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Catalyst for preparing divalent alcohol by hydrogenating dibasic acid ester and preparation method and application thereof

A dicarboxylic acid ester and catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the complex preparation process, no industrial application precedent, and harsh conditions. and other problems, to achieve the effect of low reaction temperature, favorable for industrial application and improved stability

Active Publication Date: 2009-12-02
HAO HUA CHENGDU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second step of hydrogenation of oxalate to ethylene glycol is still in the research stage, and there is no precedent for industrial application
However, the preparation process of this series of catalysts is complicated and the conditions are harsh. The activity of the catalyst is related to the content of impurities and the physical properties of the carrier. It is necessary to strictly limit the impurities such as S and Fe in the catalyst and raw materials. The carrier needs to be pretreated. Physical properties such as pore diameter and pore volume also need to be strictly limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 34.5g of sodium silicate to configure 200mL aqueous solution, weigh 24.1g of Cu(NO 3 ) 2 and 1.2g Ni(NO 3 ) 2Add deionized water to prepare a 200mL mixed salt solution, raise the temperature and keep it at 50°C, then add a sodium silicate aqueous solution dropwise under stirring, and control the pH value of the solution at the end of the reaction to 7.0; After washing with deionized water three times and suction filtering; the catalyst was dried at 80°C for 12 hours, and then calcined at 350°C for 6 hours to finally obtain catalyst A. Catalyst A was formed and screened to 20-40 mesh and placed in a reaction tube. With pure hydrogen at a flow rate of 100mL / min, it was reduced at 250°C for 6 hours and then adjusted to the reaction process conditions for hydrogenation reaction. Reaction raw material selects dimethyl oxalate.

[0032] Catalyst reaction conditions and results are shown in Table 1.

[0033] Table 1 Catalyst test data comparison

[0034] E...

Embodiment 2

[0036] Weigh 24.1g Cu(NO 3 ) 2 and 1.0g Mn(NO 3 ) 2 Add deionized water to prepare a mixed salt solution with a concentration of 0.2M, add dropwise 28% ammonia water, stir and mix evenly, and control the pH value to 11; into the salt solution and stirred for 2 hours; heated the above solution to 70°C, and reacted at constant temperature for 5 hours until the pH value of the solution at the end of the reaction was 7.0; after the reaction was completed, the feed solution was filtered while it was hot, and then washed three times with deionized water and then Suction filtration; the catalyst was dried at 90°C for 12 hours, and then calcined at 500°C for 6 hours to finally obtain catalyst B. Catalyst B was formed and screened to 20-40 mesh and placed in a reaction tube. With pure hydrogen at a flow rate of 100mL / min, it was reduced at 260°C for 4 hours and then adjusted to the reaction process conditions for hydrogenation reaction. Reaction raw material selects dimethyl oxalat...

Embodiment 3

[0039] Catalyst preparation is the same as in Example 2, the difference is that the deionized water washing is replaced by ethanol washing twice, the reaction raw material is diethyl oxalate, the reduction condition is that the hydrogen content gradually increases from 2% to 100%, and finally adjusted at 300 ° C for 4 hours. To the reaction process conditions to react.

[0040] Catalyst reaction conditions and results are shown in Table 1.

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PUM

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Abstract

The invention relates to a catalyst for preparing divalent alcohol by hydrogenating dibasic acid ester and a preparation method and application thereof, which belong to the technical field of catalytic hydrogenation. The catalyst takes metal copper as a main active component, one or a few of rare earth elements or transitional metal elements as a cocatalyst, and SiO2 as a carrier, wherein the content of the metal copper is 5 to 50 percent of the weight of the catalyst, the content of the cocatalyst is 0.1 to 10 percent of the weight of the catalyst, and the balance of the carrier. The catalyst can be used for the reaction for preparing the divalent alcohol by hydrogenating the dibasic acid ester, such as the preparation of ethylene glycol by using diethyl oxalate; and the catalyst has better activity, selectivity and stability, high time space yield of products, simple flow and easiness for continuous operation.

Description

technical field [0001] The invention discloses a catalyst for synthesizing dihydric alcohols by gas-phase hydrogenation of dibasic carboxylic acid esters, a preparation method and application thereof, and belongs to the technical field of catalytic hydrogenation. Background technique [0002] Dihydric alcohol is an important basic raw material of organic chemical industry, such as ethylene glycol, it is not only used for the production of polyethylene terephthalate (PET, polyester resin), alcohol ester resin, polyester fiber and polyester It is an important raw material for plastics, and it is a commonly used high-boiling point solvent. The freezing point of its 60% aqueous solution is -40°C. It can be used as a winter car antifreeze and a refrigerant for aircraft engines; it is also used in the production of plasticizers, paints, and adhesives. Agents, surfactants and indispensable components of capacitor electrolyte. In addition, it is also widely used in the tobacco indu...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/889B01J23/83C07C29/149C07C31/20
CPCY02P20/52
Inventor 王科范鑫袁小金许红云
Owner HAO HUA CHENGDU TECH
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