN108752601A (zh) * | 2018-05-28 | 2018-11-06 | 安徽汇利涂料科技有限公司 | 一种相反转法水性聚酯乳液的制备方法 |
| CN111349222A (zh) * | 2020-04-26 | 2020-06-30 | 江苏富菱化工有限公司 | 一种柔性不饱和聚酯树脂及其制备方法 |
| CN111393585A (zh) * | 2020-04-07 | 2020-07-10 | 湖南湘江关西涂料(长沙)有限公司 | 水性树脂及其制备方法与应用、水性涂料及涂膜制品 |
| CN111574697A (zh) * | 2020-04-30 | 2020-08-25 | 嘉宝莉化工集团股份有限公司 | 改性不饱和聚酯树脂及其制备方法和应用 |
| CN115322607A (zh) * | 2022-09-06 | 2022-11-11 | 安徽新大陆特种涂料有限责任公司 | 一种氯化聚酯合金耐热防腐涂料及其制备工艺 |
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| CN111393585A (zh) * | 2020-04-07 | 2020-07-10 | 湖南湘江关西涂料(长沙)有限公司 | 水性树脂及其制备方法与应用、水性涂料及涂膜制品 |
| CN111349222A (zh) * | 2020-04-26 | 2020-06-30 | 江苏富菱化工有限公司 | 一种柔性不饱和聚酯树脂及其制备方法 |
| CN111574697A (zh) * | 2020-04-30 | 2020-08-25 | 嘉宝莉化工集团股份有限公司 | 改性不饱和聚酯树脂及其制备方法和应用 |
| CN115322607A (zh) * | 2022-09-06 | 2022-11-11 | 安徽新大陆特种涂料有限责任公司 | 一种氯化聚酯合金耐热防腐涂料及其制备工艺 |
| CN115322607B (zh) * | 2022-09-06 | 2023-10-13 | 安徽新大陆特种涂料有限责任公司 | 一种氯化聚酯合金耐热防腐涂料及其制备工艺 |
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