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Method for catalytic synthesis of diaryl ethane

A technology for diaryl ethane and aromatic compounds, applied in the field of catalytic synthesis of diaryl ethane, which can solve the problems of difficult control of reaction conditions, unsatisfactory PXE yield, and difficult disposal of waste acid

Inactive Publication Date: 2010-02-17
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The following documents disclose the preparation of diaryl ethane by the reaction of aromatic compounds and styrene (or its derivatives): Japan Petrochemical Co., Ltd. and domestic manufacturers all use concentrated sulfuric acid as a catalyst to synthesize PXE, but the reaction conditions Difficult to control, low yield, difficult waste acid treatment, severe corrosion to production equipment, etc.; JP63-238028 (1988), using Y-shaped zeolite; Polymer Journal 12NO.6 (1880), 407, using Nafion, Amberlyst 15 or CF 3 SO 3 H; and EP-A-421340 using L zeolite
But the PXE productive rate of above-mentioned all synthetic methods is not ideal

Method used

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  • Method for catalytic synthesis of diaryl ethane
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  • Method for catalytic synthesis of diaryl ethane

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: the synthesis of Al-MCM-41 molecular sieve catalyst

[0019] (1) Weigh a certain amount of sodium silicate and dissolve it in 40ml of deionized water, and stir it at 30°C to 40°C to dissolve it to obtain a sodium silicate solution; weigh a certain amount of cetyltrimethyl bromide Dissolve ammonium in 25ml of deionized water and stir to dissolve at 50°C to 60°C to obtain a template solution; add sodium silicate solution to the template solution while stirring, and stir for 30 minutes at room temperature to obtain an initial gel mixture (2) Dissolve a certain amount of aluminum sulfate in 15ml deionized water and add to the above solution, stir for 30min to obtain a white colloidal solution; (3) adjust the pH value to about 10 with 2mol / L dilute sulfuric acid, and then stir 1.5h, the mixture was moved into a polytetrafluoroethylene-lined stainless steel reactor, sealed, and crystallized in an oven at 110°C for 3 days; (4) after the crystallization was comple...

Embodiment 2

[0020] Embodiment 2: the preparation of H type mordenite

[0021] With a concentration of 1mol / L NH 4 NO 3 The solution performs NH on the sample of sodium mordenite NaM[n(Si) / n(Al)=23.5] 4 + To exchange, press NH 4 NO 3 The ratio of solution (volume) / zeolite (mass) is 10 / 1, stirred at 95°C, exchanged for 1 hour and then left for 20 minutes, poured off the residual liquid and replaced it with fresh solution for re-exchange, this process was repeated 4 times in total, using a vacuum pump Suction filter and wash with hot distilled water. Dry at 110°C for 10h, and then bake in a muffle furnace at 550°C for 5h to obtain a hydrogen-type catalyst. After 1mol / LNH 4 NO 3 After desalting 5 times, the Na in the zeolite + The content has been reduced to 0.032%.

Embodiment 3

[0022] Embodiment 3: the synthesis of diaryl ethane (depending on the catalyst)

[0023] Add 20 to 40 g of aromatic compounds and 0.24 to 0.44 g of catalyst (such as mesoporous molecular sieve Al-MCM-41) into a 100 ml four-necked flask equipped with a stirrer, condenser, thermometer and constant pressure dropping funnel. Under standard atmospheric pressure, the reaction temperature is 120-160°C, heat to reflux, and then slowly add 4 g of styrene dropwise under stirring. The fixed concentration of styrene should not exceed 0.05%, and the reaction time is 1-4 hours. The crude product is first distilled off unreacted raw materials by atmospheric distillation (140-190°C), and then the fraction is collected at a residual pressure of 0.01-0.001MPa and a temperature of 190-250°C to obtain the product.

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Abstract

The invention relates to a method for preparing diaryl ethane of a formula I by reacting an aromatic compound of a formula II with styrene of a formula III in the presence of a solid acid catalyst under the condition that the reaction temperature is between 120 and 160 DEG C, the pressure is one standard atmosphere, the mass ratio of the raw materials of the styrene (a formula III) and the aromatic compound (a formula II) is between 1:5 and 1:10, the dosage of the catalyst is 0.1 to 2 percent of the total batch charging mass percent, and the reaction time is 1 to 4 hours. The method is characterized by using a self-made mesoporous molecular sieve A1-MCM-41 or a loaded phosphotungstic acid and a modified mordenite of a loaded molybdophosphoric aicd as the solid acid catalyst. In a formula (I), each one of R<1>, R<2>, R<3>, R<4>, R<5> and R<6> is hydrogen or C1-C8-alkyl. In the formula (II), each one of R<1>, R<2>, R<3>, R<4>, R<5> and R<6> is the same as that in the formula (I), and R<1> in the formula (III) is the same as that in the formulae (I) and (II).

Description

technical field [0001] The invention relates to a method for catalyzing the synthesis of diaryl ethane, by making aromatic compounds and styrene in the medium-pore molecular sieve Al-MCM-41 or the modified mordenite loaded with phosphotungstic acid and phosphomolybdic acid as solid acid The reaction is carried out in the presence of a catalyst, thereby increasing the yield. Background technique [0002] Diaryl ethane is a high boiling point solvent, referred to as PXE. Because of its low viscosity, high boiling point, low freezing point, high solubility, strong color rendering ability, stable electric heating performance, and high voltage resistance, it is currently widely used as a solvent for pressure-sensitive dyes of carbon-free copy paper and electrical insulating oil. In addition, it can also be used as a plasticizer, organic heat carrier and lubricating oil for plastic processing. It has become a fine chemical product with a very large market demand, so how to impro...

Claims

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Application Information

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IPC IPC(8): C07C2/66C07C15/52B01J29/04B01J29/18
Inventor 宿新泰肖峰党富民孙超饶雪辉王吉德
Owner XINJIANG UNIVERSITY
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