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Dimethyl diphenyl methane catalytic synthesizing process

A technology of dimethyldiphenylmethane and synthesis process, applied in the field of green catalytic synthesis process, can solve problems such as environmental pollution, complex reaction process and the like, and achieve the effect of high activity and reuse activity

Inactive Publication Date: 2005-10-05
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the reaction process is complicated, a large amount of waste water and by-products after alkali neutralization are generated, and the environmental pollution is serious.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, in the reactor of 150 milliliters, add 1 gram of phosphotungstic acid, 48 milliliters of toluene (450 millimoles), 2.7 grams of polyoxymethylene (90 millimoles) successively, after sealing, replace the air in the reactor with nitrogen ( Five times), then start stirring and heating, and start timing when the temperature in the reactor reaches 140° C. After 4 hours of reaction, stop heating and stirring, take out the reactor and quickly cool to room temperature, and open the reactor. The reaction solution and the catalyst are centrifuged, and the catalyst can be recovered and reused. The reaction solution was subjected to vacuum rectification, unreacted toluene was recovered and reused; the rectified solid product was dissolved with ethanol, and then vacuum rectification was repeated twice to obtain 13.74 grams of solid product. The product identified by chromatography, mass spectrometry, infrared and hydrogen nuclear magnetic resonance is dimethyl diphenylm...

Embodiment 2

[0025] Embodiment 2, according to the same reaction condition (140 ℃, 4 hours) and separation steps of embodiment 1, catalyst selects 1 gram of phosphomolybdic acid, silicotungstic acid, 10% SO 4 2- / ZrO 2 , HX molecular sieve, HY molecular sieve, HZSM-5 molecular sieve, Hβ molecular sieve, mordenite, the output of the product dimethyl diphenylmethane obtained is as shown in table 1:

[0026] catalyst

Embodiment 3

[0027] Embodiment 3, according to the same reaction conditions (140 DEG C, 4 hours) and raw material composition (toluene 450 millimoles, polyoxymethylene 90 millimoles) of embodiment 1, the catalyst selects different amounts of phosphotungstic acid for use, investigated successively 0.2 grams, 0.3 gram, 0.4 gram, 0.5 gram, 1.5 gram, 2.0 gram, the output of dimethyl diphenylmethane under the catalyst action of 2.5 gram metering, the obtained result is shown in Table 2:

[0028] The amount of phosphotungstic acid

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PUM

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Abstract

This invention is dimethyl biphenyl methane synthetic catalyzing technique. It uses methylbenzene and formaldehyde as the raw materials, and under the function of solid acid catalyst to process condensation reaction. The weight ratio of methylbenzene and formaldehyde is 2 / 1-1 / 5, the reaction condition is: in the temperature of 100-200deg.C, the reaction time is 1-8 hours to get dim ethyl biphenyl methane. The catalysts comprises:HX molecular sieve, HY molecular sieve, HZSM-5 molecular sieve, H beta molecular sieve, mordenite, phosphatotungstic acid, molybdophosphoric acid, silicotungstic acid and loaded phosphatotungstic acid, molybdophosphoric acid, silicotungstic acid. This invention has simple reaction technique and little environmental pollution.

Description

technical field [0001] The invention relates to an environmentally friendly and highly efficient green catalytic synthesis process for dimethyldiphenylmethane. Background technique [0002] Dimethyldiphenylmethane (also known as xylylmethane, molecular formula: CH 3 C 6 h 4 CH 2 C 6 h 4 CH 3 , Molecular weight: 196, melting point 28-29 degrees, boiling point 289-291 degrees, soluble in ethanol, ether, etc.) is an excellent high-temperature heat carrier, insulating oil, important dyes, spices and pharmaceutical synthetic intermediates. In the industry, it can be used to synthesize pefloxacin, metaxalone, etc., and in the dye industry, it can be used to synthesize basic sophorin, etc.; at the same time, dimethyl diphenylmethane is also an important intermediate of polyamide ester (MDI). [0003] At present, there are two main synthesis processes of dimethyldiphenylmethane, one using p-xylene and p-chlorotoluene as raw materials, 3 Or direct condensation under the actio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/86C07C15/02C07C15/16
Inventor 侯昭胤金顶峰罗永明郑小明
Owner ZHEJIANG UNIV
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