Method for performing catalyzed synthesis on polyaspartic acid through one-step process of novel solid acid catalyst

A solid acid catalyst, a technology of polyaspartic acid, which is applied in the field of one-step catalytic synthesis of polyaspartic acid with a novel solid acid catalyst, can solve the problems of tediousness, unsuitability for large-scale production, and low molecular weight of polyaspartic acid. , to achieve the effect of improving molecular mass, environmental protection and pollution-free catalytic performance, and simple post-treatment process

Active Publication Date: 2017-05-10
NINGBO ZHETIE JIANGNING CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the polyaspartic acid obtained by the above method has a low molecular weight, and the process is carried out step by step, which is cumbersome and not suitable for large-scale production.

Method used

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  • Method for performing catalyzed synthesis on polyaspartic acid through one-step process of novel solid acid catalyst
  • Method for performing catalyzed synthesis on polyaspartic acid through one-step process of novel solid acid catalyst
  • Method for performing catalyzed synthesis on polyaspartic acid through one-step process of novel solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Accurately take by weighing 98g maleic anhydride and put into the reactor, add 5mL deionized water in the reactor, pass into cooling water, then drip ammoniacal liquor with the speed of 5mL / min in the described reactor, the added The molar ratio of ammonia water and maleic anhydride is 1.3:1, raise the temperature to 80°C, react for 2h, after the reaction finishes, open the outlet valve, drain the water, then add 9.8g of acid-modified montmorillonite in the reaction kettle Remove the soil (modified by 85% phosphoric acid) and 25mL of liquid paraffin, cover the lid of the reaction kettle, tighten the screws, and then continue to increase the temperature to 200 ° C, feed nitrogen to increase the pressure to 5 MPa, react for 2 hours, and pass through cooling Cool with water, when it cools down to 50°C, open the reaction kettle, release the reaction liquid from the bottom while it is hot, pour out the liquid paraffin in the reaction liquid and recover it, and put the reddish...

Embodiment 2

[0037] Accurately weigh 98g maleic anhydride and put it into the reactor, add 15mL of deionized water into the reactor, pass into cooling water, then slowly add ammoniacal liquor dropwise in the reactor, the added ammoniacal liquor and maleic butene The mol ratio of diacid anhydride is 1.3:1, raises temperature to 60 ℃, reacts 3h, after reaction finishes, open outlet valve, discharge moisture, then add the acid-modified montmorillonite (sulfuric acid) of 19.6g in described reactor Modified) and 100mL of liquid paraffin, cover the lid of the reaction kettle, tighten the screws, then continue to raise the temperature to 160°C, feed nitrogen to increase the pressure to 6MPa, react for 4 hours, feed cooling water to cool, and wait to cool to At 40°C, open the reaction kettle, release the reaction liquid from the bottom while it is hot, pour out and recover the liquid paraffin in the reaction liquid, and place the reddish-brown viscous liquid in the reactor, add 20mL deionized water...

Embodiment 3

[0039]Accurately weigh 98g maleic anhydride and put it into the reactor, add 10mL deionized water into the reactor, pass into cooling water, then drip ammoniacal liquor at a rate of 4mL / min in the reactor, the added The molar ratio of ammonia water and maleic anhydride is 1.5:1, raise the temperature to 70°C, react for 2h, after the reaction finishes, open the outlet valve, drain the water, then add 19.6g of acid-modified Mongolian in the reaction kettle Remove soil (modified by hydrochloric acid) and 60mL of liquid paraffin, cover the lid of the reaction kettle, tighten the screws, and then continue to raise the temperature to 220 ° C, feed nitrogen to increase the pressure to 4 MPa, react for 2 hours, and feed cooling water to cool , when it is cooled to 60°C, open the reaction kettle, release the reaction liquid from the bottom while it is hot, pour out the liquid paraffin in the reaction liquid and recover it, and put the reddish-brown viscous liquid in the reactor, add 20m...

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Abstract

The invention relates to the field of macromolecular synthesis and discloses a method for performing catalyzed synthesis on polyaspartic acid through a one-step process of a novel solid acid catalyst. The method comprises the following steps: (1) adding maleic anhydride into a reactor, adding deionized water, introducing cooling water for cooling, dropwise adding ammonia water, and discharging water after the reaction is completed; (2) adding an acid modified montmorillonite catalyst and liquid paraffin into the reactor, heating to a polymerization temperature, introducing cooling water for cooling after the reaction, and discharging the reaction solution; and (3) pouring and recovering the liquid paraffin in the reaction solution, adding the obtained reddish brown viscous liquid into the reactor, adding deionized water into the reactor, filtering, precipitating the filtrate by using a precipitator, separating and drying to obtain the polyaspartic acid. With the adoption of the novel solid acid catalyst, the molecular weight of the polyaspartic acid can be improved. In addition, due to the addition of slightly excessive ammonia water, polymerization and hydrolysis reactions can be carried out in the same system, the synthetic process is simplified, and large-scale production is facilitated.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a method for synthesizing polyaspartic acid by a novel solid acid catalyst in one step. Background technique [0002] With the continuous development of modern industry, the pollution of water resources is becoming more and more serious, and the industrial water treatment agent market has also set off a "green revolution", which is developing in the direction of multi-function, non-toxic and high-efficiency. At present, the applied research on polyaspartic acid in the world has become a research hotspot in developed countries, and chemical companies in the United States, Japan and Germany are the most active in the research on polyaspartic acid. Donlar Corporation of the United States developed polyaspartic acid in the early 1990s. Because polyaspartic acid has very little environmental pollution and is biodegradable, it has great potential in the field of biodegradable water-sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1092
Inventor 童东绅韩艳瑞陈焕新胡军
Owner NINGBO ZHETIE JIANGNING CHEM
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