Rhodium acetic anhydride complex, and its preparing method and application

A technology of rhodium acetic anhydride and complexes, applied in the field of acetic anhydride rhodium complexes and its preparation, can solve problems such as poor catalyst stability, limited theoretical research, and no value for industrial development, and achieve excellent catalytic activity and selectivity The effect of improving the performance and catalytic activity

Active Publication Date: 2009-12-16
JIANGSU SOPO CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the stability of this type of catalyst is not good, and it is still limited to theoretical research at present, and does not have the value of industrial development.

Method used

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  • Rhodium acetic anhydride complex, and its preparing method and application
  • Rhodium acetic anhydride complex, and its preparing method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 0.6 mole of acetic anhydride and dissolve it in 3.0 mole of methanol, stir well and divide into three parts. Under stirring in an ice bath, 0.1, 0.2, 0.3 moles of rhodium acetate were added respectively. After continuing to stir for 20 minutes, add excess diethyl ether to precipitate and filter; the product was washed with diethyl ether three times, and depressurized at room temperature to constant weight to obtain acetic anhydride rhodium complex.

[0019] The elemental analysis results of the complex are as follows:

[0020] the element

Embodiment 2

[0022] Add 0.2 grams of acetic anhydride rhodium complex, 2.48 moles of methanol, 0.65 moles of acetic acid, and 0.34 moles of methyl iodide in the reactor. After feeding CO, the temperature is raised to 140 ° C, the reaction pressure is kept at 4.0 MPa, and the stirring speed is 500 rpm. Time 30 minutes. After the reaction, the product composition was determined by gas chromatography: the conversion rate of methanol was 100%, and the product composition was 0.82 moles of methyl acetate and 1.45 moles of acetic acid.

Embodiment 3

[0024] Add 0.25 grams of rhodium complexes, 2.48 moles of methanol, 0.5 moles of acetic acid, 0.34 moles of methyl iodide, and 0.08 moles of lithium iodide in the reaction kettle. After feeding CO, the temperature was raised to 150° C., the pressure was maintained at 4.0 MPa, the stirring speed was 500 rpm, and the reaction time was 20 minutes. After the reaction, the product composition was determined by gas chromatography: the conversion rate of methanol was 100%, and the product composition was 0.57 moles of methyl acetate and 1.80 moles of acetic acid.

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Abstract

The invention discloses an acetic anhydride rhodium complex, a preparation method and an application thereof. The acetic anhydride rhodium complex provided by the present invention has a structure such as formula. The present invention selects acetic anhydride capable of forming a stable coordination structure with metal rhodium as a ligand, uses rhodium acetate as a precursor of the complex, and prepares a carbonylation catalyst with excellent performance—a rhodium acetic anhydride complex. Due to the nature of the ligand, the complex has excellent solubility in the reaction system of catalytic methanol carbonylation and catalytic methyl acetate carbonylation reaction system. It can catalyze methanol to prepare acetic acid and methyl acetate under relatively mild conditions. The preparation of acetic anhydride exhibits excellent catalytic activity and selectivity; moreover, the catalytic activity of the complex of the present invention can be significantly improved by adding lithium iodide to the reaction system.

Description

technical field [0001] The invention relates to an acetic anhydride rhodium complex and a preparation method thereof, and the application of the acetic anhydride rhodium complex in catalyzing methanol carbonylation to prepare acetic acid and in catalyzing methyl acetate carbonylation to prepare acetic anhydride. Background technique [0002] At the end of the 1960s, F.E.Paulik et al. of Monsanto Company in the U.S. reported a soluble carbonyl rhodium-iodine catalyst system (US 3769329) for methanol carbonylation, because this catalytic system had a higher catalytic effect on methanol carbonylation. Activity and selectivity, and mild reaction conditions, make a breakthrough in the research and industrial production of methanol carbonylation. After decades of development, low-pressure methanol carbonylation has become the most important synthetic method in the industrial production of acetic acid and acetic anhydride. [0003] In the process route of methanol carbonylation sy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00B01J23/46C07C51/12
Inventor 宋勤华邵守言凌晨曹宏兵袁国卿闫芳钱庆利李峰波
Owner JIANGSU SOPO CHEM
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