Equipment and method for cracking polyalkyl alpha-cyanacrylate

A technology of cyanoacrylate and polyalkylene, which is applied in the field of equipment used in this cracking method, can solve the problems of high cost of thin film evaporators and the inability to enlarge the output, etc., and achieve reduction in production rate, short heating time, and large evaporation surface Effect

Inactive Publication Date: 2009-08-05
IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a cracking equipment and method for polyalkyl α-cyanoacrylate, which basically solves the problem of easy repolymerization of cracked monomer products and high-temperature polymers, and basically overcomes the existing methods When diluting the viscosity of the polymer by adding a solvent, it is impossible to avoid the defect that the monomer is heated and polymerized when the monomer escapes, and the production cannot be enlarged, and it basically overcomes the defect of the existing high-cost thin-film evaporator.

Method used

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  • Equipment and method for cracking polyalkyl alpha-cyanacrylate
  • Equipment and method for cracking polyalkyl alpha-cyanacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 (preparation of polymer)

[0042] Take 522g of paraformaldehyde (92%, 16mol) and 1500g of water into a 3L flask, and heat to 90°C to dissolve it. Take 2008g of ethyl α-cyanoacetate, 1 liter of toluene and 15g of piperidine, stir vigorously in a 5L flask equipped with a water separator, and slowly add the above-mentioned formaldehyde solution. This is an exothermic reaction. Pay attention to controlling the feed rate and temperature control so that the reaction temperature does not exceed 80°C. After the addition was complete, it was stirred at 80° C. for 1.5 hours, and then 10 g of phosphoric acid was added. Then raise the temperature to carry out azeotropic dehydration. The azeotropic dehydration starts at 88°C. After most of the water is released, the temperature in the reaction bottle begins to rise, gradually remove the distilled toluene, and raise the temperature to 135°C. Continue at this temperature. Azeotrope until no more water drops drip from th...

Embodiment 2

[0043] Embodiment 2 (cleavage reaction)

[0044] Inject enough TCP (about 1 liter) for liquid circulation into the middle tank of the cracking equipment, heat the heat exchanger and circulate the TCP, and preheat the cracking equipment to 170°C. Then put all the TCP into the feed tank, dilute the mixture in the feed tank, then turn on the vacuum pump to lower the pressure to 4 torr, make the raw material mixture suck into the middle tank, circulate cracking and separate the product alkyl group with the supergravity machine of the present invention α-cyanoacrylates and incompletely cracked polyalkyl α-cyanoacrylates. Control the hot oil temperature of the heat exchanger to 220°C, the outlet temperature is about 207°C, and the gas inhibitor SO 2 The flow rate is about 1cc / min, and at the same time, the valve controls the continuous feeding of the raw material mixture to keep the liquid level of the middle tank approximately constant, and the principle is to maintain the liquid ...

Embodiment 3～9

[0045] Embodiment 3~9 (the influence of cracking reaction parameter)

[0046] In Table 1, the present invention has adjusted parameters such as the ratio of polyoxymethylene and ethyl α-cyanoacetate, the temperature of the heat exchanger, the temperature, pressure, and time of the cracking reaction for the polymerization reaction, and measures the yield . It can be clearly found from Table 1 that the yield of ethyl α-cyanoacrylate produced by the equipment and method of the present invention can reach more than 95%.

[0047] Table 1

[0048] Reality

[0049] 8 1.1 / 1 225 216～217 6 3.5 92.2 9 1.1 / 1 220～230 207～219 4 4 95.6

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Abstract

The invention reduces the disturbance that the alkyl alfa-cyanoacrylate product is difficultly separated from an auto polymer in the cracking process of the poly alkyl alfa-cyanoacrylate by an ultragravity separator, thereby avoiding the re-polymerization of the monomer product and the reaction products due to heating and making the coarse yield of the cracking reach more than 95 percent. Because of the porous structure rotating at a high speed, the liquid drop forwarding by centrifugation is further cut into thinner wet droplet, thereby unnecessarily increasing the volume of the equipment for increasing the surface area.

Description

technical field [0001] The present invention relates to a cracking method for poly(alkyl alpha-cyano acrylate), and more particularly relates to the equipment used in the cracking method. Background technique [0002] Alkyl α-cyanoacetate and formaldehyde can be polymerized under a basic catalyst to form polyalkyl α-cyanoacrylate, and after high-temperature cracking, a highly reactive instant glue monomer—alkyl α- Cyanoacrylate. In the air, only a small amount of water vapor can make the above-mentioned instant glue monomer polymerized. At high temperature, the monomer is also easy to polymerize and deteriorate, so the preparation of instant glue should pay attention to anhydrous and avoid high temperature. Generally speaking, after the polyalkyl α-cyanoacrylate is formed, the solvent can be used for azeotropic dehydration, and then the solvent can be removed to obtain anhydrous polymer, and then the anhydrous polymer can be cracked at high temperature reaction. The chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/19C07C255/23C07C253/30
Inventor 王天路吕芳仁简龙舜
Owner IND TECH RES INST
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