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Method for preparing unsaturated alcohol through selective hydrogenation of alpha,beta-unsaturated aldehyde

A selective hydrogenation and unsaturated technology, applied in the field of selective hydrogenation of β-unsaturated aldehydes to unsaturated alcohols, α, can solve the problems of low conversion rate of raw materials and product selectivity, small production capacity, and difficult separation of catalysts and products , achieve high raw material conversion rate and unsaturated alcohol selectivity, save energy consumption and save separation cost

Inactive Publication Date: 2017-08-18
SHANGHAI HUAYI GRP CO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of small production capacity, low raw material conversion rate and product selectivity, and difficult separation of catalyst and product in the prior art. It provides a new selective hydrogenation of α and β unsaturated aldehydes unsaturated alcohol method

Method used

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  • Method for preparing unsaturated alcohol through selective hydrogenation of alpha,beta-unsaturated aldehyde
  • Method for preparing unsaturated alcohol through selective hydrogenation of alpha,beta-unsaturated aldehyde
  • Method for preparing unsaturated alcohol through selective hydrogenation of alpha,beta-unsaturated aldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh a certain amount of MgO carrier, prepare an aqueous solution containing a certain amount of copper nitrate and lanthanum nitrate, the concentrations are 0.5M and 0.22M respectively, soak at room temperature for 12h, and then stir and dry at 100°C. The obtained sample was dried at 120° C. for 12 h, and then calcined at 400° C. for 8 h to prepare precursor 1 . Prepare palladium chloride and rhodium chloride aqueous solutions with concentrations of 0.1M and 0.01M respectively, add 0.1M ethylene glycol and stir, impregnate precursor 1 at room temperature for 12 hours, then stir and dry at 90°C, and dry the obtained samples in Dry at 120°C for 12h, and bake at 500°C for 4h. The catalyst is shaped into cylindrical particles (diameter 3.0mm, height 3.0mm), 100 grams of catalyst is packed into a fixed bed reactor, and reduced at 300°C for 10h (3.0MPa, 2000h -1 ). The supported catalyst 0.05%Rh-7%Cu-1.1%Pd-3%La / MgO was obtained.

[0023] After adding the acrolein into t...

Embodiment 2

[0027] A certain amount of copper nitrate and zirconium nitrate was formulated into a solution, and co-precipitated with aqueous sodium carbonate solution at a precipitation temperature of 50°C, then filtered, dried at 120°C for 8 hours, and calcined at 400°C for 4 hours. Prepare a certain aqueous solution of chloroauric acid and indium nitrate, the concentrations are 0.1M and 0.01M respectively, add 0.5M sodium dodecylbenzene sulfonate, soak at room temperature for 6h, then dry at 80°C, and dry at 120°C for 12h , 380 ℃ roasting 4h. The catalyst is shaped into a clover shape (diameter 3.0mm, length 3.0-5.0mm), 150 grams of catalyst is packed into a fixed-bed reactor, and reduced at 280°C for 6h (1.0MPa, 500h -1 ), to obtain a supported catalyst 5%Cu-1%Au-0.1%In / ZrO 2 .

[0028] The purity of the product obtained by rectification in the rectification tower is ≧99.5%.

Embodiment 3

[0030] Weigh a certain amount of tetrabutyl titanate, dissolve it in a small amount of ethanol, and then dissolve it in a certain amount of water. Weigh a certain amount of rhodium chloride, ruthenium chloride and manganese nitrate aqueous solution to prepare a nitrate solution. Add the nitrate solution into the tetrabutyl titanate solution, stir at 80°C, and add hydrochloric acid dropwise. After the sol was formed, it was aged at room temperature for 24 h. The gel was formed at 80°C, dried at 120°C for 12 hours, and baked at 450°C for 3 hours. The catalyst is shaped into a clover shape (diameter 3.0mm, length 3.0-5.0mm), 75 grams of catalyst is packed into a fixed bed reactor, and reduced at 250°C for 6h (2.5MPa, 3000h -1 ), to obtain a supported catalyst 0.1%Rh-2%Ru-4%Mn / TiO 2 .

[0031] The purity of the product obtained by rectification in the rectification tower is ≧99.3%.

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Abstract

The present invention relates to a method for preparing unsaturated alcohol through selective hydrogenation of alpha,beta-unsaturated aldehyde. A purpose of the present invention is to solve the problems of low production capacity, low raw material conversion rate, low product selectivity and different separation between the catalyst and the product in the prior art. The technical scheme of the present invention comprises that the method for preparing the unsaturated alcohol through the selective hydrogenation of the alpha,beta-unsaturated aldehyde is used, the alpha,beta-unsaturated aldehyde and hydrogen are continuously introduced into a fixed bed reactor, and are subjected to a continuous selective catalytic hydrogenation reaction on a catalyst under a selective reaction condition, the generated product is subjected to gas-liquid separation and rectification to obtain an unsaturated alcohol product and unreacted methacrolein, and the hydrogen obtained through the gas-liquid separation and the unreacted alpha,beta-unsaturated aldehyde obtained after the rectification are recycled. With the technical scheme of the present invention, the problems in the prior art are well solved. The method of the present invention can be used for the preparation of the unsaturated alcohol through the selective hydrogenation of alpha,beta-unsaturated aldehyde.

Description

technical field [0001] The invention relates to a method for selectively hydrogenating α and β unsaturated aldehydes to prepare unsaturated alcohols. Background technique [0002] The selective hydrogenation of α and β unsaturated aldehydes to produce unsaturated alcohols is an important reaction in chemical and chemical production, because the bond energy of C=O is 100kJ.mol larger than that of C=C -1 , it is more difficult to selectively hydrogenate C=O double bonds than C=C double bonds. Therefore, the development of C=O bond selective hydrogenation catalysts with high selectivity and high stability is the key. [0003] Unsaturated alcohols are important raw materials and intermediates for medicines, spices, pesticides, resins, etc. Usually unsaturated alcohols are prepared by direct reduction of unsaturated aldehydes such as tetrahydrolithium aluminum, sodium borohydride, aluminum isopropoxide, etc. This reaction needs to use a large amount of solvent, and it is diffi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B31/00B01J23/89B01J23/656B01J23/66B01J29/46B01J29/14C07C29/141C07C33/03C07C33/035C07C33/32
CPCB01J23/002B01J23/6562B01J23/66B01J23/8913B01J23/8946B01J23/8953B01J23/896B01J23/8966B01J29/146B01J29/46B01J2229/18B01J2523/00C07B31/00C07C29/141C07C33/03C07C33/035C07C33/32B01J2523/822B01J2523/17B01J2523/824B01J2523/3706B01J2523/22B01J2523/19B01J2523/33B01J2523/48B01J2523/821B01J2523/72B01J2523/47B01J2523/18B01J2523/827B01J2523/23B01J2523/41B01J2523/828B01J2523/842B01J2523/43B01J2523/31B01J2523/27B01J2523/845
Inventor 李永刚芮果宁春利廖湘洲孙思杰张春雷
Owner SHANGHAI HUAYI GRP CO
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