CN110845726A - 一种低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的制备方法 - Google Patents

一种低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的制备方法 Download PDF

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CN110845726A
CN110845726A CN201810952702.8A CN201810952702A CN110845726A CN 110845726 A CN110845726 A CN 110845726A CN 201810952702 A CN201810952702 A CN 201810952702A CN 110845726 A CN110845726 A CN 110845726A
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polyamide polyamine
epichlorohydrin
chloropropanol
resin
low
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刘�文
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Guangdong Paparmaking Institute
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Guangdong Paparmaking Institute
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/02Polyamines
    • C08G73/028Polyamidoamines
    • C08G73/0286Preparatory process from polyamidoamines and epihalohydrins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular 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
    • C08G65/2618Macromolecular 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 nitrogen
    • C08G65/2633Macromolecular 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 nitrogen the other compounds containing amide groups

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

本发明公开了一种促进环氧氯丙烷与水溶性聚酰胺聚胺树脂反应速率的方法,通过加入一定类型的催化剂加速环氧氯丙烷与水溶性聚酰胺聚胺的反应,提高转化率,缩短反应时间,降低环氧氯丙烷的水解,从而制备出低氯丙醇含量的聚酰胺聚胺环氧氯丙烷树脂。

Description

一种低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的制备方法
技术领域
本发明涉及一种聚酰胺聚胺环氧氯丙烷树脂的制备方法,尤其是水性条件下催化加速环氧氯丙烷与聚酰胺聚胺反应的方法。
背景技术
环氧氯丙烷改性聚酰胺聚胺水性树脂在许多领域涉及,由于反应过程的复杂性,为了提高转化率,往往需要添加过量的环氧氯丙烷或提高反应温度或者延长反应时间,从而导致在反应过程中环氧氯丙烷大量水解,生成毒性物质氯丙醇。生成后在产品中的氯丙醇去除难度大、成本高,并且也会影响产品的稳定性。因此,需要找到一种合适的工艺,在低环氧氯丙烷用量、低反应温度、短的反应时间内,提高反应转化率,减少环氧氯丙烷的水解,减低产品中氯丙醇的含量。发明内容
本发明公开了一种引入催化剂的反应工艺,能够使得环氧氯丙烷在与低浓度聚酰胺聚胺水性树脂反应时,在保持转化率一致的情况下,减少用量、降低反应温度、缩短反应时间,优化降低环氧氯丙烷的水解的反应环境,达到制备低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的目的。
本发明的方法包括如下步骤:在反应前期将一定量的苄基三乙基氯化铵或苄基三甲基氯化铵催化剂溶解于聚酰胺聚胺型水溶性树脂中,然后再加入环氧氯丙烷进行反应。催化剂用量为胺摩尔含量的0.5%~10%,最佳用量为2%~4%。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
以聚酰胺聚胺水性树脂中胺摩尔含量为基数,按胺摩尔含量的5%计算苄基三乙基氯化铵或苄基三甲基氯化铵的摩尔用量;按胺摩尔含量的100%计算环氧氯丙烷的摩尔用量。
将以上用量的苄基三乙基氯化铵或苄基三甲基氯化铵溶解于浓度为25%的聚酰胺聚胺水性树脂中,加入环氧氯丙烷,在70℃下保温反应至所需粘度。
与不加催化剂的对比,达到300cp的粘度,反应时间可缩短30min。
实施例2
以聚酰胺聚胺水性树脂中胺摩尔含量为基数,按胺摩尔含量的8%计算苄基三乙基氯化铵或苄基三甲基氯化铵的摩尔用量;按胺摩尔含量的80%计算环氧氯丙烷的摩尔用量。
将以上用量的苄基三乙基氯化铵或苄基三甲基氯化铵溶解于浓度为20%的聚酰胺聚胺水性树脂中,加入环氧氯丙烷,在60℃下保温反应至所需粘度。
与不加催化剂的对比,达到250cp的粘度,反应时间可缩短25min。

Claims (7)

1.一种低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的制备方法,其特征在于:在反应前期将一定量的苄基三乙基氯化铵或苄基三甲基氯化铵催化剂溶解于聚酰胺聚胺型水溶性树脂中,然后再加入环氧氯丙烷进行反应。
2.根据权利要求1 所述的一种低氯丙醇聚酰胺聚胺环氧树脂的制备方法的制备方法,其特征在于使用的催化剂为苄基三乙基氯化铵或苄基三甲基氯化铵。
3.根据权利要求1 所述的一种低氯丙醇聚酰胺聚胺环氧树脂的制备方法的制备方法,其特征在于催化剂用量为胺摩尔含量的0.5%~10%。
4.根据权利要求1 所述的一种低氯丙醇聚酰胺聚胺环氧树脂的制备方法的制备方法,其特征在于催化剂用量最佳为胺摩尔含量的2%~4%。
5.根据以上工艺可制备低氯丙醇型聚酰胺聚胺环氧氯丙烷树脂。
6.根据以上工艺制备的聚酰胺聚胺环氧氯丙烷树脂可用于作为造纸湿强剂。
7.根据以上工艺制备的聚酰胺聚胺环氧氯丙烷树脂可用于作为阳离子乳化剂,如AKD阳离子乳化剂。
CN201810952702.8A 2018-08-21 2018-08-21 一种低氯丙醇聚酰胺聚胺环氧氯丙烷树脂的制备方法 Pending CN110845726A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116289311A (zh) * 2023-03-29 2023-06-23 浙江百斯特化工有限公司 一种高稳定性akd施胶剂的制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116289311A (zh) * 2023-03-29 2023-06-23 浙江百斯特化工有限公司 一种高稳定性akd施胶剂的制备方法
CN116289311B (zh) * 2023-03-29 2023-09-29 浙江百斯特化工有限公司 一种高稳定性akd施胶剂的制备方法

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