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Catalyst for oxalate ester synthetic reaction and preparation method of catalyst

A synthesis reaction and oxalate ester technology, applied in the direction of carbon monoxide or formate reaction preparation, catalyst carrier, chemical instrument and method, etc., can solve the problem of active component loss stability, etc., and achieve high tolerance and selectivity High, conducive to the effect of industrial scale-up

Active Publication Date: 2014-08-06
商丘国龙新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a catalyst for the synthesis of oxalate esters and a preparation method thereof, aiming at solving the problem of poor stability of the loss of active components in the actual application process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The catalyst for the synthesis reaction of oxalate in this example uses zirconia-alumina composite oxide as a carrier, and zirconia accounts for 5% of the mass of the carrier in terms of mass. The content of active component palladium is 0.2% of carrier weight;

[0023] The metal additive is zinc, and the zinc content is 0.3% of the weight of the carrier.

[0024] Its preparation method is as follows:

[0025] (1) The zirconium-aluminum composite oxide is prepared by co-precipitation method, wherein the content of zirconia accounts for 5% of the composite oxide by mass, and the carrier is roasted by two-stage temperature programming before use; the roasting process includes from room temperature to The heating rate of ℃ / min was programmed to heat up to 300°C and roasted for 3 hours, and then the temperature was raised to 850°C for 5 hours at a heating rate of 2°C / min; It mainly exists in the form of δ-alumina or θ-alumina, with a small amount of α-alumina; the specifi...

Embodiment 2

[0030] The catalyst used for the synthesis reaction of oxalate in this example uses zirconia-alumina composite oxide as a carrier, and zirconia accounts for 16% of the mass of the carrier in terms of mass.

[0031] The content of active component palladium is 0.3% of carrier weight;

[0032] The metal additive is nickel, and the content of the nickel metal additive is 0.01% of the weight of the carrier.

[0033] Its preparation method is as follows:

[0034](1) The zirconium-aluminum composite oxide was prepared by the co-precipitation method, in which the content of zirconia accounted for 16% of the composite oxide by mass, and the carrier was calcined by a two-stage temperature program before use; The heating rate was programmed to 500°C for 1 hour, and then the heating rate was 3°C / min to 1100°C for 3 hours; after firing, the zirconia in the composite carrier mainly existed in the tetragonal crystal form, and the alumina mainly existed in the form of δ- Exist in the form ...

Embodiment 3

[0039] The catalyst for the synthesis reaction of oxalate in this example uses zirconia-alumina composite oxide as the carrier, and zirconia accounts for 20% of the mass of the carrier in terms of mass. The content of active component palladium is 0.03%% of carrier weight;

[0040] The metal additive is iron, and the iron content is 0.5% of the weight of the carrier.

[0041] Its preparation method is as follows:

[0042] (1) The zirconium-aluminum composite oxide was prepared by the co-precipitation method, in which the content of zirconia accounted for 20% of the composite oxide by mass, and the carrier was roasted by two-stage temperature programming before use; the roasting process included starting from room temperature at 5°C / min The heating rate was programmed to 400°C for 2 hours, and then the heating rate was 3°C / min to 1000°C for 4 hours; after firing, the zirconia in the composite carrier mainly existed in the tetragonal crystal form, and the alumina mainly existed...

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Abstract

The invention discloses a catalyst for the oxalate ester synthetic reaction and a preparation method of the catalyst. The catalyst uses a zirconia-aluminium oxide composite oxide as a carrier, wherein the zirconia in the composite oxide mainly exists in a square crystal form, and the aluminium oxide in the composite oxide mainly exists in a delta-aluminium oxide form. After being subjected to hydro-thermal treatment by a urea solution, the carrier is subjected to active load in the next step. A main active component of the catalyst is palladium, and an assistant is selected from one of zinc, nickel and iron. Based on the weight of the carrier, the content of the palladium is 0.03-0.3%, and the content of the assistant is 0.01-0.5%. By the adoption of the method, the prepared catalyst is uniform in active component distribution, can show the advantages of good catalytic activity and high stability when being used in the oxalate ester synthetic reaction by using gas-phase carbonic oxide and nitrous acid ester, can resist influence of industrial raw material gas impurities such as nitric oxide and methyl alcohol steam, and is more suitable for an industrialized production process.

Description

technical field [0001] The invention relates to a catalyst for the synthesis reaction of oxalate and a preparation method thereof, in particular to a catalyst and a preparation method suitable for the reaction of synthesizing oxalate from carbon monoxide and nitrite. Background technique [0002] Oxalate is an important class of organic chemical raw materials, which can be used to prepare oxalic acid, oxalyl chloride, oxamide, ethylene glycol, etc., and is an important basic chemical raw material. [0003] Since 1965, Fenton et al. in the United States discovered that under the catalysis of palladium, carbon monoxide can undergo a coupling reaction in an alcohol medium to generate oxalate, which has opened up a new direction in carbon-chemistry. my country's energy resources are characterized by relatively rich coal resources, lack of oil, and little gas; the use of synthesis gas to prepare chemical raw materials is of great significance to the rational use of energy. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/60B01J23/89B01J32/00C07C69/36C07C67/36
Inventor 刘艳侠梁旭赵立红苗杰李丰魏灵朝蒋元力
Owner 商丘国龙新材料有限公司
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