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Preparation of alpha-cyanacrylate adhesive

A cyanoacrylate and adhesive technology, which is applied in the preparation of organic compounds, carboxylic acid nitriles, non-polymer organic compound adhesives, etc., can solve the problem of α-cyanoacrylate adhesive whitening Problems with irritation, affecting the aesthetics of the surface of the article, prone to frosting and whitening, etc., to achieve the effect of simple preparation method, improved product performance, and reduced irritation

Active Publication Date: 2012-10-03
中山有行企业胶类制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still does not solve the problem of whitening and irritation of α-cyanoacrylate adhesives
[0004] As we all know, when α-cyanoacrylate adhesives are bonded, because a small part of the acrylate monomer contained in them will volatilize during the curing process, and will polymerize into small particles near the adhesive film and condense on the surface, it is easy to appear frost bleaching phenomenon
This not only affects the aesthetics of the surface of the article, but also leads to a decrease in the bonding strength, which limits the application of α-cyanoacrylate adhesives to a certain extent

Method used

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  • Preparation of alpha-cyanacrylate adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 60 parts by weight of paraformaldehyde, 200 parts by weight of toluene, and 0.2 parts by weight of piperidine into a four-necked flask equipped with a stirring dish, a thermometer, and a dropping funnel, and add 314 parts by weight of α-ethoxylate dropwise while stirring at 80°C. Ethyl cyanoacetate was refluxed to react to obtain a condensate. After cooling the reaction liquid to room temperature, add 300 parts by weight of 1% p-toluenesulfonic acid aqueous solution, vibrate, and separate into two layers after standing still, separate the oil layer, and distill the toluene in the oil layer under reduced pressure, and put it in the reaction flask Add hydroquinone and P to the condensate 2 o 5 3 parts by weight each, decompressed to a pressure of 3-5 mmHg, and depolymerized by heating at 160° C. to obtain 272 parts by weight of crude monomer with a product purity of 96.8%. Subsequently, P was added to the crude monomer 2 o 5 and 0.5% of hydroquinone, and then dist...

Embodiment 2

[0024] Using the device under the same conditions as in Implementation 1, add 60 parts by weight of paraformaldehyde, 300 parts by weight of benzene, and 1.6 parts by weight of piperidine, and drop 416 parts by weight of α-methoxyethyl cyanoacetate at 85°C , Reflux to make it react to obtain a condensation liquid. After the condensed liquid was washed twice with 200 parts by weight of water, benzene in the layer was distilled off under reduced pressure. Then, adding P to the condensate 2 o 5 and 5 parts by weight of hydroquinone, depolymerized by heating under reduced pressure at 200° C. to obtain 385 parts by weight of crude monomer with a product purity of 95.5%. Add P to the crude monomer 2 o 5 and 0.5% of hydroquinone, and then distilled to obtain 332 parts by weight of α-methoxy cyanoacrylate with a purity of 98.6%. Add SO to this compound 2 40ppm and 120ppm hydroquinone to prepare the adhesive.

Embodiment 3

[0026] Using the device with the same conditions as in Implementation 1, add 86 parts by weight of 37% formaldehyde solution, 300 parts by weight xylene, 0.1 part by weight p-toluene sulfonic acid, drop 240 parts by weight α-propoxyl at 85°C Ethyl cyanoacetate was refluxed to react to obtain a condensate. After the condensate was washed with 200 parts by weight of a 0.5% sulfuric acid aqueous solution, xylene in the oil layer was removed under reduced pressure to obtain a condensate. Then add P to the condensate 2 o 5 and 3 parts by weight of hydroquinone, depolymerized under reduced pressure and heated at 190°C to obtain 228 parts by weight of crude monomer with a product purity of 92.8%. Add P to the crude monomer 2 o 5 And each 1.0% of hydroquinone, then carry out distillation, then obtain the propoxy ethyl cyanoacrylate 203 weight parts that purity is 98.2%, add SO 2 30ppm, hydroquinone 92ppm, made adhesive.

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Abstract

The invention provides a method for preparing Alpha-cyanoacrylate adhesive which has low whitening degree, low stimulation and high toughness. The Alpha-cyanoacrylate adhesive is prepared by using paraformaldehyde or formalin and alkyl cyanoacetate as main materials, enabling the paraformaldehyde or formalin and the alkyl cyanoacetate to carry out condensation reaction at the temperature of 80-90DEG C under the action of dehydrant and alkaline catalyst and then mainly carrying out the reduced pressure distillation, heating depolymerization and other processes. Compared with similar products,the Alpha-cyanoacrylate adhesive has greatly reduced whitening degree and stimulation, thereby improving the attractiveness of an adhesive product and being good for improving the adhesive strength of the adhesive product. In addition, the method for producing the Alpha-cyanoacrylate adhesive is simple and feasible, thereby the performance of the adhesive product is remarkably improved and the manufacturing cost of the adhesive product is lowered.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and more specifically relates to a preparation method of an α-cyanoacrylate adhesive with low whitening, low irritation and high toughness. Background technique [0002] Whether in daily life or industrial production, α-cyanoacrylate adhesive (instant adhesive, also known as 502 glue) has many applications. The adhesive was first successfully developed by the American Eastman Kodark company in 1958 and introduced to the market. It has a series of unique advantages, such as no solvent, no need for heat and pressure, wide bonding range, high strength, instant curing, It is basically non-toxic and has a strong adhesive effect on biological tissues such as skin. Today, with the continuous advancement of synthesis technology, the comprehensive performance of α-cyanoacrylate adhesives is also constantly improving, and is widely used in industry, agriculture, civil and other fields. At the same t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J4/04C07C255/23C07C253/30
Inventor 方薛行
Owner 中山有行企业胶类制品有限公司
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