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Polyaspartic acid synthesized by microwave half-solvent method

A polyaspartic acid and solvent technology, applied in the field of polyaspartic acid synthesis, can solve the problems of difficult separation of solvent and product, low molecular weight of product, poor scale inhibition performance, etc. The effect of stable product performance

Active Publication Date: 2012-11-28
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can solve the low molecular weight of the product existing in the existing microwave radiation synthesis method, and the 3 Defects such as poor scale inhibition performance and difficult separation of solvent and product

Method used

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  • Polyaspartic acid synthesized by microwave half-solvent method

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specific Embodiment approach 1

[0010] Specific embodiment one: the structural formula of the polyaspartic acid of the present embodiment is The range of p+q is 30-300. The optimum range of p+q in this embodiment is 30-100.

specific Embodiment approach 2

[0011] Specific embodiment two: this embodiment synthesizes polyaspartic acid according to the following steps: the synthesis process is divided into 2 steps, the first step is raw material with maleic anhydride or fumaric acid and ammonia or ammonium salt, wherein the ammonium salt is ammonium carbonate, Ammonium bicarbonate, ammonium sulfate, ammonium hydrogen sulfate, ammonium chloride, ammonium phosphate, ammonium hydrogen phosphate or diammonium hydrogen phosphate, the stoichiometric ratio of maleic anhydride or fumaric acid to ammonia water or ammonium salt is 0.01 to 99.9, Using microwave radiation, under the conditions of microwave frequency of 915±50MHz or 2450±50MHz and microwave power of 200~20000W, a small amount of solvent is added to the reactant, and the reaction is irradiated for 1~40min. During the reaction, all the solvent is recovered to obtain a small molecular weight The polysuccinimide (PSI-I), wherein the ratio of the stoichiometric number of the solvent ...

specific Embodiment approach 3

[0013] Specific embodiment three: add 20g maleic anhydride in the single mouthed round bottom flask, according to the stoichiometric number of maleic anhydride and ammonium bicarbonate acid is 1: 1.1, add 25ml dimethylformamide, microwave power is 800W radiation 3min, Afterwards, 1200W irradiated for 3 minutes to obtain a light brown fluffy product. At 3 minutes, all dimethylformamide was recovered, and 40 ml of 3mol / L NaOH was added to the product to dissolve the product. The pH of the solution was adjusted to be acidic, and the product was filtered. The filtrate was added to 250ml of absolute ethanol, the precipitate was collected, and vacuum-dried at 70°C to obtain polyaspartic acid, the calculated yield was 96.23%, and the weight-average molecular weight reached 4882. 3 The scale inhibition rate reaches 99.12%.

[0014] Specific embodiment four: add fumaric acid 20g in single-port round bottom flask, the ratio of fumaric acid and ammonium bicarbonate stoichiometric number ...

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Abstract

The invention relates to a synthesis method of a high-molecular-weight polyaspartic acid, particularly a polyaspartic acid synthesized by a microwave half-solvent method. The invention aims to overcome the defects of low molecular weight of the product, unstable antiprecipitation property, difficulty in solvent separation and the like in the existing microwave synthesis method. The synthetic process comprises the following two steps: 1. by using maleic anhydride or fumaric acid and ammonia water or ammonium salt as raw materials, adding a small amount of solvent, and radiating with microwaves, of which the frequency is 915+ / -50 MHz or 2450+ / -50 MHz and the power is 200-20000W, for 1-40 minutes to synthesize the low-molecular-weight polysuccinimide (PSI-I), wherein the solvent is recycled completely; and 2. by using the PSI-I as the raw material, radiating with microwaves, of which the frequency is 915+ / -50 MHz or 2450+ / -50 MHz and the power is 400-50000W, under the condition of no solvent for 1-30 minutes to synthesize the high-molecular-weight polysuccinimide (PSI-II), and hydrolyzing the PSI-II to obtain the high-molecular-weight polyaspartic acid. The invention has the advantages of simple technique, no need of solvent separation, obviously higher product molecular weight, obviously higher antiprecipitation property, high reaction speed, high yield, energy saving, low pollution and the like.

Description

Technical field: [0001] The invention relates to a method for synthesizing higher molecular weight polyaspartic acid, in particular to a method for synthesizing polyaspartic acid used as a water treatment agent. Background technique: [0002] Polyaspartic acid is an internationally recognized "green chemical". Polyaspartic acid with a certain molecular weight not only has a good inhibitory performance on calcium sulfate, barium sulfate, calcium carbonate, and calcium phosphate scaling, but also has a good effect on CO 2 Corrosion has a certain corrosion inhibition effect. The synthesis and application of polyaspartic acid has become a research hotspot in the field of water treatment agents in recent years. [0003] Currently disclosed polyaspartic acid synthesis methods are many, and can be divided into two classes according to the raw materials used: one is using L-aspartic acid monomer as raw material; the other is using unsaturated dicarboxylic acid containing four carbo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C02F5/12
Inventor 张玉玲张敬红赵毅张泽润谢淑兰罗玲童
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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