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Synthesis method of adipic acid dihydrazide

An adipic acid dihydrazide and a synthesis method technology are applied in the field of chemical synthesis, can solve the problems of high cost of a strong acid cation exchange resin catalyst, unsuitable for industrialized large-scale production, complicated operation, etc. Simple and effective for improving catalytic activity

Inactive Publication Date: 2019-05-14
JIANGSU XINLU CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention uses strongly acidic cation exchange resin as a catalyst, which is expensive and complicated to operate, and is not suitable for large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of synthetic method of adipic acid dihydrazide, concrete operation steps are as follows:

[0020] (1) Inject a mixed solution of 100% methanol (0.5mol) and 75% ethanol (0.5mol) into a 500mL beaker, then add adipic acid (3.5mol) into the mixed solution of methanol and ethanol, and then add sulfuric acid A mixture of potassium hydrogen (0.1 mol) and potassium sulfate (0.4 mol) was catalyzed, the reaction system was heated to reflux, and esterification was carried out at 45°C for 0.25h under reflux and stirring.

[0021] (2) After the esterification reaction time is over, cool the system to 25°C, and under stirring, first add hydrazine hydrate (5.25mol) with a mass fraction of 80% to the system dropwise, and then stir and keep it under the condition of 25°C The hydrazination reaction was carried out for 1.5 hours. After the hydrazination reaction was completed, the catalyst was filtered out to obtain the post-reaction product. The catalyst could be reused after bein...

Embodiment 2

[0026] A kind of synthetic method of adipic acid dihydrazide, concrete operation steps are as follows:

[0027] (1) Inject a mixed solution of 100% methanol (0.75mol) and 75% ethanol (0.5mol) into a 500mL beaker, then add adipic acid (4.25mol) into the mixed solution of methanol and ethanol, and then add sulfuric acid A mixture of potassium hydrogen (0.1mol) and potassium sulfate (0.4mol) was catalyzed, the reaction system was heated to reflux, and the esterification reaction was carried out at 40°C for 1.5h under reflux and stirring.

[0028] (2) After the esterification reaction time is over, cool the system to 20°C and, under stirring, first add hydrazine hydrate (4.25mol) with a mass fraction of 80% to the system dropwise, and then stir and keep it under the condition of 20°C Carry out the hydrazination reaction for 1 hour. After the hydrazination reaction, filter out the catalyst to obtain the post-reaction product. The catalyst can be reused after treatment.

[0029] (3...

Embodiment 3

[0033] A kind of synthetic method of adipic acid dihydrazide, concrete operation steps are as follows:

[0034] (1) Inject a mixed solution of 100% methanol (0.5mol) and 80% ethanol (0.25mol) into a 500mL beaker, then add adipic acid (3.5mol) into the mixed solution of methanol and ethanol, and then add sulfuric acid A mixture of potassium hydrogen (0.1mol) and potassium sulfate (0.4mol) was catalyzed, the reaction system was heated to reflux, and the esterification reaction was carried out at 50°C for 2 hours under reflux and stirring.

[0035] (2) After the esterification reaction time is over, cool the system to 30°C, and under stirring, first add hydrazine hydrate (3.375mol) with a mass fraction of 80% to the system dropwise, and then stir and keep it under the temperature condition of 30°C Carry out the hydrazination reaction for 2hh. After the hydrazination reaction, filter out the catalyst to obtain the post-reaction product. The catalyst can be reused after treatment. ...

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PUM

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Abstract

The invention provides a synthesis method of adipic acid dihydrazide. The adipic acid dihydrazide is synthesized according to a two-step method. The synthesis method comprises the following steps: performing an esterification reaction on adipic acid and a mixture of methanol and ethanol under the catalysis of potassium hydrogen sulfate and concentrated sulfuric acid to synthesize dimethyl / diethyladipate, then performing an acylhydrazine reaction on the dimethyl / diethyl adipate and hydrazine hydrate to obtain the adipic acid dihydrazide. The obtained finished adipic acid dihydrazide product has the conversion rate of 98-99%; according to the synthesis method, the esterification reaction yield and the catalytic activity are greatly improved, and catalysts are easier and more convenient to recycle and can be reused for more times; the synthesis method is economical, practical, and convenient for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing adipic acid dihydrazide. Background technique [0002] Adipate dihydrazide (ADH), a white crystalline solid, has a symmetrical molecular structure and is a bifunctional compound. ADH is a good cross-linking agent, which can be cross-linked with carbonyl groups. The typical cross-linking with hyaluronic acid is used in medicine, and the cross-linking with diacetone acrylamide is used in water-based resins. With the increasingly stringent restrictions on volatile organic substances in coatings by environmental regulations, in recent years, domestic and foreign scholars have conducted a lot of research on water-based coatings and related products have developed rapidly, and in many application fields, they have completely or partially replaced traditional coatings. Solvent-based coatings in the sense. It can be expected that with the improvemen...

Claims

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Application Information

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IPC IPC(8): C07C243/28C07C241/04C07C69/44C07C67/08
Inventor 俞小东郑建张建忠方建
Owner JIANGSU XINLU CHEM NEW MATERIAL
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