CN112375601A - 一种超小粒径硬脂酸钙的合成方法 - Google Patents

一种超小粒径硬脂酸钙的合成方法 Download PDF

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CN112375601A
CN112375601A CN202011227423.9A CN202011227423A CN112375601A CN 112375601 A CN112375601 A CN 112375601A CN 202011227423 A CN202011227423 A CN 202011227423A CN 112375601 A CN112375601 A CN 112375601A
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陈娓
曹广宇
施庆
徐晓峰
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Changshu Juhe Chemical Co ltd
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Abstract

本发明属于涂布润滑剂制备技术领域，具体涉及一种超小粒径硬脂酸钙的合成方法。该方法包括如下步骤：向融溶状态下的硬脂酸中加入氢氧化钙水溶液、乳化剂A和乳化剂B，然后恒温反应2‑5h，反应结束后加入消泡剂和分散剂，均质至产品粒径<5un占比98％以上即可停止，加入杀菌剂，混匀，出料。本发明提供的硬脂酸钙具有优异的安定性，试验结果表明，常温1年不分层，60℃烘箱6个月不分层。

Description

一种超小粒径硬脂酸钙的合成方法
技术领域
本发明属于涂布润滑剂制备技术领域，具体涉及一种超小粒径硬脂酸钙的合成方法。
背景技术
随着涂布机的更新换代，涂布速度越来越快，为了使涂料能适应高涂布速度，涂布时能迅速分散，并具有较好的流平性，需要在涂料中添加涂布润滑剂。一方面，涂布润滑剂能降低湿涂料的界面张力，使流体润滑，改善湿涂层的流动性，使其在涂布时易流平铺展；在干燥过程中使水分与涂料易分离；降低纸张表面与滚轴接触时的表面摩擦力；提高干湿涂层的塑性，提高干涂层的剥离性；减少各种辊轴的污染，改善因涂层干裂而引起的起毛掉粉现象，提高涂布纸的可裁切性能等。另一方面，在实际生产过程中，涂布润滑剂可以从涂层迁移到压光软辊的表面，使软辊被润滑剂薄层所覆盖，降低涂料层对软辊的粘附程度；还可以通过减轻涂料和涂布装置之间的摩擦力，改善涂料在涂布过程中的使用性能，减少涂布过程中的“粘缸”现象。因此，涂布润滑剂成为造纸涂料中应用较广，使用量较多的一种重要的功能性助剂。
发明内容
为了克服现有技术中存在的上述问题，本发明的目的在于提供一种超小粒径硬脂酸钙合成方法。
为了实现上述发明目的，本发明的其中一个技术方案为：
一种超小粒径硬脂酸钙合成方法，其包括如下步骤：
向融溶状态下的硬脂酸中加入氢氧化钙水溶液、乳化剂A和乳化剂B的混合液，然后恒温反应2-5h，反应结束后加入消泡剂和分散剂，均质至产品粒径<5un占比98％以上即可停止，加入杀菌剂，混匀，出料；其中乳化剂A由如下重量份的各物质组成：
乳化剂A
Figure BDA0002764031310000011
Figure BDA0002764031310000021
乳化剂B由如下重量份的各组成组成：
Figure BDA0002764031310000022
优选地，氢氧化钙水溶液、乳化剂A和乳化剂B的混合液是以缓慢滴入的方式加入，滴入时间控制在1-3h。
所述的氢氧化钙水溶液是由5-200g氧化钙与10-1000g水配制而成。
优选地，融溶状态下的硬脂酸是指将硬脂酸加热至90C。
优选地，所述消泡剂的含量为相当于硬脂酸加入量的0.1-2wt％。
优选地，所述消泡剂为CL-66、CL-33中的一种或两种。此两种消泡剂购于江苏四新科技应用研究所股份有限公司。
优选地，所述杀菌剂为卡松、聚六亚甲基双胍盐酸盐和羟乙基六氢均三嗪的一种或两种。
优选地，所述杀菌剂的含量为相当于硬脂酸加入量的0.1-4wt％。
优选地，所述分散剂为丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物。
进一步优选地，丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物的重均分子量为10000-100000。
优选地，所述分散剂的含量为相当于硬脂酸加入量的0.1-3wt％。
优选地，所述均质是指在20-50Mpa压力下进行。
优选地，所述均质时搅拌转速为20-500转/min。
有益效果
本发明与现有技术相比，具有如下优点：
1、本发明提供一种超小粒径的硬脂酸钙，产品粒径为3-5un(占比95％以上)
2、该产品的粘度适中，经检测为10-100cp。
3、本发明提供的硬脂酸钙具有优异的安定性，试验结果表明，常温1年不分层，60℃烘箱6个月不分层。
具体实施方式
下面通过具体实施例对本发明的方法进行说明，以使本发明技术方案更易于理解、掌握，但本发明并不局限于此。下述实施例中所述实验方法，如无特殊说明，均为常规方法；所述试剂和材料，如无特殊说明，均可从商业途径获得。
实施例1
一种超小粒径硬脂酸钙合成方法，其包括如下步骤：
S1在三口烧瓶内加入硬脂酸150g加热至90℃，完全溶解后滴入氢氧化钙水溶液(由100g氧化钙和100g水制成)、乳化剂A和乳化剂B的混合液，滴入时间为60分钟，开始恒温2h，恒温结束加入消泡剂CL-33 15g(相当于硬脂酸的0.1％)、分散剂丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物15g(分子量10000，相当于硬脂酸的0.1％，浓度为10％水溶液，预先采用30Mpa压力进行均质)；
S2分散剂均质完成后将上述反应液在20Mpa压力进行均质，至产品粒径<5un占比98％以上即可停止，加入杀菌剂，混匀，出料；
其中乳化剂A由如下重量份的各物质组成：
乳化剂A
Figure BDA0002764031310000031
乳化剂B由如下重量份的各组成组成：
Figure BDA0002764031310000041
实施例2
一种超小粒径硬脂酸钙合成方法，其与实施例1的区别在于：乳化剂A由如下重量份的各物质组成：
乳化剂A
Figure BDA0002764031310000042
实施例3
一种超小粒径硬脂酸钙合成方法，其与实施例1的区别在于：
乳化剂B由如下重量份的各组成组成：
Figure BDA0002764031310000043
实施例4
一种超小粒径硬脂酸钙合成方法，其与实施例1的区别在于：
乳化剂B由如下重量份的各组成组成：
Figure BDA0002764031310000044
Figure BDA0002764031310000051
实施例5
一种超小粒径硬脂酸钙合成方法，其与实施例1的区别在于：
步骤S1中加入消泡剂15g(相当于硬脂酸的0.1％，其中，CL-33 7.5g、CL-667.5g)。
实施例6
一种超小粒径硬脂酸钙合成方法，其与实施例1的区别在于：
步骤S1中加入的分散剂丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物15g(分子量100000，浓度为10％水溶液，预先采用30Mpa压力进行均质)。
性能实验
1、粒径测试
采用马尔文激光粒度分析仪对各实施例提供的超小粒径硬脂酸钙的粒径进行检测，结果如下表1。
表1
产品粒径/um 3-5um粒径占比％
实施例1 3.125 95.83
实施例2 3.346 96.12
实施例3 3.227 96.03
实施例4 3.125 96.03
实施例5 3.654 96.27
实施例6 3.276 96.31
2、安定性测试
测试方法
将各实施例提供的超小粒径硬脂酸钙置于250ml透明玻璃瓶内分别至于常温25℃与60℃烘箱内进行观察。测试结果如下表2-3。
表2常温下硬脂酸钙的安定性能
Figure BDA0002764031310000061
表3 60℃烘箱条件下硬脂酸钙的安定性能
Figure BDA0002764031310000062
此外，对各样品在常温25℃观察一年未见水层，60℃烘箱内观察6个月未见水层，成品分析结果与实验开始时检测结果相同。
最后应当说明的是，以上内容仅用以说明本发明的技术方案，而非对本发明保护范围的限制，本领域的普通技术人员对本发明的技术方案进行的简单修改或者等同替换，均不脱离本发明技术方案的实质和范围。

Claims (10)

1.一种超小粒径硬脂酸钙合成方法，其特征在于，包括如下步骤：
向融溶状态下的硬脂酸中加入氢氧化钙水溶液、乳化剂A和乳化剂B，然后恒温反应2-5h，反应结束后加入消泡剂和分散剂，均质至产品粒径<5un占比98％以上即可停止，加入杀菌剂，混匀，出料；其中乳化剂A由如下重量份的各物质组成：
乳化剂A
Figure FDA0002764031300000011
乳化剂B由如下重量份的各组成组成：
Figure FDA0002764031300000012
2.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，融溶状态下的硬脂酸是指将硬脂酸加热至90C。
3.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述消泡剂的含量为相当于硬脂酸加入量的0.1-2wt％。
4.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述消泡剂为CL-66、CL-33中的一种或两种。
5.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述杀菌剂为卡松、聚六亚甲基双胍盐酸盐和羟乙基六氢均三嗪的一种或两种。
6.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述杀菌剂的含量为相当于硬脂酸加入量的0.1-4wt％。
7.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述分散剂为丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物。
8.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，丙烯酸与N,N二甲基丙基三甲基氯化铵的共聚物的重均分子量为10000-100000。
9.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述分散剂的含量为相当于硬脂酸加入量的0.1-3wt％。
10.根据权利要求1所述的超小粒径硬脂酸钙合成方法，其特征在于，所述均质是指在20-50Mpa压力下进行。
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