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PbO/ZrO2 catalyst for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate

A technology of methyl phenyl carbonate and diphenyl carbonate, which is applied in the field of PbO/ZrO2 catalysts, can solve problems such as difficult recycling and reuse, and difficult product separation, and achieve the effect of good reusability and simple preparation method

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AI Technical Summary

Problems solved by technology

Although these catalysts have high activity and good selectivity, they are difficult to separate from the product and are not easy to recycle and reuse.

Method used

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  • PbO/ZrO2 catalyst for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate
  • PbO/ZrO2 catalyst for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate
  • PbO/ZrO2 catalyst for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate

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Experimental program
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Effect test

Embodiment 1

[0025] Preparation of PbO / ZrO by impregnation method 2 catalyst. Take 4.2g ZrO 2 The carrier was added to 1.12g Pb(NO 3 ) 2 In the aqueous solution, stir evenly, let it stand for 24h, dry in an oven at 110°C for 24h, and then bake at 600°C in an air atmosphere for 5h to obtain PbO / ZrO with a PbO loading of 15.2%. 2 catalyst. In a 100mL three-necked round-bottomed flask equipped with a thermometer, nitrogen conduit, rectifying column, and fractionating head, the air in the high-purity nitrogen replacement device was introduced, and then 22.8g of raw materials MPC and PbO / ZrO were added. 2 Catalyst 0.9g, slowly heat up to 200 ℃ for reaction, the dimethyl carbonate fraction is continuously distilled through the rectification column during the reaction. After the reaction, the still liquid and fractions were qualitatively analyzed by HP-6890 / 5973 gas chromatography-mass spectrometer of Hewlett-Packard Company in the United States, and the quantitative analysis was carried out...

Embodiment 2

[0027] Preparation of PbO / ZrO by Mechanical Mixing 2 catalyst. Take 4.2g ZrO 2 Carrier and 1.12g Pb(NO 3 ) 2 Mix in an agate mortar, grind evenly, and bake in air at 600°C for 5 hours to obtain PbO / ZrO with a PbO loading of 15.2%. 2 catalyst. The analysis method of disproportionation reaction condition and product is the same as embodiment 1, and the activity result of catalyst is as follows: the methyl phenyl carbonate conversion rate is 64.8%, and diphenyl carbonate selectivity is 99.5%.

Embodiment 3

[0029] Preparation of PbO / ZrO by Co-precipitation 2 catalyst. Take 11.0g ZrOCl 2 ·8H 2 O and 1.12g Pb(NO 3 ) 2 Add it into 100mL deionized water, heat to 90°C to dissolve the solid completely; under strong stirring, slowly add ammonium hydroxide dropwise until the pH of the solution reaches about 9.3, and age the white suspension at 60°C for 12h; filter , washed, dried at 110°C for 24h, and then calcined at 600°C for 5h to obtain PbO / ZrO with a PbO loading of 15.2%. 2 catalyst. The disproportionation reaction conditions and the analysis method of product are the same as embodiment 1, and the activity result of catalyst is as follows: the conversion rate of methyl phenyl carbonate is 73.7%, and the selectivity of diphenyl carbonate is 99.7%.

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Abstract

The invention discloses a PbO / ZrO2 catalyst for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate and mainly solves problems of difficulty in catalyst separation, low diphenyl carbonate yield and the like. The catalyst takes ZrO2 as a carrier and PbO as an active component; PbO mass content is 1.9%-47.5% and preferably 7.6%-22.8%; an impregnation method, a mechanical grinding method or a coprecipitation method is adopted for preparation, and a calcination temperature is 400-800 DEG C. The PbO / ZrO2 catalyst is used for synthesis of diphenyl carbonate by disproportionation of methyl phenyl carbonate, methyl phenyl carbonate conversion rate is up to 76.6%, and diphenyl carbonate yield reaches 76.1%. The catalyst can be easily filtered, separated and recovered from a reaction system and high in stability, and after recycling for five times, the diphenyl carbonate yield still reaches 75% while diphenyl carbonate selectivity is kept above 99%. Therefore, the PbO / ZrO2 catalyst is high in practical application value.

Description

technical field [0001] The present invention relates to a kind of PbO / ZrO that is used for the liquid phase disproportionation reaction of methyl phenyl carbonate to synthesize diphenyl carbonate 2 catalyst. Background technique [0002] Diphenyl carbonate (DPC) is an organic carbonate with a wide range of uses, and it is the main raw material for the synthesis of polycarbonate by non-phosgene method. The transesterification of dimethyl carbonate (DMC) with phenol is considered to be one of the most promising industrial synthetic routes for non-phosgene synthesis of DPC. The transesterification of DMC and phenol is carried out in two steps: first, DMC and phenol are transesterified to generate intermediate methylphenyl carbonate (MPC) (Formula 1), and then MPC is disproportionated to generate DPC (Formula 2). The reaction rate of the first step of transesterification is much lower than that of the second step of disproportionation reaction, so the first step is the rate-co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/14C07C69/96C07C68/06
Inventor 陈彤王松林张华王公应曾毅
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