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Synthesis method of alpha-cyanoacrylate

A technology of cyanoacrylate and synthesis method, which is applied in the direction of chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve the problems of restricting application fields and yellowing by adding modifiers, and achieve improved chroma , improve stability, and expand the scope of application

Active Publication Date: 2019-04-26
HEBEI CHENGXIN
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  • Description
  • Claims
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Problems solved by technology

[0003] In view of the yellowing phenomenon in most of the existing α-cyanoacrylate products, it is necessary to add a modifier to change the chromaticity, but the addition of the modifier limits its application field. The present invention provides a changeable Synthesis of alpha-cyanoacrylates of alpha-cyanoacrylate chroma

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  • Synthesis method of alpha-cyanoacrylate
  • Synthesis method of alpha-cyanoacrylate

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[0022] The embodiment of the present invention provides a synthesis method of α-cyanoacrylate, comprising the following process steps:

[0023] A synthetic method for α-cyanoacrylate, comprising the following processing steps:

[0024] a, cyanoacetate and formaldehyde are added in the organic solvent and mixed to obtain a mixed solution, wherein the molar ratio of cyanoacetate and formaldehyde is (1-1.1): 1; an alkaline catalyst (sodium hydroxide , potassium hydroxide, pyridine, hexahydropyridine, ethanolamine and triethylamine), the molar amount of basic catalyst added is 0.1%~0.4% of the molar weight of cyanoacetate; At a temperature of 72-85°C, react for 2 to 5 hours to condense cyanoacetate and formaldehyde to obtain α-cyanoacrylate oligomers. The condensation reaction equation is:

[0025]

[0026] b. Add a plasticizer to the obtained α-cyanoacrylate oligomer, the amount of the plasticizer added is 5%-30% of the mass of the cyanoacetate, and the temperature is raised ...

Embodiment 1

[0034] A synthetic method for ethyl α-cyanoacrylate, comprising the following processing steps:

[0035] a. Add 300g of ethyl cyanoacetate and 80g of formaldehyde into dichloroethane and mix to obtain a mixed solution, add 45g of hexahydropyridine as a basic catalyst to the mixed solution, and react for 2h at a temperature of 80°C to make Ethyl cyanoacetate is condensed with formaldehyde to obtain oligomers of α-ethyl cyanoacrylate.

[0036] b. Add 50 g of dioctyl phthalate to the obtained ethyl α-cyanoacrylate oligomer, and raise the temperature to 140° C. to remove the dichloroethane solvent.

[0037] c. Add 8g of phosphorus pentoxide and 4g of hydroquinone to the α-cyanoacrylate ethyl oligomer from which dichloroethane has been removed, crack and distill at -0.098Mpa and 150°C to obtain 280g of α - crude monomer of ethyl cyanoacrylate;

[0038] d. Add 8ppm p-toluenesulfonic acid and 2ppm phosphorous acid to the crude monomer of ethyl cyanoacrylate. After mixing evenly, ad...

Embodiment 2

[0041] A synthetic method for methoxyethyl α-cyanoacrylate, comprising the following processing steps:

[0042] a. Add 300g of methoxyethyl cyanoacetate and 70g of formaldehyde into dichloroethane and mix to obtain a mixed solution, add 42g of hexahydropyridine as a basic catalyst to the mixed solution, and react at a temperature of 75°C 3h, condense methoxyethyl cyanoacetate and formaldehyde to obtain oligomers of α-methoxyethyl cyanoacrylate.

[0043] b. Add 30 g of dioctyl phthalate to the obtained α-methoxyethyl cyanoacrylate oligomer, and raise the temperature to 150° C. to remove the dichloroethane solvent.

[0044] c. Add 10g of phosphorus pentoxide and 5g of hydroquinone to the α-methoxyethyl cyanoacrylate oligomer from which dichloroethane has been removed, and crack and distill at -0.098Mpa and 180°C to obtain 240 g of crude monomer of methoxyethyl α-cyanoacrylate;

[0045] d. Add 12ppm p-toluenesulfonic acid and 2ppm phosphorous acid to the crude monomer of α-meth...

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Abstract

The invention relates to the technical field of adhesive optimization and in particular discloses a synthesis method of alpha-cyanoacrylate. The synthesis method comprises the following steps: a, carrying out a condensation reaction on cyanide acetate and formaldehyde in the presence of an alkali catalyst to obtain a cyanoacrylate oligomer; b, putting a plasticizer into the cyanoacrylate oligomer,and heating to remove an organic solvent; c, adding a polymerization inhibitor, and carrying out splitting distillation to obtain a crude monomer of alpha-cyanoacrylate; d, adding a stabilizer, uniformly mixing, adding activated carbon, standing still and layering, and retaining supernate; e, carrying out vacuum distillation on the supernate to obtain the alpha-cyanoacrylate. By adopting the synthesis method of the alpha-cyanoacrylate, the problem that the alpha-cyanoacrylate can be yellowed is substantially solved, a product obtained through distillation has small chroma and is good in stability, and the probability of yellowing of the product in the storage and use process is reduced.

Description

technical field [0001] The invention relates to the technical field of adhesive optimization, in particular to a method for synthesizing α-cyanoacrylate. Background technique [0002] There are more and more applications of α-cyanoacrylate adhesives (instant adhesives) in industry, medical care, beauty, military, daily life, etc., and different industries have more and more requirements for different instant adhesives. The more stringent, but most of the methods of conventional synthesis of α-cyanoacrylates have the phenomenon of product yellowing, and the use of some fine processing, medical and beauty industries is subject to certain restrictions. At present, most manufacturers pass the α-cyanoacrylate Adding modifiers to cyanoacrylic acid monomers to improve the yellowing phenomenon has achieved certain results, but adding modifiers to the original adhesive is equivalent to introducing new chemical substances, and the introduction of these modifiers is often difficult. H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/23
CPCC07C253/30C07C255/23
Inventor 王虹张朝纯范春艳孙洁浩刘少军高强董津
Owner HEBEI CHENGXIN
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