CN112961288B - 一种降粘型涂料分散剂的制备方法以及降粘型涂料分散剂 - Google Patents
一种降粘型涂料分散剂的制备方法以及降粘型涂料分散剂 Download PDFInfo
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- 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
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Abstract
本发明提供一种降粘型涂料分散剂的其制备方法以及降粘型涂料分散剂，所述聚醚类分散剂主要由以下几种材料制备而成：69.70‑73.52份醇头、136.31‑143.88份环状单体、0.6‑2.0份催化剂、154.99‑163.60份酸类物质、5.4‑7.9份还原剂、8.6‑11.3份引发剂、7.3‑9.7份中和剂、3.8‑5.7份链转移剂，其余为去离子水。本发明以聚醚与酸作为反应原材料，在制备分散剂的过程中，设置一定的酸醚比，合理地调控分散剂分子的空间构型，提升分散剂的性能，使得涂料浆体的流动度提高，因此在原料的份数选取上的控制十分重要，制备得到的分散剂也有着更优异的性能。
Description
技术领域
本发明属于分散剂技术领域，涉及到涂料的分散领域，具体是一种用聚醚合成的降粘型涂料分散剂。
背景技术
分散剂是一种能使固体颗粒均匀分散于水等介质中的物质。分散剂广泛应用在化工领域，常见分散剂多用于材料生产和使用过程中，帮助物料颗粒与介质混合形成均匀稳定的悬浮液。目前来看，在水溶液中使用的分散剂一般为高分子电解质或聚羧酸及其衍生物，这类分散剂存在的问题是分散剂分子柔顺性不高，容易增加了物料颗粒的粘性，导致生产使用中容易在设备内形成沉淀，影响设备使用。
公开号为CN110607090A的中国专利申请公开了一种水性涂料用高分子分散剂及其制备方法。该发明公开了一种水性涂料用高分子分散剂及其制备方法，该高分子分散剂由苯乙烯-马来酸酐共聚物、乙二醇乙醚和聚乙二醇聚合而成，其制备方法包括以下步骤；将苯乙烯-马来酸酐共聚物、乙二醇乙醚、聚乙二醇和溶剂加入反应釜，再加入引发剂和中和剂水溶液，60～120℃恒温反应2～12h。该发明的高分子分散剂的结构中含有苯环、羟基等多个锚固基团，可以与颜料表面发生强吸附作用，对无机颜料和有机颜料均具有优异的分散效果。
公开号为CN109486271A的中国专利申请公开了一种涂料有机分散剂及其制备方法。该发明公开了一种涂料有机分散剂，由以重量份为单位的下列各组分制备而成：99％的丙烯酸144份，30％的过氧化氢33.2份，42％的液碱191份，0.15％的硫酸铜溶液11.5份，100份的去离子水。将硫酸铜溶液和去离子水注入合成容器中，启动搅拌器，升温至75～85℃后，同时滴加丙烯酸、过氧化氢和75％的配料量的液碱，三种液体均控制在两小时内滴完，滴加完毕后立即冷却至60度以下，加入剩下的液碱，50℃温度条件下反应2～4个小时，反应结束后，经200目尼龙网过滤，称量包装入库。该发明采用硫酸铜作为链转移剂，以过氧化氢作为引发剂，以部分中和来控制分子量，具有分子量易控制、不含有机溶剂、反应浓度高、工艺简单反应周期短、低温存放不析出结晶物等优点。
公开号为CN106916480A的中国专利申请公开了一种水性涂料分散剂。该发明公开了一种水性涂料分散剂，由以下成分制成，丙烯酸、甲基丙烯酸甲酯、醋酸丁酯、高分子羧酸聚合物、聚醚改性聚硅氧烷、氧化铬、滑石粉、乙二醇、有机溶剂、引发剂、亚硫酸钠、中和剂；该发明分散剂能够降低水性涂料的表面张力,增强对颜料颗粒的润湿作用,使颜料颗粒在液相中稳定的分散，并且能够与涂料表面基团迅速牢固的结合,使颜料粒子稳定的悬浮在水溶剂中，使颜料获得较好的分散，达到最佳的分散效果，通过添加氧化铬、滑石粉，来提高分散效果和分散速度。
区别以上专利，本发明所制备的是一种降粘型涂料分散剂针对现有分散剂的所存在的不足，提升了分散剂分子的柔顺性，提高了分散剂分子对固体颗粒的包覆面积，降低固体颗粒的粘性，增强分散剂的分散性能。
发明内容
本发明提供一种降粘型涂料分散剂的制备方法以及降粘型涂料分散剂，制备的分散剂拥有比普通分散剂优异的性能，且制备方法简单，成本低、稳定性好。
本发明的发明构思如下：本发明使用带双键的醇头和环状单体加聚得到聚醚，再由聚醚与酸反应合成得到分散剂，选取聚醚作为制备分散剂的原料的目的是利用聚醚中的醚键使分散剂分子有更好的柔韧性与亲水性，同时增加了分散剂分子与涂料颗粒结合后的包覆面积，起到了更好的空间位阻作用，降低了涂料颗粒的粘性。因此本发明的分散剂的分散性能优于其他分散剂的分散性能，同时也增强了涂料分子的其他性能。
为解决以上问题，本发明的技术方案如下：
一种降粘型涂料分散剂的制备方法，该方法包括如下步骤：
使醇头和环状单体在催化剂的作用下合成聚醚；使所述聚醚在还原剂、引发剂、链转移剂的作用下与酸类物质反应，制得聚醚分散剂；以及在所述聚醚分散剂中加入中和剂，制得降粘型涂料分散剂。
以原料总量为1000质量份计，各原料的用量为：醇头69.70-73.52质量份、环状单体136.31-143.88质量份、酸类物质154.99-163.60质量份、催化剂0.6-2.0质量份、还原剂5.4-7.9质量份、引发剂8.6-11.3质量份、链转移剂3.8-5.7质量份、中和剂7.3-9.7质量份、其余为水。
作为优选，所述的醇头为4-乙烯基苯基-甲醇。
作为优选，所述的环状单体为环氧乙烷和/或环氧丙烷。
作为优选，所述的酸类物质为丙烯酸。
进一步，所述降粘型涂料分散剂固含量为37-43％，最优为40％。
固含量，即涂料分散剂中除水之外其他原料质量总和在总量为1000的溶液中的质量百分数。固含量＝(聚醚醇头+环状单体+催化剂+酸类物质+还原剂+引发剂+链转移剂+中和剂)/1000*100％。
更进一步，制备所述降粘型涂料分散剂的各原料的总质量份数为1000份。
作为优选，所述的酸醚质量比为1:(1.25-1.41)。
“酸醚质量比”中的“酸”是指所述酸类物质，“酸醚质量比”中的“醚”是指本发明中使醇头与环状单体聚合而成的聚醚。
作为优选，所述的催化剂为无水氯化铝、三氟化硼、浓硫酸、卤化氢、芳基磺酸、无机磷化合物、羧酸、有机阳离子交换树脂和苯酚铝、氢氧化钠、氢氧化钾、氰化钠、四氢铝锂、三氟化硼乙烯醚、DMC中的一种或几种组成，最优选为质量比为1:3的无水氯化铝和四氢铝锂的组合物。
作为优选，所述的还原剂为连二亚硫酸钠、抗坏血酸、甲醛合次硫酸氢钠、麦芽糖糊精、亚硫酸氢钠、焦亚硫酸钠、次亚磷酸钠中的一种或几种组成，最优选为质量比为1:1的连二亚硫酸钠和焦亚硫酸钠的组合物。
作为优选，所述的引发剂为过硫酸铵、偶氮二异丁腈、过氧化二碳酸二异丙酯、过氧化苯甲酰(BPO)、过氧化二叔丁基(DTBP)、过氧化二碳酸二环己酯中的一种或几种组成，最优选为质量比为3:1的偶氮二异丁腈和过氧化苯甲酰的组合物。
作为优选，所述的链转移剂为巯基乙酸、巯基丙酸、巯基乙醇、巯基丙醇中的一种或几种组成，最优选为质量比为2:3的巯基丙酸和巯基乙醇的组合物。
作为优选，所述的中和剂为氢氧化钠、氢氧化钾、碳酸钠、碳酸氢钠、碳酸钾、甲醇钠、乙醇钠、乙醇胺、二乙醇胺、三乙醇胺、三异丙醇胺中的一种或几种组成，最优选为质量比为1:4的乙醇钠和乙醇胺的组合物。
作为一种优选，降粘型涂料分散剂制备过程依次包括如下操作步骤：
步骤一：在装有搅拌器、温度计的高压反应釜中加入68.70-72.52份醇头和0.6-2.0份催化剂，氮气置换3次后开始抽真空至表压-0.098MPa，然后升温至120℃开始脱水1～2h，测氧含量，待氧含量合格后，降温至115℃。开始向反应釜通入环状单体，向反应釜中通入58.80-62.07份环氧乙烷和77.51-81.81份环氧丙烷，控制压力小于0.4MPa，通完后于115-130℃保温老化至负压，降温出料，得到粗聚醚。
步骤二：将粗聚醚置于反应釜中，氮气负压置换3次，升温至120-140℃搅拌1.5-2.5h，降温至90℃，后加入蒸馏水搅拌1-1.5h，边抽真空边升温至120℃，得到成品聚醚。
步骤三：将制得的成品聚醚加入反应釜中，采用水浴加热升温至45℃。将5.4-7.9份还原剂、8.6-11.3份引发剂、3.8-5.7份链转移剂和水配制成A液，将154.99-163.60份酸类物质、0.5-1.0份醇头和水配制成B液，用滴加泵将A、B液滴加至反应釜中，其中A液滴加1-1.5小时，B液滴加1.5-2小时。滴加完A、B液后保温1小时制得聚醚类分散剂。
步骤四：将7.3-9.7份中和剂加入制得的聚醚类分散剂中并补水至总质量为1000，即得到所需的聚醚类分散剂溶液。
与现有技术相比，本发明的优点和有益效果在于：
1、本发明采用聚醚作为合成分散剂的单体，聚醚能增加分散剂分子支链的柔性，增强分散剂分子对涂料颗粒的包覆性，提升了分散剂的空间位阻作用。
2、本发明使用的原料酸醚比为4.2:1，这种酸醚比能很好地改善用400分子量聚醚合成的分散剂的性能，合成出侧链密度较高的分散剂分子，增强分散剂对涂料颗粒的分散性能，有效地增加涂料颗粒的净浆流动度。
3、本发明所使用的醇头为4-乙烯基苯基-甲醇，双键与羟基处在苯环对位，双键的活性较好，反应的可控性更高，并且可以减少引发剂用量，降低反应成本。
4、本发明的散剂分子粘度小，稳定性高，拥有优秀的分散性能，散剂增强了涂料涂层的韧性，还有着优良的降粘性能。该分散剂大分子链中以醚键连接，适当提升了分散剂分子的柔顺性，提高了分散剂分子对固体颗粒的包覆面积，降低固体颗粒的粘性，因此本发明相较于聚羧酸分散剂有着更加优异的分散性能。
5、本发明使用醇头与环状单体制备聚醚，再利用聚醚与酸类物质进行反应制得分散剂，其中本发明采用水洗精制法制备聚醚，得到的聚醚纯度较高。制备方法简便，生产过程及设备要求低，其工艺流程简便适合大量生产分散剂并且所生产的分散剂适合大面积使用。
附图说明
图1为实施例4与广州厚洹化学助剂有限公司HH2190水性分散剂试样稳定性图。
图左的试样为实施例4的试样、图右的试样为广州厚洹HH2190水性分散剂试样。
具体实施方式
下面，将结合具体实施例和对比例对本发明的技术方案和有益效果做进一步的详细说明，但应理解，以下实施例不应在任何程度上被理解为对本申请权利要求书所请求保护范围的限制。在实施例和对比例中，如无特殊说明，“份”是指“质量份”，“比”是指“质量比”。固含量，即涂料分散剂中除水之外其他原料质量总和在总量为1000的溶液中的质量百分数。
实施例1
一种降粘型涂料分散剂的制备方法及降粘型涂料分散剂，由下述各组分聚合而成，原料总质量为1000份，各组分包括：
4-乙烯基苯基-甲醇69.22份、环氧乙烷59.42份、环氧丙烷79.91份、质量比为1:3的无水氯化铝和四氢铝锂的组合物1.2份、丙烯酸158.37份、质量比为1:1的连二亚硫酸钠和焦亚硫酸钠的组合物5.9份、质量比为3:1的偶氮二异丁腈和过氧化苯甲酰的组合物9.2份、质量比为2:3的巯基丙酸和巯基乙醇的组合物4.3份、质量比为1:4的乙醇钠和乙醇胺的组合物7.8份、其余为水，总质量为1000份。
一种降粘型涂料分散剂及其制备方法，制备过程依次包括如下操作步骤：
步骤一：在装有搅拌器、温度计的高压反应釜中加入69.22份4-乙烯基苯基-甲醇和质量比为1:3的无水氯化铝和四氢铝锂的组合物1.2份，氮气置换3次后开始抽真空至表压-0.098MPa，然后升温至120℃开始脱水1.2h，测氧含量，待氧含量合格后，降温至115℃。开始向反应釜通入59.42份环氧乙烷和79.91份环氧丙烷，控制压力小于0.4MPa，通完后于116℃保温老化至负压，降温出料，得到粗聚醚。
步骤二：将粗聚醚置于反应釜中，氮气负压置换3次，升温至125℃搅拌1.7h，降温至90℃，后加入蒸馏水搅拌1h，边抽真空边升温至120℃，得到成品聚醚。
步骤三：将制得的成品聚醚加入反应釜中，采用水浴加热升温至45℃。将5.9份质量比为1:1的连二亚硫酸钠和焦亚硫酸钠的组合物、9.2份质量比为3:1的偶氮二异丁腈和过氧化苯甲酰的组合物、4.3份质量比为2:3的巯基丙酸和巯基乙醇的组合物和水配制成A液，将158.37份丙烯酸、1.0份4-乙烯基苯基-甲醇和水配制成B液，用滴加泵将A、B液滴加至反应釜中，其中A液滴加1.1小时，B液滴加1.7小时。滴加完A、B液后保温1小时制得聚醚类分散剂。
步骤四：将7.8份质量比为1:4的乙醇钠和乙醇胺的组合物加入制得的聚醚类分散剂中并补水至总质量为1000，即得到所需的分散剂溶液。
实施例2-6
实施例2-6用于说明本发明的降粘型涂料分散剂的制备方法以及由该方法制备的降粘型涂料分散剂。
在本实施例中，除了原料的组分及用量如表1中所示、步骤中的参数如表2中所示之外，使用与实施例1相同的方法，制得实施例2-6的降粘型涂料分散剂，其中实施例4为最优选。实施例1作为与实施例4相对比的试样，来说明固含量的优选。
对比例1-2
对比例1-2作为与实施例4相对比的试样，来说明酸醚质量比的优选。
在对比例中，除了原料的组分及用量如表1中所示、步骤中的参数如表2中所示之外，使用与实施例1相同的方法，制得对比例1-2的降粘型涂料分散剂。
对比例3为广州厚洹化学助剂有限公司HH2190水性分散剂。
将热塑性丙烯酸树脂与实施例1-6及对比例1-3的分散剂混合进行检测，得到下表3。粘结强度、断裂延伸率根据GB_T16777_2008的标准进行测试，黏度根据ASTMD4287-2000的标准进行检测。稳定性的测量方法是将分散剂溶液在25℃的温度下静置15天，测得沉淀厚度。
表1
表2
| 粘结强度(MPa) | 稳定性(25℃，15d) | 黏度(MPa*s) | 断裂延伸率(％) | |
| 对比例1 | 0.6 | 7.6mm沉淀 | 705 | 550 |
| 对比例2 | 0.5 | 8.3mm沉淀 | 716 | 565 |
| 对比例3 | 0.5 | 10.6mm沉淀 | 800 | 540 |
| 实例1 | 1.0 | 3.5mm沉淀 | 530 | 630 |
| 实例2 | 0.8 | 3.7mm沉淀 | 495 | 600 |
| 实例3 | 0.9 | 3.4mm沉淀 | 525 | 610 |
| 实例4 | 1.2 | 3.3mm沉淀 | 480 | 660 |
| 实例5 | 0.8 | 3.6mm沉淀 | 490 | 655 |
| 实例6 | 1.1 | 3.5mm沉淀 | 510 | 645 |
表3
由上表可知，本发明的分散剂分子粘度小，稳定性高，拥有优秀的分散性能，并且其性能优于广州厚洹化学助剂有限公司HH2190水性分散剂。结合实例4可以明显看出本发明的分散剂增强了涂料涂层的韧性，除了分散剂稳定性强、分散效果好外，还有着优良的降粘性能。此外本发明的制备方法简便，对生产过程和设备要求低，适合大量生产和大面积使用。
Claims (9)
1.一种降粘型涂料分散剂的制备方法，其特征在于，该方法包括：使醇头和环状单体在催化剂的作用下合成聚醚；使所述聚醚在还原剂、引发剂、链转移剂的作用下与酸类物质反应，制得聚醚分散剂；以及在所述聚醚分散剂中加入中和剂，制得降粘型涂料分散剂，以原料总量为1000质量份计，各原料的用量为：醇头69.70-73.52质量份、环状单体136.31-143.88质量份、酸类物质154.99-163.60质量份、催化剂0.6-2.0质量份、还原剂5.4-7.9质量份、引发剂8.6-11.3质量份、链转移剂3.8-5.7质量份、中和剂7.3-9.7质量份，其余为水，所述醇头为4-乙烯基苯基-甲醇，所述环状单体为环氧乙烷和/或环氧丙烷，所述酸类物质为丙烯酸；酸醚质量比为1:(1.25-1.41)。
2.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述降粘型涂料分散剂中除水以外其他原料的用量为37-43质量％。
3.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述降粘型涂料分散剂中除水以外其他原料的优选用量为40质量％。
4.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述催化剂为无水氯化铝、三氟化硼、浓硫酸、卤化氢、芳基磺酸、无机磷化合物、羧酸、有机阳离子交换树脂和苯酚铝、氢氧化钠、氢氧化钾、氰化钠、四氢铝锂、三氟化硼乙烯醚、DMC中的一种或几种。
5.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述还原剂为连二亚硫酸钠、抗坏血酸、甲醛合次硫酸氢钠、麦芽糖糊精、亚硫酸氢钠、焦亚硫酸钠、次亚磷酸钠中的一种或几种组成。
6.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述引发剂为过硫酸铵、偶氮二异丁腈、过氧化二碳酸二异丙酯、过氧化苯甲酰(BPO)、过氧化二叔丁基(DTBP)、过氧化二碳酸二环己酯中的一种或几种组成。
7.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述链转移剂为巯基乙酸、巯基丙酸、巯基乙醇、巯基丙醇中的一种或几种组成。
8.根据权利要求1所述的降粘型涂料分散剂的制备方法，其特征在于，所述中和剂为氢氧化钠、氢氧化钾、碳酸钠、碳酸氢钠、碳酸钾、甲醇钠、乙醇钠、乙醇胺、二乙醇胺、三乙醇胺、三异丙醇胺中的一种或几种组成。
9.一种由权利要求1-8中任意一项所述方法制得到的降粘型涂料分散剂。
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