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Method for preparing acetic acid through catalytic carbonylation reaction

A technology of carbonylation reaction and reaction, which is applied in the field of preparing acetic acid by catalytic carbonylation reaction, can solve the problems of poor stability of rhodium catalyst, short oxidation time of product potassium permanganate, low reactivity, etc.

Active Publication Date: 2013-04-03
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the prior art has poor stability of the rhodium catalyst under low water conditions, low reactivity when producing acetic acid by carbonylation in low water, and short oxidation time of the product potassium permanganate, and provides a new The method for preparing acetic acid by catalytic carbonylation reaction

Method used

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  • Method for preparing acetic acid through catalytic carbonylation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Ruthenium complex Li + / H + [Ru(CO) 3 I 3 ] - Preparation: add ruthenium acetate or ruthenium iodide to acetic acid solution, add lithium iodide and water, HI, introduce CO, react at 3.0MPa, 190°C for 2h, and separate the ruthenium complex Li + / H + [Ru(CO) 3 I 3 ] - , IR v (CO): about 2106.7cm -1 , about 2039.0cm -1 , NMR spectrum, carbonyl peak position: 13 CNMR (100 MHz, CDCl 3 ): δ about 186.3ppm, through Xevo G2 QTof mass spectrometry, ESI / negative: 566.6020.

[0046]Add rhodium acetate, methyl iodide, distilled water, methyl acetate and lithium iodide once in the zirconium material autoclave that pressure gauge is housed in 200ml, make the rhodium concentration in the reaction system be 700ppm, methyl iodide 12wt%, distilled water 6wt%, Methyl acetate is 20wt%, lithium iodide is 6wt%, and the rest is acetic acid solvent. Keep the reaction temperature at 190°C and the reaction pressure at 3.0MPa. The average STY of the acetic acid reacted was 7.5 mo...

Embodiment 2

[0048] Ruthenium complex Li + / H + [Ru(CO)I 3 ] - , Li + / H + [Ru(CO) 2 I 3 ] - , Li + / H + [Ru(CO) 3 I 3 ] - Preparation: add ruthenium acetate or ruthenium iodide to acetic acid solution, add lithium iodide, water, HI, introduce CO, react at 2.0MPa, 190°C for 1h, and further separate and obtain the ruthenium complex Li + / H + [Ru(CO)I 3 ] - , Li + / H + [Ru(CO) 2 I 3 ] - , Li + / H + [Ru(CO) 3 I 3 ] - , Xevo G2 QTof mass spectrum, ESI / negative: 566.6020, 538.6073, 510.6120.

[0049] Add rhodium acetate, methyl iodide, distilled water, methyl acetate and lithium iodide once in the zirconium material autoclave that pressure gauge is housed in 200ml, make the rhodium concentration in the reaction system be 700ppm, methyl iodide 12wt%, distilled water 6wt%, Methyl acetate is 20wt%, lithium iodide is 6wt%, and the rest is acetic acid solvent. Keep the reaction temperature at 190°C and the reaction pressure at 3.0MPa. The average STY of the acetic...

Embodiment 3

[0051] Ruthenium complex [Ru(CO) 4 I 2 ] Preparation: put Ru 3 (CO) 12 and I 2 Dissolved in n-hexane, cooled to -40°C through a dry ice-acetone bath, then gradually warmed to room temperature, removed the solvent and dried in vacuum to obtain a brown solid, which was obtained by infrared analysis as [Ru(CO) 4 I 2 ] and [Ru(CO) 3 I 2 ] 2 mixture, the mixture was dissolved in CH 2 Cl 2 In the airtight container, 1.0 MPa of CO gas was introduced, and then heated to 40°C. After the reaction, the solvent CH was removed. 2 Cl 2 , to obtain a yellow solid as [Ru(CO) 4 I 2 ], IR v(CO) / cm -1 (CH 2 Cl 2 ): 2161, 2106, 2097, 2068.

[0052] Add rhodium acetate, methyl iodide, distilled water, methyl acetate and lithium iodide once in the zirconium material autoclave that pressure gauge is housed in 200ml, make the rhodium concentration in the reaction system be 700ppm, methyl iodide 12wt%, distilled water 6wt%, Methyl acetate is 20wt%, lithium iodide is 6wt%, and the res...

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Abstract

The invention relates to a method for preparing acetic acid through a catalytic carbonylation reaction, and mainly solves the problems of low stability of rhodium catalyst under the low water condition, low reaction activity when producing the acetic acid through low-water carbonylation, and short product oxidization time. Methanol or derivative of the methanol is adopted as a raw material, and is carbonylated with a liquid reaction composition to synthesize acetic acid; the reaction composition comprises the rhodium catalyst, a halogen promoter, methyl acetate, the acetic acid, water, a iodide-salt cocatalyst and a ruthenium complex used as a stabilizing agent, wherein the ruthenium complex is selected from at least one of [Ru(Co)aIb]n, Mn<+>[Ru(CO)aIb]<->n or Mn<+>[RuIb]<->n. The technical scheme solves the problems better, and can be applied in the industrial production of preparing the acetic acid through the catalytic carbonylation reaction.

Description

technical field [0001] The invention relates to a method for preparing acetic acid by catalyzing carbonylation reaction, in particular to a method for producing acetic acid by low-water carbonylation using ruthenium complex as a catalyst stabilizer. Background technique [0002] Acetic acid is an environmentally friendly organic acid and an important chemical intermediate and solvent for chemical reactions, from which hundreds of downstream products can be derived, such as vinyl acetate monomer, cellulose acetate, acetic anhydride, acetate, chloroacetic acid, Terephthalic acid, polyvinyl alcohol and metal acetate are widely used in the synthesis of medicine, synthetic fibers, light industry, textiles, leather, pesticides, explosives, rubber and metal processing, food and fine organic chemicals. [0003] The continuous production of acetic acid by the carbonylation reaction of methanol or methyl acetate with carbon monoxide is the most important method for producing acetic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/08C07C51/12B01J31/20
Inventor 高山林赖春波王苏李媛廖本仁张春雷揭元萍曾义红曹智龙刘艳
Owner SHANGHAI HUAYI GRP CO
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