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Catalyst for synthesizing dimethyl oxalate by CO as well as preparation method and application of catalyst

A technology of dimethyl oxalate and catalyst, which is applied in the field of catalyst and its preparation for synthesizing dimethyl oxalate with CO, can solve the problems of unresolved Cl ion corrosion, low selectivity of target products, high production cost, etc., and solve equipment corrosion , Solubility improvement, and the effect of improving utilization rate

Active Publication Date: 2017-07-07
NINGBO JINYUANDONG PETROCHEM ENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production cost of this invention is relatively high, and the corrosion problem caused by Cl ions has not yet been solved, and the selectivity of the target product is not strong, and there are many by-products. Therefore, it is necessary to further improve the method

Method used

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  • Catalyst for synthesizing dimethyl oxalate by CO as well as preparation method and application of catalyst

Examples

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preparation example Construction

[0023] The preparation method of this catalyst is made up of the following steps: 1. The acetate of metal strontium or barium and water are made into the acetate aqueous solution, and the concentration of the acetate aqueous solution is 0.002~0.2mol / L, and the carrier is heated at a temperature of Immerse in acetate aqueous solution at 40-60°C for 10-24 hours, then dry at 100-120°C for 4-8 hours to obtain the first solid, in which metal strontium or barium acetate and water are formulated into vinegar Aqueous salt solution refers to the acetate aqueous solution made of metal strontium acetate and water or the acetate aqueous solution made of metal barium acetate and water; 2. The metal palladium acetate or oxalic acid The salt is added with water to prepare an aqueous solution, the concentration of the aqueous solution is 0.01-0.3mol / L, then a water-soluble organic polymer is added to the aqueous solution to form a mixed solution, and the amount of the water-soluble organic pol...

Embodiment 1

[0035] Make an aqueous solution of strontium acetate and deionized water, the concentration of the aqueous solution is 0.5M, and the specific surface area is 275m 2 / g Al 2 o 3 Immerse in this solution for 12 hours at 50°C, and then dry at 100°C for 7 hours to obtain a solid; make an aqueous solution of palladium acetate, acetic acid and deionized water with a concentration of 0.08M, and then add polyvinyl alcohol to achieve a concentration of 6.5% of this aqueous solution; the solid impregnated with strontium was immersed in this solution for 12 hours, and then dried at 100°C for 5 hours and then taken out to obtain a solid; the fixed object was deionized with deionized water at room temperature After washing for 8 hours, it was dried at 105°C for 10 hours and calcined at 410°C for 14 hours to obtain catalyst 1.

[0036] The aqueous solution after washing at room temperature and the aqueous solution obtained by soaking strontium are subjected to normal pressure distillation...

Embodiment 2

[0038] Make an aqueous solution of barium acetate and deionized water, the concentration of the aqueous solution is 0.15M, and the specific surface area is 275m 2 / g Al 2 o 3 Immerse in this solution for 22 hours at 60°C, and then dry at 110°C for 5 hours to obtain a solid; make an aqueous solution of palladium acetate, acetic acid and deionized water at a concentration of 0.2M, and then add polyacrylamine to a concentration of 7.5% of this aqueous solution; soak the solid object impregnated with barium in this solution for 9 hours, then dry it at 110°C for 6 hours and take it out to obtain a solid object; put the fixed object at room temperature with deionized water After washing for 6 hours, it was dried at 115°C for 9 hours and calcined at 450°C for 12 hours to obtain catalyst 2.

[0039] The aqueous solution after washing at room temperature and the aqueous solution obtained by soaking barium are subjected to normal pressure distillation to separate polyacrylamine and wa...

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Abstract

The invention discloses a catalyst for synthesizing dimethyl oxalate by CO. The catalyst is prepared from metallic palladium as an active component, Al2O3 as a carrier and metallic strontium or metallic barium as an auxiliary catalyst, wherein the content of the metallic palladium is 0.05 to 1.0 percent of the weight of the carrier; the content of the metallic strontium or the metallic barium is 0.02 to 0.5 percent of the weight of the carrier. The catalyst is prepared by the following steps: preparing acetate of the metallic strontium or the metallic barium and deionized water into an aqueous solution; adding water into the acetate or oxalate of the metallic barium to obtain an aqueous solution; adding a water-soluble organic polymer into the aqueous solution to form a mixed solution; washing a solid substance obtained in the second step with water at room temperature for 5 to 10 hours, then drying the washed substance at the temperature of 100 to 120DEG C for 8 to 12 hours, and subsequently roasting the dried substance at the temperature of 400 to 500DEG C for 10 to 15 hours to obtain the required catalyst. The catalyst has the advantages that the loading capacity of metal is low, the conversion rate of raw materials is high, and the production cost of the catalyst is effectively reduced; the problem of equipment corrosion in a preparation process of the catalyst is solved, and the production cost of the catalyst is reduced.

Description

technical field [0001] The invention relates to the technical field of dimethyl oxalate preparation, in particular to a catalyst for synthesizing dimethyl oxalate with CO, a preparation method and an application method thereof. Background technique [0002] Dimethyl oxalate is an important raw material for coal-to-ethylene glycol. Ethylene glycol is an important chemical raw material, mainly used to make polyester polyester, polyester resin, and can produce synthetic resin PET, namely polyethylene terephthalate, fiber grade PET is polyester fiber, bottle grade PET is used to make mineral water bottles, etc. It can also produce alkyd resin, glyoxal, etc., and is also used as antifreeze, etc., and has a wide range of uses. In the past ten years, due to the rising demand of the domestic polyester industry, the import dependence has always been as high as 60%, and the domestic production gap is relatively large. my country is rich in coal and lacks oil, and more and more atte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58B01J35/10C07C67/36C07C69/36
CPCC07C67/36B01J23/58B01J35/633B01J35/647B01J35/615C07C69/36
Inventor 项裕桥臧未一
Owner NINGBO JINYUANDONG PETROCHEM ENG TECH
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