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Catalyst for preparation of acetic acid and methyl acetate through carbonylation of methanol and preparation method thereof

A methanol carbonylation and methyl acetate technology, applied in the preparation of carbon monoxide or formate reaction, chemical instruments and methods, carbon monoxide reaction to prepare carboxylic acid, etc., can solve the strong corrosion of halogen accelerators, increase production costs, corrosion equipment, etc. problems, to achieve high catalyst selectivity, improve catalytic activity, and improve the effect of crystallization

Active Publication Date: 2013-01-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is following shortcoming in this method: precious metal rhodium catalyst is expensive and raw material is in short supply and has improved production cost, and in homogeneous catalyzed reaction, product separation is difficult, and catalyzer is easy to run off and causes cost to rise; Make promotor with iodomethane to have strong impact on reaction system Corrosion and difficult separation of catalyst and product in liquid phase
The conversion rate of methanol is about 99.5%, and the conversion rate of acetic acid is as high as 99.8%, but due to the 2 S04 is a catalyst, and there are problems such as corrosion of equipment and environmental pollution.
[0010] Carbonylation of methanol to ester is a very attractive and atom-economical process in the chemical industry. However, there are currently three problems in the carbonylation of methanol at home and abroad that are similar to the preparation of acetic acid. The cost and shortage of precious metal rhodium catalysts, halogen The strong corrosion of the accelerator and the difficult separation of the catalyst and the product in the liquid phase are three major problems
Many studies are devoted to finding a catalyst for gas-phase carbonylation at low pressure. Although Ni / C catalysts with iodide as a promoter have good activity and selectivity for gas-phase carbonylation of methanol, they still have disadvantages. , on the one hand, the corrosion is serious, and on the other hand, the product separation is very difficult. At present, it is difficult to find a heterogeneous catalyst that can effectively carry out the carbonylation reaction without a halogen promoter.

Method used

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  • Catalyst for preparation of acetic acid and methyl acetate through carbonylation of methanol and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take by weighing 10g mordenite (commercially available), 0.63g CuCl 2 2H 2 O. First, the HMOR was pre-fired at 500°C for 3 hours, cooled, and sealed for later use. The copper chloride weighed above was dissolved in 50 ml of absolute ethanol, and magnetically stirred at room temperature until completely dissolved. Then pour 10g of HMOR into the dissolved solution, stir until the mordenite is evenly dispersed, then start to heat up to 90°C, and continue stirring until the ethanol evaporates completely. The resulting solid was dried overnight in an oven at 120°C. in N 2 Under atmosphere, the dried solid was calcined at 350°C for 4h. Get 5% CuCl 2 / HMOR catalyst, where CuCl 2 The loading amount is 5%.

Embodiment 2

[0031] Take by weighing 10g mordenite (commercially available), 0.63g CuCl 2 2H 2 O and 1.84 g NiCl 2 ·6H 2O. First, the HMOR was pre-fired at 300°C for 2 hours, cooled, and sealed for later use. The copper chloride and nickel chloride weighed above were dissolved in 50 ml of absolute ethanol, and magnetically stirred at room temperature until completely dissolved. Then pour 10g of HMOR into the dissolved solution, stir until the mordenite is evenly dispersed, then start to heat up to 90°C, and continue stirring until the ethanol evaporates completely. The resulting solid was dried overnight in an oven at 90°C. in N 2 Under atmosphere, the dried solid was calcined at 300°C for 3h. Get 5% CuCl 2 -10%NiCl 2 / HMOR catalyst, where CuCl 2 The loading is 5%, NiCl 2 The loading amount is 10%. .

Embodiment 3

[0033] Take by weighing 10g mordenite (commercially available), 0.92g NiCl 2 ·6H 2 O and 1.88g CuCl 2 2H 2 O. First, the HMOR was pre-fired at 500°C for 3 hours, cooled, and sealed for later use. Dissolve the nickel chloride and copper chloride weighed above in 50 ml of absolute ethanol, and stir magnetically at room temperature until completely dissolved. Then pour 10g of HMOR into the dissolved solution, stir until the mordenite is evenly dispersed, then start to heat up to 90°C, and continue stirring until the ethanol evaporates completely. The resulting solid was dried overnight in an oven at 120°C. in N 2 Under atmosphere, the dried solid was calcined at 350°C for 4h. Catalyst 15% CuCl 2 -5%NiCl 2 / HMOR, where CuCl 2 The loading is 15%, NiCl 2 The loading amount is 5%.

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Abstract

The invention discloses a catalyst for preparation of acetic acid and methyl acetate through carbonylation of methanol, which comprises an active component and a carrier, which the active component includes at least one of CuCl2 and NiCl2, and the carrier is mordenite. The invention also discloses a method for preparing the catalyst for preparation of acetic acid and methyl acetate through carbonylation of methanol by using an impregnation method, which comprises the following steps: impregnating the mordenite in a compound solution containing the active component; after a certain period of time, removing the residual liquid; and drying, and roasting to obtain the catalyst for preparation of acetic acid and methyl acetate through carbonylation of methanol. In the preparation method, the active component is evenly distributed in the catalyst system, and the catalytic activity of the catalyst is enhanced; and one part of CuCl2 and NiCl2 enter pores of the mordenite to become the active component, and the active component is less possible to lose. The catalyst prepared by the invention is suitable for preparation of acetic acid and methyl acetate through direct carbonylation of methanol, has high selectivity, and can be used without adding any corrosive assistant, thereby greatly lowering the cost.

Description

technical field [0001] The invention relates to a catalyst for preparing acetic acid and methyl acetate and a preparation method thereof, in particular to a catalyst for preparing acetic acid and methyl acetate by carbonylation of methanol and a preparation method thereof. Background technique [0002] Acetic acid is an important organic chemical raw material, which can produce cellulose acetate, vinyl acetate, acetic anhydride, acetate, etc., and is widely used in fiber, plasticizer, adhesive, copolymer resin, pharmaceutical, dye, food and other industries. The synthesis methods of acetic acid mainly include the oxidation of acetaldehyde or ethylene, the fermentation of carbohydrates and the carbonylation of methanol. Because methanol has the advantages of sufficient raw material supply, low cost, and relatively small environmental pollution, the production of acetic acid by methanol carbonylation has accounted for more than 60% of the world's acetic acid production, and th...

Claims

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Application Information

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IPC IPC(8): B01J29/24C07C53/08C07C51/12C07C69/14C07C67/36
Inventor 王树荣骆仲泱邱坤赞方梦祥岑可法朱玲君
Owner ZHEJIANG UNIV
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