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Preparation and application of ruthenium-palladium double-active-center catalyst for carbonylation synthesis of acetic acid or acetic anhydride

A chemical synthesis and catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, carbon monoxide reaction to prepare carboxylic acid, etc., can solve problems such as deactivation, achieve low cost and reduce cost , the effect of inhibiting the precipitation of metal ions

Pending Publication Date: 2022-05-20
JIANGSU SOPO GRP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it is well known that palladium ion has good catalytic activity in carbonylation reaction, but it is easy to be deactivated by carbon monoxide reduction, which needs further research to meet production needs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] After mixing 0.25 moles of 2-vinylpyridine, 0.25 moles of acrylic acid, 0.5 moles of methyl acrylate and trace crosslinker (the content of the crosslinker monomer is 0.3% of the total amount of monomer molars), added to the benzene solvent and stirred, slowly added 1% of the monomer mole number of azo diisobutyronitrile as the initiator, reacted at 65 °C for 1h, after the solution was cooled, filtered by ether precipitation, then dissolved with acetone, repeatedly dissolved and precipitated 3-4 times, placed in vacuum to reduce pressure to constant weight, to obtain polymer ligand 1.

[0029] 0.03g lithium hydroxide and 2g polymer ligand 1 was dissolved in a mixture of 95% ethanol water mixed solvent, stirred at room temperature for 1h, and then added excess ether for precipitation, placed in vacuum under pressure to obtain product A;

[0030] Place 0.03g PdCl 2 Dispersed in ethanol, add dilute hydrochloric acid dropwise to make it fully dissolved, and add product A, at 30 ...

Embodiment 2

[0033]In a 250ml pressure vessel, 2.75g ruthenium palladium dual active center catalyst 1 (the system contains ruthenium about 2500ppm, palladium about 190ppm), methanol 1.1mol, iodomethane 0.2mol (co-catalyst), acetic acid 0.75mol (in the continuous reaction process usually retains a certain amount of acetic acid as a solvent to maintain the stability of the catalyst, no addition can also be reacted, but the continuous cycle usually has a certain amount of acetic acid); after the carbon monoxide is introduced, the temperature rises to 150 °C, The stirring speed is 500 rpm, the reaction pressure is controlled by 3.5MPa, and the reaction time is 30 minutes to obtain acetic acid.

[0034] The conversion frequency of the catalyst calculated by ruthenium is 478.8 / h, the conversion rate of methanol is 51.4%, the catalyst is simulated by the laboratory flash process, the catalyst is reused for catalytic reaction, the reaction conditions are unchanged, the catalyst is recycled 50 times, ...

Embodiment 3

[0036] In a 250ml pressure kettle, 5.47g ruthenium palladium dual active center catalyst 1 (the system contains ruthenium about 5000ppm, palladium about 380ppm), methanol 1.1mol, iodomethane 0.2mol (co-catalyst), acetate 0.75mol (in the continuous reaction process usually retain a certain amount of acetic acid as a solvent to maintain catalyst stability, no addition can also be reacted, but continuous cycles usually have a certain amount of acetic acid); after the carbon monoxide is introduced, the temperature rises to 150 °C, The stirring speed is 500 rpm, the reaction pressure is controlled by 3.5MPa, and the reaction time is 30 minutes to obtain acetic acid.

[0037] The conversion frequency of the catalyst calculated by ruthenium is 392.0 / h, the conversion rate of methanol is 84.1%, after the laboratory simulation flash process, the catalyst is reused for catalytic reaction, the reaction conditions are unchanged, the catalyst is recycled 50 times, the conversion frequency of t...

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Abstract

The invention belongs to the field of carbonylation synthesis of acetic acid and acetic anhydride, and discloses preparation and application of a ruthenium-palladium double-active-center catalyst for carbonylation synthesis of acetic acid or acetic anhydride. A micro-crosslinked hydrophilic polymer is prepared to serve as a metal ruthenium ligand, meanwhile, palladium ions are introduced to serve as a cocatalyst, a system expands into a cage-shaped structure in reaction liquid, and due to the ionization effect and the water holding effect of the system, the evaporation speed of a solution in the cage-shaped system can be greatly decreased, and therefore ruthenium precipitation is effectively inhibited. Compared with a conventional rhodium catalyst for preparing acetic acid through carbonylation, the metal ruthenium is low in price, the cost of the catalyst can be effectively reduced, and although the activity of a catalytic system is lower than that of a rhodium catalyst system, the catalytic system is good in stability and high in selectivity due to the comprehensive action of the system, so that the catalyst system has the characteristics of low cost and long service life.

Description

Technical field [0001] The present invention belongs to the field of carbonylated synthesis of acetic acid and acetic anhydride, specifically relates to the preparation and application of carbonylated synthesis of acetic acid or acetic anhydride of ruthenium palladium biactive center catalyst. Background [0002] The carbonylation reaction of methanol and carbon monoxide under the action of homogeneous rhodium catalyst to prepare acetic acid was an invention of Paulik et al. (US3769329) of Monsanto Company in the United States in the early 1970s, which opened up a new and important process route for the carbonyl synthesis of methanol. On this basis, later Halcon (BE819455), Ealtman, Ajinamoto (JapanKokai50 / 30,820), ShowaDenko (JapanKokai50 / 47,922), BP (B. VonSchlotheim, Chem.Industrie 1994, 9 / 89. 80) and Hoechst (DE2450965) made breakthroughs in the study of the same [Rh(CO)2I2]-anionic structure form of catalyst active species for the preparation of acetic anhydride by methyl ac...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C51/12C07C53/12C07C53/08
CPCB01J31/223C07C51/12B01J2531/821B01J2531/824C07C53/12C07C53/08Y02P20/584
Inventor 胡宗贵闫丰文邵守言朱桂生黄志军王忠华袁国卿段红宇唐丽
Owner JIANGSU SOPO GRP
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