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Catalyst for synthesizing methyl acetate through methanol carbonylation, preparation method and application thereof

A methyl acetate and catalyst technology, applied in the field of methyl acetate synthesis, can solve the problems of long reaction induction period, poor catalyst stability, etc., and achieve the effect of green process, low production cost and mild reaction conditions

Active Publication Date: 2015-03-11
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For metal sulfide catalysts, the complexity of sulfur occurrence forms leads to a longer reaction induction period and poor catalyst stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1.7g CuCl 2 .2H 2 O was dissolved in 180ml of deionized water, and 20.0g of HZSM-5 molecular sieve with a silicon-aluminum ratio of 35 was added to the solution, and the suspension was refluxed and stirred at 80°C for 5h, filtered and washed, and the resulting filter cake was dried at 100°C for 14h , Calcined at 500°C for 5h to obtain Cu / ZSM-5 catalyst.

[0023] 0.06g AgNO 3 Dissolve in 20ml of deionized water, add the Cu / ZSM-5 catalyst obtained above to this solution, impregnate at 30°C for 8h, then dry at 100°C for 14h, and roast at 500°C for 5h to obtain Cu-Ag / ZSM-5 catalyst, catalyst The mass composition is: ZSM-5:Cu:Ag=100:3.2:0.2

[0024] Catalyst in H 2 Under the atmosphere, reduce at 550°C for 5h, drop to 300°C, and introduce a mixture of methanol steam and CO preheated at 140°C, and the composition of the raw gas is CH 3 OH / CO=30v / 90v, the reaction gas space velocity is 3000ml / g cat .h, the reaction pressure is 2.0MPa, and the reaction performance of the ...

Embodiment 2

[0026] 2.9g CuCl 2 .2H 2 O was dissolved in 150ml of deionized water, and 20.0g of HZSM-5 molecular sieve with a silicon-aluminum ratio of 50 was added to the solution, the suspension was refluxed and stirred at 90°C for 4h, filtered and washed, and the obtained filter cake was dried at 120°C for 12h , Calcined at 400°C for 8h to obtain Cu / ZSM-5 catalyst.

[0027] 0.2g (NH 4 ) 2 MoO 4 Dissolve in 25ml of deionized water, add the Cu / ZSM-5 catalyst obtained above to this solution, impregnate at 40°C for 5h, then dry at 120°C for 12h, and roast at 400°C for 8h to obtain Cu-Mo / ZSM-5 catalyst, catalyst The mass composition is: ZSM-5:Cu:Ag=100:5.5:0.5.

[0028] Catalyst in H 2 Under the atmosphere, reduce at 600°C for 1 hour, drop to 340°C, and feed the mixture of methanol steam and CO to preheat at 140°C. The raw gas composition is CH 3 OH / CO=20v / 80v, the reaction gas space velocity is 1000ml / g cat .h, the reaction pressure is 1.5MPa, and the reaction performance of the cat...

Embodiment 3

[0030] 4.6g CuCl 2 .2H 2 O was dissolved in 180ml of deionized water, and 20.0g of HZSM-5 molecular sieve with a silicon-aluminum ratio of 80 was added to the solution, the suspension was refluxed and stirred at 60°C for 10h, filtered and washed, and the obtained filter cake was dried at 80°C for 24h , Calcined at 500°C for 5h to obtain Cu / ZSM-5 catalyst.

[0031] 0.25gAgNO 3 Dissolve in 30ml of deionized water, add the Cu / ZSM-5 catalyst obtained above to this solution, impregnate at 50°C for 4h, then dry at 80°C for 12h, and roast at 500°C for 8h to obtain Cu-Ag / ZSM-5 catalyst, catalyst The mass composition is: ZSM-5:Cu:Ag=100:8.6:0.8.

[0032] Catalyst in H 2 Reduction at 320°C for 5 hours in the atmosphere, lowered to 230°C, and a mixture of methanol steam and CO preheated at 130°C was introduced, and the raw gas composition was CH 3 OH / CO=30v / 70v, the reaction gas space velocity is 2000ml / g cat .h, the reaction pressure is 0.5MPa, and the reaction performance of the ...

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Abstract

A catalyst for synthesizing methyl acetate through methanol carbonylation is composed of HZSM-5, copper oxide and an additive of a metal M oxide, wherein a mass ratio of the HZSM-5, copper and M is 100:3-15:0.2-5. The catalyst is simple in a preparation method. The preparation method is green. The catalyst is high in selectivity of the methyl acetate and is good in stability.

Description

technical field [0001] The invention relates to a method for synthesizing methyl acetate, in particular to a catalyst for carbonylation of methanol to synthesize methyl acetate as well as its preparation method and application. technical background [0002] Methyl acetate is an important chemical product, which is widely used in many industries such as textile, fragrance and medicine, and has considerable potential utilization value in leather and polyester industries. At the same time, as an important platform compound, methyl acetate is widely used in the synthesis of scarce products such as vinyl acetate and methyl acrylate, especially the technical route of producing acetic anhydride through carbonylation of methyl acetate has become the mainstay of acetic anhydride synthesis technology. Development Direction The existing methyl acetate synthesis processes are mainly acetic acid-methanol esterification and methanol liquid-phase carbonylation. The acetic acid-methanol es...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/46B01J29/48C07C67/36C07C69/14
Inventor 李德宝郭荷芹侯博陈从标肖勇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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