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Method for preparing adipic acid dihydrazide

A technology of adipic acid dihydrazide and adipic acid, which is applied in the field of preparation of adipic acid dihydrazide, can solve the problems of large environmental hazards, strong corrosion, side reactions, etc., to reduce production costs and improve conversion The effect of reduction in rate and reuse

Inactive Publication Date: 2016-05-04
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first step of the esterification reaction, concentrated sulfuric acid is mostly used as a catalyst, which has problems such as strong corrosion, great environmental hazards, and side reactions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Take 50g of adipic acid and add it to 55g of methanol, then add 5g of D001 type macroporous strong acidic cation exchange resin, heat the reaction system to reflux state, and perform esterification reaction under reflux state and stirring for 5 hours, the esterification reaction time After the end, cool the system to 5-40°C, and under stirring, first add 30g of ammonia water with a concentration of 25% dropwise to the system, and then add 40g of hydrazine hydrate with a concentration of 80% dropwise. The hydrazino reaction is carried out under the temperature condition of ℃ for 3 hours, and after the hydrazino reaction is completed, the catalyst is filtered out to obtain the product after the reaction; the catalyst can be reused after being treated.

[0021] (2) After distilling the methanol out of the reaction product by distillation, the crude product of adipic acid dihydrazide is obtained; the crude product of adipic acid dihydrazide is washed with ice water for 3...

Embodiment 2

[0023] (1) Add 50g of adipic acid to 45g of methanol, then add 8g of D061 type macroporous strong acidic cation exchange resin, heat the reaction system to reflux state, and carry out esterification reaction under reflux state and stirring for 5 hours, the esterification reaction time After the end, cool the system to 5-40°C, under stirring, first add 40g of ammonia water with a concentration of 25% dropwise to the system, and then add 40g of hydrazine hydrate with a concentration of 80%, after the dropwise addition, stir and 5-40 The hydrazino reaction is carried out under the temperature condition of ℃ for 3 hours, and after the hydrazino reaction is completed, the catalyst is filtered out to obtain the product after the reaction; the catalyst can be reused after being treated.

[0024] (2) After distilling the methanol out of the reaction product by distillation, the crude product of adipic acid dihydrazide is obtained; the crude product of adipic acid dihydrazide is washed ...

Embodiment 3

[0026] (1) Add 50g of adipic acid to 60g of methanol, then add 8g of D061 type macroporous strong acidic cation exchange resin, heat the reaction system to reflux state, and perform esterification reaction under reflux state and stirring for 4 hours, the esterification reaction time After the end, cool the system to 5-40°C, and under stirring, first add 30g of ammonia water with a concentration of 25% dropwise to the system, and then add 40g of hydrazine hydrate with a concentration of 80% dropwise. The hydrazino reaction is carried out under the temperature condition of ℃ for 2 hours. After the hydrazino reaction is completed, the catalyst is filtered out to obtain the product after the reaction; the catalyst can be reused after being treated.

[0027] (2) After distilling the methanol out of the reaction product by distillation, the crude product of adipic acid dihydrazide is obtained; the crude product of adipic acid dihydrazide is washed with ice water for 3 times, and then...

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Abstract

The invention discloses a method for preparing adipic acid dihydrazide. The method comprises the following steps of (1) adding adipic acid and strong-acidic cation exchange resin taken as a catalyst into methanol, then heating a reaction system till a reflux state is formed, and performing an esterification reaction under the reflux state; after the completion of the esterification reaction, adding ammonia water into the reaction system at a temperature of 5 to 40 DEG C, then adding hydrazine hydrate, and enabling the reaction system to perform a hydrazination reaction at a temperature of 5 to 40 DEG C; after the completion of the hydrazination reaction, filtering out the catalyst, and preparing a reaction product; (2) obtaining an adipic acid dihydrazide crude product by means of removing methanol from a product obtained through a distillation reaction; obtaining the adipic acid dihydrazide through washing and drying the adipic acid dihydrazide crude product. The method disclosed by the invention has the advantages that the conversion rate can be improved, the side reaction is less, the catalyst can be recycled, and the production cost is low.

Description

technical field [0001] The invention relates to a preparation method of adipic acid dihydrazide. Background technique [0002] Adipate dihydrazide (ADH), white crystalline powder, bifunctional compound, is an important cross-linking agent, which can be cross-linked with diacetone acrylamide in aqueous emulsion and water-soluble polymer post-crosslinking effect. At present, the existing technology is to synthesize adipate dihydrazide in two steps. First, adipic acid and methanol are used as raw materials to synthesize the crude product of dimethyl adipate, and then the fine product of dimethyl adipate is obtained through separation and purification, and then Reaction with hydrazine hydrate to prepare adipate dihydrazide. [0003] Adipate dihydrazide and diacetone acrylamide are used as monomers for ketohydrazine crosslinking, and the research on the synthesis of ADH is much less than the synthesis and application of diacetone acrylamide. The literature reports the method o...

Claims

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Application Information

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IPC IPC(8): C07C241/04C07C243/28
CPCY02P20/584C07C241/04C07C243/28
Inventor 崔佳惠陈晓辉刘亭邢晓华朱丹
Owner SHANDONG TIANYI CHEM
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