Method for synthesizing diisocyanate containing ether linkage through direct phosgenation method

A diisocyanate and phosgenation technology, applied in chemical instruments and methods, preparation of isocyanic acid derivatives, preparation of organic compounds, etc., can solve the problems of limited hardness and strength of downstream products, and achieve excellent yellowing resistance, The effect of excellent high temperature resistance

Inactive Publication Date: 2019-10-08
甘肃银光聚银化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at the same time, because the molecular structure of aliphatic diisocyanate does not contain benzene rings, the hardness and strength of downstream products are limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 4kg of amyl acetate to a 20L glass kettle reactor, then pass through gaseous phosgene, after the phosgene is dissolved and saturated, add 1kg of H 2 NCH 2 O(CH 2 ) 2 OCH 2 NH 2 (EDR-120) and 4kg amyl acetate were mixed evenly, and the solution was added into the glass kettle reactor according to the flow rate of 30ml / min using a metering pump. Continue to feed gaseous phosgene into the reactor, control the temperature of the system at 20°C-30°C, continue to react for 1 hour after the dropwise addition is completed, and raise the temperature to 110°C-130°C for thermo-actinization after the luminescence reaction is completed React until the photochemical solution is clear and transparent, and the reaction is over. to OCNCH 2 O(CH 2 ) 2 OCH 2 NCO (EDI-172) photochemical liquid is dephosphorized, desolventized, and refined to obtain qualified OCNCH 2 O(CH 2 ) 2 OCH 2 NCO (EDI-172) product. OCNCH 2 O(CH 2 ) 2 OCH 2 NCO (EDI-172) product yield is 76.8%. ...

Embodiment 2

[0024] Add 5.5kg of o-dichlorobenzene into a 20L glass kettle reactor, then pass into gaseous phosgene, after the phosgene is dissolved and saturated, add 1kg of H 2 NCH 2 O(CH 2 ) 2 OCH 2 NH 2 (EDR-120) and 4.5kg o-dichlorobenzene were mixed evenly, and the solution was added into the glass kettle reactor at a flow rate of 15ml / min using a metering pump. Continue to feed gaseous phosgene into the reactor, control the temperature of the system at 0°C-40°C, continue the reaction for 0.5h after the dropwise addition is completed, and raise the temperature to 120°C-150°C after the luminescence reaction is completed. Chemical reaction, until the actinic liquid is clear and transparent, the reaction is over. to OCNCH 2 O(CH 2 ) 2 OCH 2 NCO (EDI-172) photochemical liquid is dephosphorized, desolventized, and refined to obtain qualified OCNCH 2 O(CH 2 ) 2 OCH 2 NCO (EDI-172) product. OCNCH 2 O(CH 2 ) 2 OCH 2 The product yield of NCO (EDI-172) was 81.2%.

Embodiment 3

[0026] Add 3kg of chlorobenzene into a 20L glass kettle reactor, then pass through gaseous phosgene, after the phosgene is dissolved and saturated, add 1kg of H 2 N (CH 2 ) 3 O(CH 2 ) 2 O(CH 2 ) 3 NH 2 (EDR-176) and 4kg of chlorobenzene were mixed evenly, and the solution was added to the glass kettle reactor at a flow rate of 50ml / min using a metering pump. Continue to feed gaseous phosgene into the reaction kettle, control the temperature of the system at 10°C-20°C, continue the reaction for 1 hour after the dropwise addition is completed, and raise the temperature to 100°C-110°C for thermoactinization after the luminescence reaction is completed React until the photochemical solution is clear and transparent, and the reaction is over. For OCN (CH 2 ) 3 O(CH 2 ) 2 O(CH 2 ) 3 NCO (EDI-228) photochemical liquid dephosphorization, desolventization, product refining to obtain qualified OCN (CH 2 )3 O(CH 2 ) 2 O(CH 2 ) 3 NCO (EDI-228) products. OCN (CH 2 ) ...

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PUM

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Abstract

The invention provides a method for synthesizing diisocyanate containing ether linkage through a direct phosgenation method. The method comprises the specific steps that (1) phosgene is introduced to-10-40 DEG C inert liquid to be dissolved until phosgene saturates; (2) the phosgene is introduced continuously, meanwhile an ether linkage containing diamine solution is dropwise added at -10-40 DEGC, and cold photochemical reaction is conducted to generate carbamic chloride; (3) the temperature is risen to 80-200 DEG C, hydrogen chloride of the carbamic chloride is removed to generate a diisocyanate containing the ether linkage actinic solution; and (4) phosgene removing, solvent removing, and product purification are conducted on the actinic solution to obtain diisocyanate containing the ether linkage. The diisocyanate containing the ether linkage belongs to the field of fat diisocyanate, oxygen is introduced in the main chain except a NCO perssad in the molecular structure; and meanwhile, downstream products further have excellent high temperature resistant performance, and the special requirements of performance of the downstream products are met. The operating process is simpleand easy to control, and the diisocyanate containing the ether linkage is suitable for commercial process.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for synthesizing ether bond-containing diisocyanate by direct phosgenation. Background technique [0002] Isocyanate is a kind of special chemical with NCO functional group. Bulk isocyanate is divided into two series of products: aromatic isocyanate (such as MDI, TDI) and aliphatic isocyanate (such as HDI), which are widely used in polyisocyanate, polyurethane, polyurea , Synthesis of polymer adhesives, insecticides, herbicides, etc. In addition, there are some isocyanates with superior performance but high prices and low dosage, which are mainly used in high-end fields such as high-grade coatings, optoelectronic materials, and medical polyurethane materials. These isocyanates are called special isocyanates. [0003] Because aliphatic diisocyanate does not contain benzene ring, it will not produce benzene ring conjugated quinone structure chromophore under the irradiatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C263/20C07C265/04
CPCC07C263/10C07C263/20C07C265/04
Inventor 滕志君刘耀宗梁睿渊马瑞进张永波何爱晓张义新柳晟王超白立安张燕李龙孙树龙宋学勇
Owner 甘肃银光聚银化工有限公司
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