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Preparation method of core-shell catalyst for catalyzing hydrodeoxygenation of guaiacol to prepare cyclohexanol

A catalyst, core-shell type technology, applied in the field of preparation of core-shell type catalysts, can solve the problem of low conversion rate of guaiacol and cyclohexanol selectivity, and achieve low cost, good catalytic activity, and good stability

Active Publication Date: 2020-11-27
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN107649169A uses molecular sieves to support any two or three active components in Ni, Co, Cu, Mg, Al, Fe to prepare cyclohexanol by catalyzing the hydrodeoxygenation of guaiacol, and the reaction takes place under high pressure ( 3 ~ 6MPa), long reaction time (6 ~ 10h) conditions, and guaiacol conversion rate cyclohexanol selectivity is low

Method used

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  • Preparation method of core-shell catalyst for catalyzing hydrodeoxygenation of guaiacol to prepare cyclohexanol
  • Preparation method of core-shell catalyst for catalyzing hydrodeoxygenation of guaiacol to prepare cyclohexanol
  • Preparation method of core-shell catalyst for catalyzing hydrodeoxygenation of guaiacol to prepare cyclohexanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of a core-shell catalyst, comprising the following steps:

[0028] (1) Two 20 mL, 0.1 mol / L cetyltrimethylammonium bromide (CTAB) aqueous solutions were prepared respectively. Among them, one part contains 6g hydrazine hydrate, so that one part contains 0.54g Co(NO 3 ) 2 ·6H 2 O and 1.8mL of 1mol / L NaOH;

[0029] (2) Mix the two prepared CTAB solutions and seal at 80°C for 2 hours;

[0030] (3) The product obtained in step (2) was taken out, washed alternately with ethanol and deionized water for 2 to 3 times, and vacuum-dried overnight at 50° C. to obtain 0.11 g of Co nanoparticles;

[0031] (4) Co nanoparticles were prepared several times, and 0.31g Co nanoparticles were dispersed in a mixed solution of 80mL deionized water and 20mL ethanol;

[0032] (5) 1.724g Ce(CH 3 COO) 3 , 8.83g Na 2 SiO 3 9H 2 O was dissolved in 50mL deionized water, and 6.5g (NH 4 ) 2 CO 3 Dissolve in 50mL of deionized water, and add the two together into the s...

Embodiment 2

[0037] (1)-(3) are the same as embodiment 1;

[0038] (4) Prepare Co nanoparticles repeatedly, get 0.187g Co, all the other are with embodiment 1 (4);

[0039] (5) 1.32g TiCl 4 , 5.30g Na 2 SiO 3 9H 2 O dissolved in 50mL deionized water, take 5g Na 2 CO 3 Dissolve in 50mL of deionized water, and add the two together into the suspension in step (4) under the condition of mechanical stirring at 80°C, and keep for 0.5h;

[0040] (6) Take out the precipitate obtained in step (5), filter and wash it to neutrality, place it in n-butanol at 50°C and evaporate it to dryness, then place it in an oven at 100°C for 12h, and put the catalyst in a hydrogen flow before using After reduction at 400℃ for 3h, the obtained Co@TiO 2 -SiO 2 Core-shell catalyst, active component Co mass fraction is 10%, m TiO2 :m SiO2 =1:2.

[0041] Core-shell catalyst applications are as follows:

[0042] In a fixed bed tubular reactor, add 0.2g Co@TiO 2 -SiO 2 (1:2) catalyst, the reaction temperature...

Embodiment 3

[0044] (1)-(3) are the same as embodiment 1;

[0045] (4) Prepare Co nanoparticles repeatedly, get 0.125g Co, all the other are with embodiment (1);

[0046] (5) 2.72g Al(NO 3 ) 3 9H 2 O, 3.5g Na 2 SiO 3 9H 2 O dissolved in 50mL deionized water, take 5gNa 2 CO 3 Dissolve in 50mL of deionized water, and add the two together into the suspension in step (4) under the condition of mechanical stirring at 60°C, and keep for 0.5h;

[0047] (6) Take out the precipitate obtained in step (5), filter and wash it to neutrality, place it in n-butanol at 50°C and evaporate it to dryness, then place it in an oven at 100°C for 12h. After reduction at 400℃ for 3h, the obtained Co@Al 2 o 3 -SiO 2 Core-shell catalyst, active component Co mass fraction is 10%, mAl2O3:mSiO2=1:2.

[0048] Applications of core-shell catalysts are as follows:

[0049] In a fixed bed tubular reactor, add 0.2g Co@Al 2 o 3 -SiO 2 (1:2) catalyst, the reaction temperature is 220°C, the reaction pressure is...

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Abstract

The invention belongs to the field of preparation of catalysts, and particularly relates to a preparation method of a core-shell catalyst for catalyzing hydrodeoxygenation of guaiacol to prepare cyclohexanol. The preparation method comprises the following steps: firstly, preparing cobalt nanoparticles by utilizing a solvent reduction method, and then preparing the Co-coated MxOy-SiO2 core-shell type catalyst taking Co as a core and taking MxOy-SiO2 as a shell by utilizing a post-synthesis method, wherein M = Ce, Ti and Al. The catalyst is simple in preparation process and low in cost, the reaction is carried out at low pressure and low temperature, and energy consumption is low. Besides, the prepared core-shell type catalyst shows good reaction activity in guaiacol hydrodeoxygenation reaction, is good in stability, can be roasted and recycled after reaction, and has good economic benefits.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a preparation method of a core-shell catalyst used to catalyze the hydrodeoxygenation of guaiacol to prepare cyclohexanol. Background technique [0002] As an important chemical raw material, cyclohexanol has been widely used in many industrial production fields. It can be used to produce adipic acid, hexamethylenediamine, caprolactam, etc., and can also be used as a raw material for fuel production. Cyclohexane prepared by hydrodehydration is one of the main components of gasoline. In addition, cyclohexanol can also be used in solvents, coatings, medicines, plasticizers, etc. At present, the industrial production of cyclohexanol is mainly realized through the oxidation of cyclohexane and the hydrogenation of phenol, which is inconsistent with the sustainable development strategy and increases the consumption of fossil energy. [0003] Guaiacol accounts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J23/83B01J35/10C07C29/20C07C35/08
CPCB01J23/002B01J23/83B01J23/75C07C29/20C07C2601/14B01J35/396B01J35/61C07C35/08
Inventor 鲁墨弘赵梦阳胡双进陈晨李明时张伟
Owner CHANGZHOU UNIV
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