Homogeneous rhodium catalytic system of oxo-acetic anhydride and its use

A carbonylation and catalytic system technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of slow reaction, The reaction rate has no development value and other problems, so as to achieve the effect of improving activity, facilitating adjustment and optimization, and wide range of working conditions

Inactive Publication Date: 2007-04-04
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the carbonylation of methyl acetate using a rhodium-based catalyst for the carbonylation of methanol to acetic acid, the reaction proceeds so slowly that the reaction rate is not commercially exploitable even at temperatures up to 220°C.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add [Rh(CO) 2 Cl] 2 0.144g, methyl acetate 0.70mol, acetic acid 0.24mol, methyl iodide 0.22mol, LiI 3 ·3H 2 O 6.0g, (CH 3 CO) 2 O 0.15mol, (NH 4 ) 3 PO 4 4H 2 O 1.0g; after replacing the air in the reactor with carbon monoxide twice, fill the system with hydrogen at a pressure of 0.10MPa and carbon monoxide at a pressure of 3.0MPa; then heat up to 180±5°C and set the stirring speed at 400 rpm , the total reaction pressure is controlled to 5.0MPa, and the reaction time is 15min. Methyl acetate conversion rate is 48.2%, and the space-time yield of acetic anhydride is 9.8mol (CH 3 CO) 2 O / (L·h).

Embodiment 2

[0038] Add [Rh(CO) to the 250ml zirconium autoclave 2 Br] 2 0.200g, methyl acetate 0.70mol, acetic acid 0.24mol, methyl iodide 0.22mol, LiI 3 ·3H 2 O 10.0g, (CH 3 CO) 2 O 0.15mol, Zn 3 (PO 4 ) 2 4H 2 O 1.0g; after replacing the air in the reactor with carbon monoxide twice, fill the system with hydrogen at a pressure of 0.5MPa and carbon monoxide at a pressure of 3.0MPa; then heat up to 200±5°C and set the stirring speed at 400 rpm , the total reaction pressure is controlled to 5.0MPa, and the reaction time is 15min. Methyl acetate conversion rate is 57.5%, and the space-time yield of acetic anhydride is 13.8mol (CH 3 CO) 2 O / (L·h).

Embodiment 3

[0040] Add [Rh(CO) to the 250ml zirconium autoclave 2 I] 2 0.250g, methyl acetate 0.60mol, acetic acid 1.15mol, methyl iodide 0.22mol, LiI 3 ·3H 2 O 6.0g, (CH 3 CO) 2 O 0.15mol, Li 3 PO 4 1.5g; after replacing the air in the reactor with carbon monoxide twice, fill the system with hydrogen at a pressure of 0.2MPa and carbon monoxide at a pressure of 3.0MPa; then heat up to 180±5°C, set the stirring speed at 400 rpm, The total reaction pressure is controlled to 6.0MPa, and the reaction time is 15min. The methyl acetate conversion rate is 83.2%, and the space-time yield of acetic anhydride is 12.7mol (CH 3 CO) 2 O / (L·h).

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Abstract

A Ru catalyst system with high activity and stability for preparing oxo acetoanhydride from methyl acetate by catalytic homogenizing reaction features that the phosphate additive is used in it besides the alkyl iodine and the iodate of alkali metal are used as its cocatalyst.

Description

technical field [0001] The invention relates to a homogeneous reaction catalyst system for carbonylation of acetic anhydride. [0002] The invention also relates to the use of the catalyst system described above. Background technique [0003] Acetic anhydride is not only a compound used in large quantities as a raw material for the production of cellulose acetate, but also an important raw material for the synthesis of chemical products such as drugs, fragrances, and dyes. [0004] Acetic anhydride is produced initially by wood pulp distillation, then by the ketene process based on acetic acid, acetone, and finally by the oxidation of acetaldehyde. Methyl acetate carbonylation has now partially replaced these traditional, more expensive methods. [0005] Driven by rising oil and raw material prices in the 1970s, novel metal-catalyzed acetic anhydride production processes were intensively studied and resulted in production technologies using syngas as feedstock. Syngas is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J27/08B01J27/14B01J31/16C07C51/56C07C53/12
Inventor 袁国卿钱庆利石秀丽张抒峰李峰波闫芳邵守言凌晨曹宏兵
Owner INST OF CHEM CHINESE ACAD OF SCI
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