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Preparation method of polysuccinimide and polyaspartic acid

A technology of polysuccinimide and polysuccinic acid imide, which is applied in the field of chemical synthesis, can solve problems affecting product content and performance, low recycling rate, and complicated recycling, so as to achieve good product performance and high product quality , the effect of thorough response

Pending Publication Date: 2020-12-15
南京艾普拉斯生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aspartic acid, maleic anhydride and their derivatives are reacted in a liquid organic solvent, and the polymerization temperature is generally controlled at about 200°C. After a certain period of polymerization, an extractant is added to the mixed solution, and polysuccinimide becomes a precipitate from Precipitate in the solution, then purify, filter, dry, this process is also more loaded down with trivial details, the selected solvent includes sulfur-containing or oxygen-containing heteroatom cyclic organic compounds, such as cyclobutane, 1,3,5-trimethylbenzene, propylene carbonate , diethylbenzene and their mixtures, high-boiling alkanols and their mixtures, n-alkanes and their mixtures. Due to the low viscosity of these solvents in the later stage of the reaction, the more polysuccinimides produced by polymerization, resulting in a large amount of polysuccinimide The agglomeration of succinimide affects the complete progress of the reaction, and even terminates the reaction early, which in turn affects the content and performance of the product. In addition, the recovery of these solvents is relatively complicated, and it is harmful to a certain extent, and the reuse rate is low.

Method used

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  • Preparation method of polysuccinimide and polyaspartic acid
  • Preparation method of polysuccinimide and polyaspartic acid
  • Preparation method of polysuccinimide and polyaspartic acid

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preparation example Construction

[0032] The present application provides the first preparation method of polysuccinimide, and the preparation method includes the following steps.

[0033] Step 11: Providing the ammonium maleate salt.

[0034] Ammonium maleate can be provided first to prepare polysuccinimide through ammonium maleate.

[0035] Alternatively, the ammonium maleate finished product can be provided directly.

[0036] Of course, you can also make your own ammonium maleate. Specifically, ammonium maleate can be prepared by various methods.

[0037] For example, ammonium maleate can be obtained by reacting fumaric acid with an ammonia-containing compound. Alternatively, the nitrogen-containing compound and fumaric acid may be reacted for a first time at a second temperature to obtain the ammonium maleate salt. Wherein, the second temperature may be 70-100°C, such as 75°C, 80°C, 85°C, 90°C, etc. The first time may be 1-5h, such as 2h, 3h, 4h and so on.

[0038] For another example, maleic acid an...

Embodiment 1

[0086] (1) Preparation of polysuccinimide

[0087] Add 196g of maleic anhydride to a 2000mL four-necked bottle, then add 200g of deionized water, stir and heat up to 60°C for hydrolysis. Then, 85 g of 28% (mass fraction) ammonia water was slowly added dropwise to the hydrolyzed solution. After the dropwise addition, the solution was warmed up to 85° C. and aged for 3 hours to obtain an ammonium maleate solution. Add 200g of methyl silicone oil with a viscosity of 100CS into the reaction kettle, increase the temperature of the methyl silicone oil in the reaction kettle to 180-190°C, and then slowly add the maleamide salt solution into the methyl silicone oil dropwise. edge access N 2 After the dropwise addition was completed, the reaction was incubated for 2 hours, and then the temperature was lowered to room temperature to obtain a heat transfer oil solution containing polysuccinimide.

[0088] (2) Preparation of polyaspartic acid

[0089] Add the prepared liquid caustic so...

Embodiment 2

[0091](1) Preparation of polysuccinimide

[0092] Add 196g of maleic anhydride to a 2000mL four-necked bottle, then add 200g of deionized water, stir and heat up to 60°C for hydrolysis. Then, 85 g of 28% (mass fraction) ammonia water was slowly added dropwise to the hydrolyzed solution. After the dropwise addition, the solution was warmed up to 85° C. and aged for 3 hours to obtain an ammonium maleate solution. Add 200g of simethicone oil with a viscosity of 100CS into the reactor, increase the temperature of the simethicone in the reactor to 180-190°C, then slowly add the maleamide salt solution into the simethicone, Inject N while dropping 2 After the dropwise addition was completed, the reaction was incubated for 2 hours, and then the temperature was lowered to room temperature to obtain a heat transfer oil solution containing polysuccinimide.

[0093] (2) Preparation of polyaspartic acid

[0094] Add the prepared liquid caustic soda to the heat-conducting oil solution c...

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Abstract

The application provides a preparation method of polysuccinimide and polyaspartic acid. The method comprises the following steps: providing ammonium maleate or aspartic acid; using heat conduction oilas a reaction medium, so that ammonium maleate or aspartic acid is subjected to thermal shrinkage polymerization to generate polysuccinimide. According to the method, the safe and environment-friendly heat conduction oil is used for replacing an organic solvent which is difficult to recover, harmful and not environment-friendly, so that the reaction is easier to carry out in the direction of generating polysuccinimide, the raw material conversion rate is higher, the reaction is more thorough, and the product performance is good.

Description

technical field [0001] The application relates to the technical field of chemical synthesis, in particular to the preparation method of polysuccinimide and polyaspartic acid. Background technique [0002] Polysuccinimide is a highly reactive linear polyimide, which can be easily ring-opened by amino groups to generate polyasparagine with side chains. Using the special ring-opening properties of polysuccinimide, many derivatives containing special side chains have been prepared and used as drug carriers and sustained-release agents. The preparation of polysuccinimide with good linearity and high relative molecular weight and its application in the development of pharmaceutical excipients has always attracted much attention. Polyaspartic acid is the product of polysuccinimide ring-opening hydrolysis. [0003] Among them, polysuccinimide can be formed by thermal condensation polymerization of aspartic acid, maleic anhydride and derivatives thereof. Aspartic acid, maleic anhy...

Claims

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Application Information

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IPC IPC(8): C08G73/10
CPCC08G73/1092
Inventor 欧敏梅龙毅
Owner 南京艾普拉斯生物科技有限公司
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