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Catalyst for hydrogenation, preparation method thereof and use thereof

A hydrogenation reaction and catalyst technology, which is applied to the hydrogenation reaction catalyst and its preparation and application fields, can solve the problems of short service life of the catalyst and no precedent for industrial application, achieve good stability, reduce separation equipment and procedures, and reduce production. cost effect

Inactive Publication Date: 2010-06-16
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above catalysts have a short service life, and the process of gas-phase hydrogenation of oxalate to ethylene glycol has no industrial application precedent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In the first step, pour 45g of treated white carbon black into a round bottom flask, mix with 100g of deionized water and add nitric acid to adjust the pH to 3. 360g containing 118g Cu(NO 3 ) 2 The copper nitrate solution is mixed with the above solution, mixed evenly and placed in a 75°C water bath for subsequent use;

[0041] In the second step, the prepared 5wt% ammonia solution is slowly added dropwise to the above solution, stirring is maintained during the dropwise addition, and the water bath is refluxed; the pH value of the final solution is controlled to be 8.

[0042] After the third step, the reaction is completed, the feed liquid is filtered while it is hot, washed with deionized water several times, and then washed with ethanol and suction filtered;

[0043] In the fourth step, the catalyst filter cake is dried at 95°C for 12 hours and then calcined at 450°C for 6 hours. Obtain the catalyst, code-named A.

[0044] Catalyst A was broken and screened to 4...

Embodiment 2

[0047] The first step is to pour 40g of diatomaceous earth into a round bottom flask, mix it with 200g of deionized water, add 60g of potassium carbonate solid, mix well and put it in a water bath at 75°C for later use; the pH value is 12;

[0048] The second step prepares 200g containing 88g Cu(NO 3 ) 2 and 3g Ni(NO 3 ) 2 copper nitrate / nickel nitrate solution.

[0049] The third step is to slowly add the metal solution dropwise to the mixed solution of diatomaceous earth, electric stirring and reflux reaction in a water bath at 75°C for 2 hours, then let it stand for 8 hours, and control the pH value to 9; refer to Example 1 to wash and dry the catalyst After the post-processing operation, the catalyst was obtained, code-named B.

[0050] Put Catalyst B into the reaction tube by crushing and screening 20-40 mesh; raise the reaction tube from room temperature to 350 °C at a rate of 4 °C / min, during which the hydrogen content gradually increases from 0.5% to 100%, and finall...

Embodiment 3

[0053] Catalyst preparation is the same as embodiment 2, and difference is that the second step is replaced with 88g Gu(NO 3 ) 2 , 1.5gCo(NO 3 ) 2 and 1.5g Mn(NO 3 ) 2 mixed solution. Get catalyst, code name C.

[0054] The reduction condition was to raise the reaction tube from room temperature to 300°C at a rate of 2°C / min, during which the hydrogen content gradually increased from 10% to 100%, and finally adjusted to the reaction process conditions after reduction under pure hydrogen for 6 hours.

[0055] The reaction raw material is methyl glycolate, and the catalyst reaction process conditions and results are shown in Table 1.

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Abstract

The invention provides a catalyst for hydrogenation, a preparation method thereof and use thereof. The chemical formula of the catalyst is CuOx-ROy / SiO2. The catalyst of the invention is used for hydrogenation in a gas-phase method for preparing glycol and is prepared from the raw materials including but not limited to oxalate or ethyl glycolate and hydrogen. The catalyst of the invention requires low reaction temperature and allows for a wide temperature range. The catalyst of the invention has extremely high operation elasticity, high activity and selectivity within a temperature range of 160 to 260 DEG C and a pressure range of 1 to 10 MPa, high time space yield, over 99 percent raw material conversion rate, over 96 percent target product selectivity, less than 0.1 percent by-product yield, high stability and a one-pass service life of up to 3,500 hours. The catalyst can greatly reduce energy consumption, save follow-up product separation equipment and procedures reduce production cost and avoid equipment corrosion and environmental pollution.

Description

technical field [0001] The invention relates to a catalyst for hydrogenation reaction and its preparation method and application. Background technique [0002] Polyol is an important organic chemical raw material, such as ethylene glycol, which is mainly used in the manufacture of non-ionic surfactants, ethanolamines, polyester fibers, antifreeze and explosives, and is also used to prepare low freezing point coolants (for engines) ), can also be used directly as a solvent. In addition, it is also widely used in the tobacco industry, textile industry and cosmetic industry. [0003] Most of the existing production processes of ethylene glycol use petroleum routes, using ethylene as raw material, first producing ethylene oxide by direct oxidation, and then producing ethylene glycol through liquid-phase catalytic or non-catalytic hydration. Such as Chinese patent 02112038.2, US patent 5874653, and Japanese patent 82106631 all disclose this route. In this method, a large amoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78C07C31/20C07C29/12
CPCY02P20/52
Inventor 戴成勇李永刚吴良泉周亚明唐大川王东辉肖本端施春晖
Owner SHANGHAI HUAYI ENERGY CHEM
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