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A kind of preparation method of 4,4' diphenylmethane diisocyanate

A technology of diisocyanate and diphenylmethane, which is applied in the field of preparation of 4,4' diphenylmethane diisocyanate, can solve the problems of inconsistency in atom economy, difficulty in transportation and long-term maintenance, cumbersome preparation methods, etc., and achieve High reactivity and stability, no three wastes, and simple process

Active Publication Date: 2021-07-20
万仑新材料(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively active chemical properties of aldehydes, it is difficult to transport and maintain them for a long time.
[0004] Patent CN1966489B discloses a two-step method for preparing diphenylmethane diisocyanate. In the method, firstly, aniline and formaldehyde are acid-condensed to obtain a mixture of amines, then react with phosgene, and distill to obtain diphenylmethane diisocyanate. Although the method has excellent yield and yield, the preparation method is cumbersome and uses highly toxic phosgene, which does not conform to atom economy

Method used

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  • A kind of preparation method of 4,4' diphenylmethane diisocyanate
  • A kind of preparation method of 4,4' diphenylmethane diisocyanate
  • A kind of preparation method of 4,4' diphenylmethane diisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 0.0240g (0.02mmol) copper-centered polyoxometalates [NH 4 ] 4 [CuMo 6 o 18 (OH) 6 ]·7H 2 O(CuMo 6 ), 0.3966g (2mmol) 4,4'-diaminodiphenylmethane, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride and 6mL solvent toluene, finally Put an oxygen balloon with carbon dioxide on the top of the reaction tube, and react at 30°C for 12h; The purified white molten solid was confirmed to be the product 4,4'-diphenylmethane diisocyanate by NMR.

Embodiment 2

[0030] Add 0.0240 g (0.02 mmol) iron-centered polyoxometalate [NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 O(FeMo 6 ), 0.3966g (2mmol) 4,4'-diaminodiphenylmethane, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride and 6mL solvent toluene, finally Put an oxygen balloon with carbon dioxide on the top of the reaction tube, and react at 30°C for 12h; The purified white molten solid was confirmed to be the product 4,4'-diphenylmethane diisocyanate by NMR.

Embodiment 3

[0032] Add 0.0234g (0.02mmol) of chromium-centered polyoxometalates [NH 4 ] 3 [CrMo 6 o 18 (OH) 6 ]·7H 2 O(CrMo 6 ), 0.3966g (2mmol) 4,4'-diaminodiphenylmethane, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride and 6mL solvent toluene, finally Put an oxygen balloon with carbon dioxide on the top of the reaction tube, and react at 30°C for 12 hours; after the reaction, take the above sample and measure GC-MS, it is known that the conversion rate of the reaction substrate is greater than 92%, and the product selectivity is 91%. The purified white molten solid was confirmed to be the product 4,4'-diphenylmethane diisocyanate by NMR.

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Abstract

The invention relates to a preparation method of 4,4'-diphenylmethane diisocyanate, which comprises adding a catalyst polyoxometalate and a solvent into a reaction vessel, and then adding raw materials 4,4'-diaminodiphenylmethane and phenylsilane, bound The acid agent and the dehydrating agent are mixed evenly together, and finally gaseous carbon dioxide is added, and the magnetic stirring is fully reacted at a certain temperature to obtain the product. The method of the present invention adopts M-Anderson type heteropolyacid as a catalyst, the required reaction conditions of the catalyst are mild, the specific selectivity is high, recyclable and environmentally friendly, the cleanliness of the industrial reaction is improved, and the economical efficiency of the process is improved. The production cost and the generation of three wastes are reduced, the pressure on environmental protection is reduced, and it is beneficial to industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 4,4' diphenylmethane diisocyanate. Background technique [0002] 4,4'-Diphenylmethane diisocyanate is the main downstream product of aromatic hydrocarbons, widely used in the production of polyurethane elastomers, synthetic fibers, artificial leather, solvent-free coatings and other polyurethane materials. The traditional synthesis method uses Pd, Ru, Rh, Au, Ir and other precious metals as catalysts. Although it has many advantages, the disadvantages of catalysts are expensive, high dosage and cannot be recycled and reused, which limits its industrial application. wide application. Therefore, chemists strive to find a green, efficient and recyclable catalyst. [0003] After the traditional preparation of diphenylmethane diisocyanate reacts with aniline and formaldehyde, it is neutralized with alkali and then distilled to obtain diphenylmethane...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C265/14C07C263/00
CPCC07C263/00C07C265/14Y02P20/584
Inventor 余焓但德敏吴志康魏永革韩生
Owner 万仑新材料(上海)有限公司