Method for producing alpha-cyanoacrylate adhesive by continuous feeding

An adhesive and ethyl cyanoacetate technology, which is applied in the field of continuous feed production of α-cyanoacrylate adhesives, can solve the problem of reducing product yield and production efficiency, reducing the initial concentration of reactants, and slowing down the polycondensation reaction. speed and other issues, to achieve the effect of reducing the temperature range of depolymerization, reducing energy consumption, and reducing production energy consumption

Active Publication Date: 2021-02-19
山东禹王和天下新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] According to the above description, the traditional preparation process of ethyl α-cyanoacrylate adopts the feeding method of adding dropwise formaldehyde aqueous solution or ethyl cyanoacetate, and the molar ratio of ethyl cyanoacetate and formaldehyde will constantly change during the polycondensation process, resulting in The molecular weight distribution range of the generated α-ethyl cyanoacrylate prepolymer is very wide, resulting in a wide range of depolymerization temperature, and the later depolymerization temperature exceeds 200 ° C, which is very unfavorable to product quality
At the same time, the traditional process adds the organic solvent at one time, which will play a dilution role, reduce the initial concentration of the reactants, and slow down the speed of the polycondensation reaction
This will not only increase the energy consumption in the depolymerization process, but also reduce the yield and production efficiency of the product

Method used

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  • Method for producing alpha-cyanoacrylate adhesive by continuous feeding

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A device for producing α-cyanoacrylate adhesive with continuous feed, the structure is as follows figure 1 Shown, comprise first mixer 7, second mixer 8, preheater 9, pre-reactor 10 and polycondensation reactor 12, first mixer 7 is connected with ethyl cyanoacetate feeding pump 1 and organic solvent feed Feed pump 2, the second mixer 8 is connected with the second feed pump 3, the second feed pump 3 is used to input formaldehyde, basic catalyst, the first mixer 7 is connected with the preheater 9, and the preheater 9 is connected with the The second feed pump 3 is commonly connected with the second mixer 8, and the second mixer 8, the pre-reactor 10 and the polycondensation reactor 12 are connected in sequence. An intermediate feed pump 11 is arranged between the pre-reactor 10 and the polycondensation reactor 12 . A rotameter is arranged between the first mixer 7 and the ethyl cyanoacetate feed pump 1 and the organic solvent feed pump 2 , and a rotameter 6 is arranged...

Embodiment 2

[0038] Utilize the device of embodiment 1 to carry out the method for continuous feed production α-cyanoacrylate adhesive, comprise steps as follows:

[0039] Ethyl cyanoacetate and 1,2-dichloroethane enter the first mixer 7 from the feed pump at a flow rate of 1530kg / h and 1200kg / h to mix evenly, then preheat through the heat exchanger 9, and then mix with the following The flow rate of 1050kg / h enters the formaldehyde and hexahydropyridine through the second feed pump 3 into the second mixer 8, enters the pre-reactor 10 for preliminary polycondensation reaction, and finally enters the polycondensation reactor 12 through the intermediate feed pump 11 Carry out sufficient polycondensation reaction to form α-cyanoacrylate ethyl ester prepolymer; then use 1,2-dichloroethane azeotropic dehydration; then add 10kg inhibitor and 450kg plasticizer, under 3mmHg vacuum condition High-temperature depolymerization, complete cracking at 160-180°C and collect the crude product; finally, th...

Embodiment 3

[0042] Utilize the device of embodiment 1 to carry out the method for continuous feed production α-cyanoacrylate adhesive, comprise steps as follows:

[0043] Ethyl cyanoacetate and 1,2-dichloroethane are respectively fed into the first mixer 7 by the feed pump at a flow rate of 1360kg / h and 1060kg / h, and then preheated by the heat exchanger 9, and then mixed with 930kg The formaldehyde and hexahydropyridine entered by the flow rate of / h through the second feed pump 3 are mixed uniformly in the second mixer 8, enter the pre-reactor 10 for preliminary polycondensation reaction, and finally enter the polycondensation reactor 12 through the intermediate feed pump 11 Carry out sufficient polycondensation reaction in , form α-ethyl cyanoacrylate prepolymer, carry out dehydration, depolymerization, refining by the same condition of embodiment 2, obtain the monomer that purity is 99.9%, and calculated mass yield is 82% . Under these conditions, the molecular weight of the obtained ...

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Abstract

The invention relates to a method for producing an alpha-cyanoacrylate adhesive by continuous feeding, which comprises the following steps: pumping ethyl cyanoacetate and an organic solvent into a first mixer by a feeding pump respectively, conducting uniform mixing, and preheating the mixed material 1 by a heat exchanger to obtain a preheated material 1; and converging and mixing the preheated material 1 with formaldehyde and a basic catalyst entering through a feeding pump in a second mixer to obtain a mixed material 2, performing primary polycondensation reaction on the mixed material 2, and then performing polycondensation reaction to obtain an ethyl alpha-cyanoacrylate prepolymer with centralized molecular weight distribution. The method provided by the invention maintains a constantmolar ratio of ethyl cyanoacetate to formaldehyde in the reaction process. According to the invention, continuous feeding of raw materials in the synthesis stage of the ethyl alpha-cyanoacrylate prepolymer is realized, the homogeneity of the polymerization degree of the ethyl alpha-cyanoacrylate prepolymer is improved, the depolymerization temperature range of the ethyl alpha-cyanoacrylate prepolymer is reduced, the energy consumption in the production process is reduced, and the yield and the production efficiency of the product are improved.

Description

technical field [0001] The invention belongs to the field of preparing α-cyanoacrylate ethyl adhesive, and more specifically relates to a method for continuously feeding the α-cyanoacrylate adhesive. Background technique [0002] α-Ethyl cyanoacrylate, also known as 502 glue, is one of the most common types of adhesives on the market. Due to its single component, low viscosity, fast curing speed, high bonding strength, good transparency, Basic non-toxic, easy to use and other advantages, has been widely used in the bonding of metal, plastic, wood, rubber, leather, ceramics, glass and many other materials. [0003] The traditional production process of α-ethyl cyanoacrylate adhesive is: first add ethyl cyanoacetate and organic solvent to the reaction kettle, and then gradually add formaldehyde aqueous solution containing alkaline catalyst, or, first add Aqueous formaldehyde solution, organic solvent, basic catalyst, and then gradually add ethyl cyanoacetate dropwise to fully...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J4/04B01J19/18B01J4/00B01F13/10
CPCC09J4/00B01J4/001B01J19/1862B01J2204/002B01F33/80B01F33/8362
Inventor 朱传华李国旗齐维彬王鹏刘杨
Owner 山东禹王和天下新材料有限公司
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