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Rhodium acetic anhydride complex, and its preparing method and use

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: 2007-11-14
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 use

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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

This invention relates to acetic anhydride rhodium complex, preparation method and application. Formulae I is the structure of this acetic anhydride rhodium complex. The invention selects acetic anhydride which be able to forming stable coordinate structure with metal rhodium as ligand, adopts acetic acid rhodium as precursor of complex, prepare a good performance hydroformylation catalyst: acetic anhydride rhodium complex. For the property of ligand, this complex has fine solubility in katalyzing carbonylation of methanol reaction system as well as katalyzing methyl acetate carbonylation system; under relatively gentle condition katalyze methanol to prepare acetic acid and katalyze methyl acetate to prepare acetic anhydride, present excellent catalytic activity and selectivity; furthermore, if add lithium iodide to reaction system, catalytic activity of complex will be greatly advanced.

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 U.S. Monsanto Company 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 synthesis...

Claims

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Application Information

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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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