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A kind of preparation method of dimethyl biphenyl diisocyanate

A technology of dimethyl biphenyl diisocyanate and di-o-toluidine, which is applied in the preparation of isocyanic acid derivatives, the preparation of organic compounds, chemical instruments and methods, etc., and can solve difficult-to-control and large-scale industrial production and process flow Complicated and cumbersome, mucosal irritation and other problems, to achieve high reactivity and stability, simple process, and no three wastes

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

[0004] Patent No. CN1935783B discloses a synthesis method of 3,3'-dimethyl-4,4'-biphenyl diisocyanate, but the process is complex and cumbersome, difficult to control and large-scale industrial production, and the process of synthesizing the target product The hydrogen chloride gas used has a strong irritating effect on the eyes and respiratory mucosa

Method used

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  • A kind of preparation method of dimethyl biphenyl diisocyanate
  • A kind of preparation method of dimethyl biphenyl diisocyanate
  • A kind of preparation method of dimethyl biphenyl diisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 0.0240 g (0.02 mmol) iron-centered polyoxometalate [NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 O(FeMo 6 ), 0.4246g (2mmol) o-toluidine, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride, 6mL anhydrous acetonitrile solvent, and finally above the reaction tube Put an oxygen balloon with carbon dioxide on it, and react at 30°C for 12 hours; after the reaction, take a sample and measure GC-MS. After testing and analysis, it is found that the conversion rate of the reaction substrate is greater than 96%, the product selectivity is 96%, and the separation and purification are excellent. Color crystals, confirmed by NMR to be the product dimethyl biphenyl diisocyanate.

Embodiment 2

[0030] Add 0.0240 g (0.02 mmol) aluminum-centered polyoxometalates [NH 4 ] 3 [AlMo 6 o 18 (OH) 6 ]·7H 2 O(AlMo 6 ), 0.4246g (2mmol) o-toluidine, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride, 6mL anhydrous acetonitrile solvent, and finally above the reaction tube Put an oxygen balloon with carbon dioxide on it, and react at 30°C for 12 hours; after the reaction, take a sample and measure GC-MS. After testing and analysis, it is found that the conversion rate of the reaction substrate is greater than 91%, the selectivity of the product is 92%, and the separation and purification are excellent. Color crystals, confirmed by NMR to be the product dimethyl biphenyl diisocyanate.

Embodiment 3

[0032] Add 0.0240g (0.02mmol) copper-centered polyoxometalates [NH 4 ] 4 [CuMo 6 o 18 (OH) 6 ]·7H 2 O(CuMo 6 ), 0.4246g (2mmol) o-toluidine, 0.2164g (4mmol) phenylsilane, 0.1012g (1mmol) triethylamine, 0.3067g (2mmol) phosphorus oxychloride, 6mL anhydrous acetonitrile solvent, and finally above the reaction tube Put an oxygen balloon with carbon dioxide on it, and react at 30°C for 12 hours; after the reaction, take a sample and measure GC-MS. After testing and analysis, it is found that the conversion rate of the reaction substrate is greater than 90%, the selectivity of the product is 90%, and the separation and purification are excellent. Color crystals, confirmed by NMR to be the product dimethyl biphenyl diisocyanate.

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Abstract

The invention relates to a method for preparing dimethyl biphenyl diisocyanate. First, a catalyst polyoxometalate and a solvent are added to a reaction vessel, and then the raw material di-o-toluidine, phenylsilane, an acid binding agent and a dehydrating agent are added and mixed together. Uniform, finally adding gaseous carbon dioxide, magnetic stirring at a certain temperature to fully react, that is, to obtain the product. The method of the invention adopts the M-Anderson type heteropoly acid as the catalyst, the catalyst requires mild reaction conditions, high specificity and selectivity, and the recyclability is environmentally friendly, the cleanliness of industrial reactions is improved, and the economy of the process is improved, Reduce manufacturing costs and the generation of three wastes, reduce environmental pressure, and facilitate industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of dimethyl biphenyl diisocyanate. Background technique [0002] Dimethyl biphenyl diisocyanate is the raw material of polyurethane elastomer, which can be used to prepare rubber, coating, foam, and can be used as raw material of oil seal material, heat-resistant resin modifier, urea-formaldehyde resin and heat-resistant coating raw material. Due to its wide application, the synthesis and application of toluene diisocyanate has attracted extensive attention of researchers at home and abroad. [0003] The traditional preparation of xylene biphenyl diisocyanate synthesizes dimethyl biphenyl diisocyanate through phosgene and 3,3'-dimethylbenzidine hydrochloride, but phosgene has great dangers in the process of preparation, storage, transportation and use Insufficiency, and extremely high requirements on operation and equipment, limit its extensive app...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C263/10C07C265/14B01J27/188B01J31/16B01J31/34
CPCB01J23/28B01J23/881B01J23/885B01J27/188B01J31/34B01J2231/4277C07C263/10C07C265/14
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