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Method for preparing isocyanate monomer

A technology of isocyanate and monomer, which is applied in the field of diisocyanate preparation based on salt-forming phosgenation reaction, can solve the problems of incomplete salt-forming reaction hydrochloride particles, low utilization rate of HCl, many side reactions, etc., and achieve stable product quality , full salt-forming reaction, easy to start and stop

Active Publication Date: 2015-09-30
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing isocyanate monomers, which can overcome the incomplete salt-forming reaction in the existing salt-forming process, the hydrochloride salt particles are large, and a large amount of amines that do not participate in the salt-forming process are wrapped, and the internal materials are difficult to participate in the process. One-step photochemical reaction, resulting in the generation of urea impurities during the photochemical process, resulting in many side reactions; it can handle higher concentrations of hydrochloride, make it undergo phosgenation reaction to obtain qualified isocyanate, and solve the problem of low utilization of HCl , the problem of high energy consumption

Method used

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  • Method for preparing isocyanate monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079]The inner diameter of the thick part of the mixer is 5cm. There are 3 sets of left-handed helical plates and right-handed helical plates. The helical plates are twisted 270°, and the length of each helical plate is 5cm. The inner diameter of the small diameter part is 4cm, the length is 30cm, and there are evenly distributed holes on the pipe wall of the small diameter part. The diameter of the holes is 1.2mm, and the opening rate is 14%. It is 90cm. The inner diameter of the outer tube of the mixer is 10 cm, the distance h between the top of the outer tube and the top of the inner tube is 15 cm, and the length of the outer tube is 90 cm. Both inner and outer tubes have a wall thickness of 1mm.

[0080] The volume of the salt-forming reaction kettle is 1000L, and nitrogen gas is first introduced to remove the air and moisture in the reaction kettle. Preload 300kg o-dichlorobenzene as the reaction solvent, and start the reactor stirrer 12 and the reaction circulation pu...

Embodiment 2

[0085] The inner diameter of the thick part of the mixer is 6cm, and there are 5 groups of spiral plates, the spiral plates are twisted 270°, and the length of each spiral plate is 5cm. The inner diameter of the small diameter part is 4cm, and the length is 30cm. There are evenly distributed holes on the pipe wall of the small diameter part. The diameter of the holes is 1mm, and the opening rate is 20%. The total length is 90cm. The inner diameter of the outer tube is 13m, the distance h between the top of the outer tube and the top of the inner tube is 20cm, and the length of the outer tube is 100cm. Both inner and outer tubes have a wall thickness of 1mm.

[0086] The volume of the salt-forming reactor is 1000L, and the air and moisture in it are removed by passing nitrogen gas. Preload 300kg o-dichlorobenzene as the reaction solvent, and start the reactor stirrer 12 and the reaction circulation pump 14. Turn on the HCl compressor 5, control the outlet absolute pressure t...

Embodiment 3

[0091] The inner diameter of the thick part of the mixer is 8cm. There are 5 groups of left-handed helical plates and right-handed helical plates. The helical plates are twisted 270°, and the length of each helical plate is 5cm. The inner diameter of the small diameter part of the inner tube is 5cm, and the length is 30cm. There are evenly distributed holes on the wall of the small diameter part. The diameter of the holes is 0.8mm, and the opening rate is 18%. The total length of the inner tube is 100cm. The inner diameter of the outer tube is 14cm, the distance h between the top of the outer tube and the top of the inner tube is 30cm, and the length of the outer tube is 110cm. Both inner and outer tubes have a wall thickness of 1mm.

[0092] The volume of the salt-forming reactor is 1000L, and the air and moisture in it are removed by passing nitrogen gas. Preload 300kg o-dichlorobenzene as the reaction solvent, and start the reactor stirrer 12 and the reaction circulation ...

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Abstract

The invention discloses a method for preparing an isocyanate monomer. The method comprises the following steps: adding a first batch of solvents in a reaction kettle and circulating; compressing HCl, conveying HCl in a salt-forming reaction kettle through the outer tube of a mixer, carrying out gas-liquid separation and then circulating HCl in a system through a Venturi mixer; mixing diamine with the residual solvents in the inner tube of the mixer, then mixing the mixture with HCl in the outer tube, and then conveying the mixture in the salt-forming reaction kettle and reacting to obtain a diamine hydrochloride solution; reacting the diamine hydrochloride solution with phosgene under a pressurization condition to obtain an isocyanate photochemical solution. The mixer comprises the inner tube and the outer tube, wherein a spiral plate is installed in the thick-diameter part of the inner tube, a hole is formed in the tube wall of the thin-diameter part of the inner tube, and the bottom of the inner tube is a detachable bottom plate; the outer tube sleeves outside the inner tube, and the bottom of the outer tube is a mixer outlet. The method disclosed by the invention reinforces the mixing effect of the gas-liquid reaction, the obtained hydrochloride particles are uniform, the use efficiency of HCl is high, the energy consumption is low, and the purity of the photochemical solution after a phosgenation reaction is high.

Description

technical field [0001] The present invention relates to a kind of method for preparing isocyanate monomer, more specifically, relate to a kind of method for preparing diisocyanate based on salt-forming phosgenation reaction. Background technique [0002] In the prior art, the phosgene method of preparing isocyanates by reacting organic primary amines and phosgene in an inert solvent is well known. The phosgene method can be divided into a direct method and a salt-forming method. The direct method is to prepare the corresponding isocyanate by directly reacting primary amine and phosgene; the salt-forming method first reacts the corresponding amine with an acid gas such as hydrogen chloride, carbon dioxide, etc. to prepare an amine salt, and then react the amine salt with phosgene. Due to the fast reaction rate of aliphatic amines and phosgene, it is easy to cause amine coating and produce urea by-products in the subsequent thermophotochemical process. The generation of amin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C265/14B01F13/10
Inventor 李建峰尚永华史培猛孙中平韩金平华卫琦黎源王占友
Owner WANHUA CHEM GRP CO LTD
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