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Method for preparing TiO2/SiO2 catalyst for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester

A technology of diphenyl carbonate and catalyst, which is applied in the field of preparation of heterogeneous catalysts, can solve problems such as the decrease of catalyst reaction activity, and achieve the effects of short preparation time, simple preparation method and high selectivity

Inactive Publication Date: 2013-05-29
JIANGSU OXIRANCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And after the calcination temperature is higher than 423K, due to the disappearance of the butyl group and the SnO 2 The crystal phase is produced, the reactivity of the catalyst drops sharply, and the yield of DPC is less than 1.6%.

Method used

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  • Method for preparing TiO2/SiO2 catalyst for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester
  • Method for preparing TiO2/SiO2 catalyst for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 9g urea and dissolve in 10.8g H 2 O, after stirring evenly, add acetylacetone and tetrabutyl titanate, and stir at room temperature for 3h. After adding tetraethyl orthosilicate, with HNO 3 Adjust the pH of the solution (the molar ratio of Ti / Si is 1:20, and the molar ratio of acetylacetone and tetrabutyl titanate is 3:5); after the gel is aged for 2 hours, the volatile components are evaporated at 50°C. Calcined at 600°C for 4h.

Embodiment 2

[0022] Carry out the transesterification reaction of dimethyl carbonate and phenol with the catalyst prepared in embodiment 1

[0023] (1) in the there-necked flask that is connected with air guide tube and thermometer, constant pressure dropping funnel and rectifying column, add the catalyst 1.0 gram of embodiment 1;

[0024] (2) under feeding nitrogen, add 15 grams of phenol;

[0025] (3) When heating to 180°C, start to add dimethyl carbonate (DMC) dropwise, and the total amount of DMC added is 13.5ml. React 9.0 hours, constantly steam the mixed fraction of methyl alcohol and dimethyl carbonate by the rectifying column in the reaction process;

[0026] (4) The mixed fraction and the reaction solution containing the main product methyl phenyl carbonate and diphenyl carbonate are all analyzed by Shimadzu GC-14B gas chromatograph, quantified by calibration and normalization method, and record: the transformation rate of phenol is 38.3%, the yields of methyl phenyl carbonate a...

Embodiment 3

[0028] The preparation step of catalyst is the same as embodiment 1, but changes TiO 2 with SiO 2 The molar ratio is shown in Table 2. Carry out the transesterification reaction of dimethyl carbonate and phenol with the prepared catalyst, the reaction conditions are the same as in Example 2, and the activity results are shown in Table 1.

[0029] Table 1 Different TiO 2 / SiO 2 The effect of molar ratio on catalyst activity

[0030]

[0031] *MPC-methylphenyl carbonate, DPC-diphenyl carbonate

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Abstract

A method for preparing TiO2 / SiO2 catalyst for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester includes: utilizing SiO2 as a carrier and TiO2 as an active component, utilizing urea as additives and diacetone as inhibitor, and roasting after dissolving and gelling, wherein the titanium and silicon mole ratio is 1:1-60. The method mainly solves the problem about low ester exchange yield of multi-phase catalyst. The TiO2 / SiO2 catalyst prepared by the method has higher catalytic activity and ester exchange selectivity for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester, phenol transformation rate can reach 42.9%, overall selectivity of ester exchange products (methyl phenyl carbonate and diphenyl carbonate) is larger than 99.9%, and byproducts are not detected. The method for preparing TiO2 / SiO2 catalyst for exchanging and synthesizing diphenyl carbonate by dimethyl carbonate and phenol ester is simple and short in preparation time, and raw materials therefore are low in cost and easy to obtain.

Description

technical field [0001] The invention discloses a preparation method of a heterogeneous catalyst for transesterifying dimethyl carbonate and phenol to synthesize diphenyl carbonate. Background technique [0002] Diphenyl carbonate (DPC) is an important chemical intermediate with low toxicity and no pollution. Many organic compounds and polymer materials can be synthesized through halogenation, nitration, hydrolysis, ammonolysis and other reactions, especially polycarbonate PC, which can replace highly toxic phosgene and bisphenol A through melt transesterification to synthesize excellent performance. The synthesis of DPC mainly adopts phosgene method, oxidative carbonylation method and transesterification method. The phosgene method is being gradually eliminated due to the highly toxic and highly corrosive raw materials. The oxidative carbonylation method has a high atom utilization rate, but the main catalyst, such as noble metal Pd, is expensive, and there are problems su...

Claims

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Application Information

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IPC IPC(8): B01J21/08C07C69/96C07C68/06
Inventor 陈彤李碧静胡晓佳王公应唐荣芝杨建刘旭冉蔡家胜
Owner JIANGSU OXIRANCHEM CO LTD
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