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Triple bond partial hydrogenation method and catalyst thereof

A catalyst, palladium catalyst technology, applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the problem of urgent improvement of reaction selectivity, many side reactions of dimerization, etc. problems, to achieve the effect of wide application range of substrates, enhanced selective adsorption, and reduction of side reactions of raw material acetylenic alcohol dimerization

Pending Publication Date: 2021-12-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for partial hydrogenation of a triple bond and its catalyst, which solves the problem that there are many side reactions in the dimerization of substrates in partial hydrogenation reactions and the reaction selectivity needs to be improved urgently

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Pd-Mn-Pb(II) / CaCO 3 (1) Partial hydrogenation catalyst preparation.

[0042]Accurately weigh 10.0g of calcium carbonate carrier at room temperature, add it to the flask, then add 100mL of deionized water to obtain a suspension, slowly add tetrachloropalladium acid (30mg / mL, 42.3mL) aqueous solution to the suspension under stirring And manganese acetate (25mg / mL, 2.0mL) aqueous solution. After the addition was complete, the mixture was stirred at room temperature for 1 hour, then heated to 80° C., and 0.5 M sodium formate solution (10.2 mL) was added in 30 minutes. The reaction mixture was stirred for 1 hour, filtered and washed with deionized water to wash the catalyst powder several times. Remove the inorganic salt impurities therein. The obtained powder was dried in an oven at 80° C. for 12 hours. The dry powder obtained above was suspended in 40 mL of deionized water and stirred for 10 minutes. After adding lead acetate (5.0wt%, 12.6g) aqueous solution in 20 minu...

Embodiment 2

[0044] Pd-Mo-Pb(II) / CaCO 3 Partial hydrogenation catalyst preparation.

[0045] Accurately weigh 5.6g of calcium carbonate carrier at room temperature, add it to the flask, then add 50mL of deionized water to obtain a suspension, slowly add tetrachloropalladium acid (30mg / mL, 23.7mL) aqueous solution to the suspension under stirring And molybdenum acetate (18mg / mL, 3.3mL) aqueous solution. After the addition was complete, the mixture was stirred at room temperature for 1 hour, then heated to 80° C., and 0.5 M sodium formate solution (5.7 mL) was added in 30 minutes. The reaction mixture was stirred for 1 hour, filtered and washed with deionized water to wash the catalyst powder several times. Remove the inorganic salt impurities therein. The obtained powder was dried in an oven at 80° C. for 12 hours. The dry powder obtained above was suspended in 40 mL of deionized water and stirred for 10 minutes. Add lead acetate (5.0wt%, 7.0g) aqueous solution over 20 minutes, after th...

Embodiment 3

[0047] Pd-W-Pb(II) / CaCO 3 Partial hydrogenation catalyst preparation.

[0048] Accurately weigh 6.3g of calcium carbonate carrier at room temperature, add it to the flask, then add 50mL of deionized water to obtain a suspension, slowly add tetrachloropalladium acid (30mg / mL, 26.7mL) aqueous solution to the suspension under stirring And tungsten tetrachloride (21mg / mL, 2.9mL) aqueous solution. After the addition was complete, the mixture was stirred at room temperature for 1 hour, then heated to 80° C., and 0.5 M sodium formate solution (6.4 mL) was added in 30 minutes. The reaction mixture was stirred for 1 hour, filtered and washed with deionized water to wash the catalyst powder several times. Remove the inorganic salt impurities therein. The obtained powder was dried in an oven at 80° C. for 12 hours. The dry powder obtained above was suspended in 40 mL of deionized water and stirred for 10 minutes. Add lead acetate (5.0wt%, 8.0g) aqueous solution over 20 minutes, after...

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Abstract

The invention provides a triple bond partial hydrogenation method and a catalyst thereof. The catalyst comprises a carrier, and a main catalyst metal palladium, an auxiliary agent metal and a poisoning agent which are loaded on the carrier; the carrier is calcium carbonate, barium sulfate, aluminum oxide and silicon oxide; the auxiliary metal is tungsten, molybdenum and manganese metal simple substances; and the poisoning agent is lead salt, zinc salt and chromium salt. The catalyst in the hydrogenation method provided by the invention has excellent partial hydrogenation activity and selectivity, and can realize partial hydrogenation of carbon-carbon triple bonds at high yield to obtain an olefin product. In the reaction process, carbon dioxide and a small amount of alcohol amine are introduced into the reaction system, so that the occurrence of dimerization side reaction of the raw material alkynol is reduced, and the selectivity of partial hydrogenation reaction is further improved.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis and catalyst preparation, and in particular relates to a triple bond partial hydrogenation method and a catalyst thereof. Background technique [0002] The triple bond selective hydrogenation reaction is widely used in various chemical fields, whether it is bulk chemicals or fine chemicals. For example, in refining, cracking ethylene generally contains a small amount of acetylene, which has a strong poisoning effect on polyethylene catalysts, so it is necessary to purify acetylene in ethylene before polymerization. The method widely used at present is to partially hydrogenate acetylene Get ethylene. In the field of fine chemicals, allyl alcohol is a widely existing structural unit, such as allyl salicylate, allyl cinnamate, allyl caproate, leaf alcohol, linalool, dihydromyrcenol, etc., in Its molecular structure has an allyl structure, and one of the most commonly used methods to obtain th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C33/025C07C33/02C07C33/035B01J27/232B01J27/053B01J23/652B01J23/656B01J37/02
CPCB01J27/232B01J27/053B01J23/6525B01J23/6527B01J23/6562B01J37/0201C07C29/17C07C33/025C07C33/02C07C33/035
Inventor 黄文学闫化莲马宏宇薛勇勇孙媛媛马文成王永军黎源
Owner WANHUA CHEM GRP CO LTD
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