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Catalyst for catalyzing methanol carbonylation, preparation method of catalyst and method for preparing acetic acid and methyl acetate by methanol carbonylation

A technology of methanol carbonylation and methyl acetate, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, carbon monoxide reaction to prepare carboxylic acid, etc. , the reactivity and lifespan are not ideal, etc., to achieve the effect of high yield, high conversion rate and high stability

Active Publication Date: 2018-04-24
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some progress has been made in the research of nickel-based catalytic systems, the stability, reactivity and lifespan of such catalysts are not ideal, and the current research is still in the laboratory stage.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:

[0050] Weigh 5.72g of nickel nitrate, dissolve in 20g of distilled water, slowly add 10g of SiO2 under slow stirring 2 In this method, after ultrasonic impregnation for 1 hour, standing at room temperature for impregnation for 24 hours, drying at 80°C for 8 hours, drying at 120°C for 16 hours, and roasting at 500°C for 3 hours to obtain a catalyst precursor.

[0051] Catalyst precursor in 20vol1% CH 4 -80vo1%H 2 In the mixed gas, reduce at 350 ℃ for 4h, that is.

[0052] Methanol carbonylation was carried out in a pressurized continuous fixed-bed reactor to prepare acetic acid and methyl acetate, and the activity of the catalyst prepared in this example for catalyzing methanol carbonylation was evaluated.

[0053] The specific operation is as follows: before the reaction, the catalyst (6 mL) was first reduced in hydrogen at 300° C. for 3 h, and then the temperature o...

Embodiment 2

[0060] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:

[0061] Weigh 8.58g of nickel nitrate, dissolve it in 15g of distilled water, slowly add 10g of Al under slow stirring 2 o 3 In , after ultrasonic impregnation for 3 hours, it was impregnated at room temperature for 36 hours, then dried at 100°C for 24 hours, and calcined at 550°C for 5 hours to obtain a catalyst precursor.

[0062] Catalyst precursor using 10vol1% ethane-90vol1% H 2 In the mixed gas, reduce it at 390°C for 5h to get it.

[0063] The method provided in Example 1 was used to evaluate the activity of the catalyst for methanol carbonylation provided in this example.

[0064] The specific reaction conditions are as follows: at 250° C., 5 MPa, the feed rate of hydrogen is 222 mL / min, the feed rate of CO is 111 mL / min, and the feed rate of methanol is 0.2 mL / min.

[0065] When reacting for 72 hours, it was measured that the conversion rate of methanol was ...

Embodiment 3

[0067] A catalyst for catalyzing the carbonylation of methanol, which is prepared by the following method:

[0068] Weigh 4.66g of nickel chloride, dissolve it in 12g of distilled water, slowly add it into 10g of activated carbon under slow stirring, after ultrasonic impregnation for 2 hours, after impregnating at room temperature for 48 hours, first bake at 80°C for 8h, then at 120°C Baking for 24 hours for drying, and baking at 500° C. for 6 hours in a nitrogen atmosphere to obtain a catalyst precursor.

[0069] Catalyst precursor in 10vol1% butane-90vol1% H 2 The mixed gas was reduced at 400°C for 6h to obtain.

[0070] The method provided in Example 1 was used to evaluate the activity of the catalyst for methanol carbonylation provided in this example.

[0071] The specific reaction conditions are as follows: at 290° C., 6 MPa, the feed rate of hydrogen is 222 mL / min, the feed rate of CO is 111 mL / min, and the feed rate of methanol is 0.2 mL / min.

[0072] When reacting ...

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PUM

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Abstract

The invention provides a catalyst for catalyzing methanol carbonylation, a preparation method of the catalyst and a method for preparing acetic acid and methyl acetate by methanol carbonylation. The preparation method of the catalyst comprises the following steps: impregnating a carrier in a metal salt solution of nickel, then drying, roasting and reducing mixed gases of alkane and hydrogen at thetemperature of 300 to 1000 DEG C, wherein the nickel accounts for 1 to 20 percent of the mass of the carrier. The preparation method has the advantages of simple preparation process, low energy consumption and capability of realizing scale production; the catalyst prepared by the method can efficiently catalyze the methanol carbonylation to obtain the acetic acid and the methyl acetate; meanwhile, the catalyst has the advantages of high conversion rate for methanol, excellent catalytic activity, better stability and longer service life. When the catalyst is applied to the method for preparingthe acetic acid and the methyl acetate by the methanol carbonylation, the conditions required by a catalytic reaction are relatively mild and the preparation efficiency is effectively improved at thesame time.

Description

technical field [0001] The invention relates to the field of catalysts, and in particular to a catalyst for catalyzing methanol carbonylation, a preparation method thereof, and a method for preparing acetic acid and methyl acetate by methanol carbonylation. Background technique [0002] Acetic acid is an important organic chemical raw material, which can be used to produce vinyl acetate monomer, anhydride, terephthalic acid, polyvinyl alcohol, acetates, cellulose acetate, etc. . In recent years, due to the development of downstream products of acetic acid, acetic acid has become one of the few petrochemical products whose output and demand are growing rapidly. [0003] As an important organic chemical, methanol is widely used in industry and can be used to produce various chemical products such as formic acid, formaldehyde, acetic acid, vinyl acetate, methyl formate and dimethyl carbonate. Methanol carbonylation is an important field of methanol application. Synthesis of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C51/12C07C53/08C07C67/36C07C69/14C07C27/22
CPCB01J23/755B01J37/0201B01J37/08B01J37/18B01J37/343C07C51/12C07C67/36C07C53/08C07C69/14
Inventor 许晓伟谢忠杨德亮于丽萍赵妍侯红霞王建伟王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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