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Method for improving storage stability of alpha-cyanacrylate adhesive

A technology for cyanoacrylate and storage stability is applied in the field of improving the storage stability of alpha-cyanoacrylate adhesives, which can solve the problems such as the decrease of the curing speed of alpha-cyanoacrylate, achieve simple operation, wide application prospects, Significant economic benefits

Inactive Publication Date: 2008-01-02
北京科化新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when 150-200ppm of sulfur dioxide is added, the curing speed of α-cyanoacrylate will drop by more than two times

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation of embodiment 1.α-ethyl cyanoacrylate

[0018] Mix ethyl cyanoacetate and formaldehyde aqueous solution as starting materials in a reaction kettle, and in the presence of hexahydropyridine, use dichloroethane that can azeotrope with water as a dehydrating agent, and the addition amount is 60ml / mol formaldehyde , carry out the condensation reaction at a temperature of 80±5°C and normal pressure; add acetyl chloride after the dehydration is complete, reflux stably for 2 hours under full stirring, recover the dehydrating agent dichloroethane and the alcohol-removing agent acetyl chloride, add five Phosphorus oxide, hydroquinone inhibitor, cracking and distillation under the condition of 0.5-25mmHg vacuum and 160-190℃, and rectification to obtain α- Ethyl cyanoacrylate refined monomer, productive rate is 65%, wherein the molar ratio of ethyl cyanoacetate and formaldehyde is 1.05: 1.00, the input amount of hexahydropyridine is 3ml / mol formaldehyde, the add-on...

Embodiment 2

[0022] The preparation of embodiment 2.α-methoxy ethyl cyanoacrylate

[0023] Mix methoxyethyl cyanoacetate and paraformaldehyde as starting materials in a reactor, in the presence of hexahydropyridine, at a temperature of 60±5°C, with a vacuum of 30mmHg at the beginning and 2mmHg at the end Condensation reaction is carried out under the condition of dehydration, after the dehydration is complete, add trimethylchlorosilane, reflux stably for 2 hours under full stirring, recover the alcohol removal agent trimethylchlorosilane, add phosphorus pentoxide, hydroquinone polymerization inhibitor, Carry out pyrolysis distillation again under the condition of 0.5 ~ 25mmHg vacuum and 160 ~ 200 ℃, and then through rectification, the α-methoxyethyl cyanoacrylate monomer with a purity of less than 50ppm and a purity of more than 99.2% can be obtained. Productive rate is at 60%, wherein the feeding molar ratio of methoxyethyl cyanoacetate and paraformaldehyde is generally 1.07: 1.00, and th...

Embodiment 3

[0027] The preparation of embodiment 3.α-methyl cyanoacrylate

[0028] Mix methyl cyanoacetate and paraformaldehyde (with a particle size of 40-120 mesh) in a reaction kettle, and carry out condensation reaction with toluene as a dehydrating agent under normal pressure at a temperature of 100°C in the presence of a sodium hydroxide catalyst , its addition is 60ml / mol paraformaldehyde; After dehydration is complete, add acetic anhydride, reflux stably for 1 hour under sufficient stirring, reclaim dehydrating agent toluene and alcohol removal agent acetic anhydride, add phosphorus pentoxide, pyrocatechol and After p-tert-butylphenol polymerization inhibitor, cracking distillation is carried out under the condition of vacuum degree of 0.5-25mmHg and temperature of 160-190°C, and rectification, the yield of 65% with alcohol content less than 50ppm can be obtained and purity of 99.2% α-methyl cyanoacrylate monomer; wherein, the molar ratio of methyl cyanoacetate and paraformaldehyd...

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PUM

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Abstract

The invention discloses an improving method of storage stability of alpha-cyano acrylate adhesive in the alpha-cyano acrylate adhesive domain, which comprises the following steps: adopting cyanoacetate and formagene or formaldehyde solution as raw material; using low-boiling point organic solvent to coboil with water as dehydrant under alkaline catalyst; doing condensing reaction at 80-100 deg. c under normal pressure or 60+-5deg. c without vacuum degree at 0.5-50mmHg without dehydrant; adding alcohol removing agent after dehydrating completely to stir sufficiently; refluxing stably for 0.5-2h; recycling (dehydrant)alcohol removing agent to add inhibitor to do cracking distilling with vacuum degree at 0.5-25mmHg under 160-220 deg. c; rectifying; obtaining the product; obtaining the product with alcohol content less than 50ppm to keep biological property over normal temperature.

Description

technical field [0001] The invention belongs to the field of alpha-cyanoacrylate adhesives, in particular to a method for improving the storage stability of alpha-cyanoacrylate adhesives. Background technique [0002] The poor storage stability of the instant adhesive with α-cyanoacrylate monomer as the main component is its main shortcoming. The main reason for its poor stability is that the monomer contains a small amount of alcohol and a small amount of water and monomer. Effect, easy to occur anionic polymerization and curing. In order to improve its stability, a lot of research has been carried out at home and abroad in the past 30 years. At present, the existing methods are to add polymerization inhibitors or use physical methods to encapsulate the adhesive monomer with paraffin oil or inert gas, but these methods have defects. For example, adding a polymerization inhibitor to the product will affect the curing time and bonding strength of the adhesive, and these meth...

Claims

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Application Information

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IPC IPC(8): C09J133/14C07C255/18C07C253/32
Inventor 袁有学任惠敏李琦冉建新
Owner 北京科化新材料科技有限公司
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