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Catalyst for synthesizing ethylidene diacetate

A technology of diethylene acetate and catalysts, which is applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problem of low yield and selectivity of diethylene acetate low, high selectivity of diethylene acetate, etc., to improve activity and stability, improve yield and selectivity

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the technical problems to be solved by this invention is the problem of low yield and low selectivity of diacetate, and a new catalyst for the synthesis of diacetate is provided, which has diacetate The characteristics of high yield and high selectivity to diethylene acetate

Method used

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  • Catalyst for synthesizing ethylidene diacetate
  • Catalyst for synthesizing ethylidene diacetate
  • Catalyst for synthesizing ethylidene diacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of catalyst: NiCl containing 6.35gNi, 3.10gMo and 1.60gSn 2 6H 2 O, MoCl 5 and SnCl 2 2H 2 O is fully mixed and dissolved in acetic acid to obtain 500ml of impregnation solution, and 1.0L of spherical SiO with a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, and stood for 2 h under N 2 The catalyst was obtained by raising the temperature to 500° C. and calcining for 4 h in the atmosphere.

[0022] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 8.0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 175°C, the molar ratio of carbon monoxide to hydrogen is 3:1, continue the reaction for 7.5h, stop the reaction....

Embodiment 2

[0045] Preparation of catalyst: Ni(NO 3 ) 2 6H 2 O, MoO 3 and Sn(NO 3 ) 2 Fully mix and dissolve in dilute hydrochloric acid to obtain 500ml of impregnation solution, and 1.0L Al 2 o 3 The carrier was immersed in the above impregnating solution, left to stand for 2 hours, heated to 400° C. and calcined for 4 hours in a He atmosphere to obtain the catalyst.

[0046] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to discharge the air in the kettle, then pressurize to 1.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 2.0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 130°C, the molar ratio of carbon monoxide to hydrogen is 1:10, continue the reaction for 3.0h, then stop the reaction.

[0047] Product analysis: The reaction mixture obtained from the above reac...

Embodiment 3

[0050] Preparation of catalyst: NiSO containing 15.0gNi, 5.00gMo and 5.00gSn 4 7H 2 O, MoO 3 Fully mixed with SnO and dissolved in concentrated hydrochloric acid to obtain 500ml of impregnating solution, and 1.0L Al 2 o 3 The carrier was immersed in the above impregnating solution, left to stand for 2 hours, and then heated to 600° C. for 4 hours in an Ar atmosphere to be calcined to obtain the catalyst.

[0051] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 10.0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 200°C, the molar ratio of carbon monoxide to hydrogen is 10:1, continue the reaction for 10.0h, stop the reaction.

[0052] Product analysis: The reac...

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Abstract

The invention relates to a catalyst for synthesizing ethylidene diacetate and a preparation method of the catalyst for synthesizing ethylidene diacetate. According to the catalyst and the preparation method, the problems that an ethylidene diacetate catalyst is relatively low in activity and selectivity in the prior art are mainly solved. The catalyst comprises a carrier as well as nickel, molybdenum and tin which are loaded to the carrier, wherein the content of nickel is 3.0g / L-15.0g / L, the content of molybdenum is 1.0g / L-5.0g / L, and the content of tin is 0.5g / L-5.0g / L; the carrier is selected from at least one of silicon oxide and aluminum oxide. According to the technical scheme, the technical problems are well solved. The catalyst can be applied to the industrial production of vinyl acetate.

Description

technical field [0001] The invention relates to a catalyst for synthesizing diethylene acetate, a preparation method and a synthesis method of diacetate. Background technique [0002] Production of vinyl acetate and acetic acid. The novel part of the whole process is the hydroformylation reaction of methyl acetate, the catalyst is modified with rhodium chloride and β-picoline and methyl iodide, and the carbon monoxide insertion reaction is the key point of the whole technology. [0003] The preparation method of synthesizing diethylene diacetate by methyl acetate has been disclosed by US4,429,150 (titled: Manufacture of ethylidene diacetate), namely with methyl acetate or methyl ether, carbon monoxide and hydrogen as raw materials, catalyst adopts VIII Diethylene acetate is synthesized in the presence of halides or acetates and phosphorus-containing polar solvents. US5,354,886 (title: Catalysts on inorganic carriers for producing ethylidene diacetate) mentioned that RhCl ...

Claims

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Application Information

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IPC IPC(8): B01J23/887C07C69/16C07C67/36
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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