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A kind of preparation method and application of composite catalyst

A composite catalyst and catalyst technology, applied in the field of catalytic chemistry, can solve problems such as the conversion rate of raw materials that are not mentioned, and achieve the effects of mild preparation conditions, simple steps and good stability

Active Publication Date: 2016-04-06
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In recent years, Huang He, Zhang Jian'an and others have respectively patented (Huang He. A method for preparing methyl ethyl ketone: China, CN101293817) (Zhang Jian'an. A method for efficiently dehydrating methyl ethyl ketone from 2,3-butanediol: China, CN101580462) uses a molecular sieve solid catalyst and a molecular sieve solid acid catalyst to catalyze 2,3-butanediol to prepare methyl ethyl ketone, the conversion rate of 2,3-butanediol can reach 90-100%, and the selectivity of methyl ethyl ketone can reach 81-91%. However, sulfuric acid, a strong corrosive substance, was cited in the modification step. In addition, Alisha Multer et al. used HZSM-5 without any treatment to catalyze the dehydration of 2,3-butanediol, a homemade biomass fermentation product, to prepare methyl ethyl ketone. The selectivity of methyl ethyl ketone can be greatly improved. 90%, but the conversion rate of raw materials is not mentioned in the literature (MulterA, McGrawN, HohnK, etal. Productionofmethylethylketonefrombiomassusingahybridbiochemical / catalyticapproach.Industrial&EngineeringChemistryResearch, 2012,52(1):56-60.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 10g of HZSM-5 with a silicon-aluminum ratio of 25 and impregnate it in CuSO 4 solution, where CuSO 4 The mass percentage of HZSM-5 was 6%. After being treated at room temperature, it was dried at 60°C, and the dried catalyst was calcined at 540°C for 3h in a muffle furnace. The calcined catalyst was impregnated with Fe(NO 3 ) 3 solution, treated at room temperature, where Fe(NO 3 ) 3 The mass percentage with HZSM-5 is 1%. Then dry it in an oven at 60°C, and roast the dried catalyst in a muffle furnace at 540°C for 3 hours to obtain Fe 2 o 3 and CuSO 4 Loaded Fe 2 o 3 -CuSO 4 -HZSM-5 composite catalyst.

[0020] Take 1g of the above-mentioned catalyst in a stainless steel fixed-bed reactor (Φ10mm×8mm×360mm), fill the upper and lower sides of the catalyst with small ceramic balls, and put it under 4ml / min N 2 Under protection, the temperature rises to 250 ° C, and the 2,3-butanediol raw material liquid obtained by the fermentation of biomass is injected i...

Embodiment 2

[0022] Take 10g of HZSM-5 with a silicon-aluminum ratio of 38 and impregnate it in CuSO 4 solution, where CuSO 4 The mass percentage of HZSM-5 was 8%. After being treated at room temperature, it was dried at 60°C, and the dried catalyst was calcined at 540°C for 3h in a muffle furnace. The calcined catalyst was impregnated with Fe(NO 3 ) 3 solution, treated at room temperature, where Fe(NO 3 ) 3 The mass percentage with HZSM-5 is 2%. Then dry it in an oven at 60°C, and roast the dried catalyst in a muffle furnace at 550°C for 3 hours to obtain Fe 2 o 3 and CuSO 4 Loaded Fe 2 o 3 -CuSO 4 -HZSM-5 composite catalyst.

[0023] Take 1g of the above-mentioned catalyst in a stainless steel fixed-bed reactor (Φ10mm×8mm×360mm), fill the upper and lower sides of the catalyst with small ceramic balls, and put it under 4ml / min N 2 Under protection, the temperature rises to 250°C, and a medium-pressure plunger pump is used to inject 30wt% of the 2,3-butanediol raw material solu...

Embodiment 3

[0025] Take 10g of HZSM-5 with a silicon-aluminum ratio of 25 and impregnate it in CuSO 4 solution, where CuSO 4 The mass percentage of HZSM-5 was 6%. After being treated at room temperature, it was dried at 60°C, and the dried catalyst was calcined at 540°C for 3h in a muffle furnace. The calcined catalyst was impregnated with Fe(NO 3 ) 3 solution, treated at room temperature, where Fe(NO 3 ) 3 The mass percentage with HZSM-5 is 4%. Then dry it in an oven at 60°C, and roast the dried catalyst in a muffle furnace at 540°C for 3 hours to obtain Fe 2 o 3 and CuSO 4 Loaded Fe 2 o 3 -CuSO 4 -HZSM-5 composite catalyst.

[0026] Take 1g of the above-mentioned catalyst in a stainless steel fixed-bed reactor (Φ10mm×8mm×360mm), and fill the upper and lower sides of the catalyst with small ceramic balls. 2 Under protection, the temperature rises to 275 °C, and the 2,3-butanediol raw material liquid obtained by the fermentation of biomass is injected into the 50wt% biomass by...

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PUM

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Abstract

The invention discloses a preparation method and application of a composite catalyst, and belongs to the technical field of catalytic chemistry. The method comprises the following steps of performing incipient impregnation on a molecular sieve matrix in a CuSO4 solution, performing incipient impregnation in a Fe(NO3)3 solution, and performing drying and calcination to obtain a Fe2O3-CuSO4-HZSM-5 composite catalyst. When the composite catalyst is used for catalytically dehydrating 2,3-butanediol obtained by biomass fermentation to prepare methyl ethyl ketone, the conversion rate of the 2,3-butanediol is close to 100 percent, the selectivity of the methyl ethyl ketone can reach 70.1 to 89.9 percent, long-term stable operation can be ensured, and high activity and selectivity can be maintained after the catalyst runs for 240 hours. According to the composite catalyst, preparation conditions are mild and simple; the composite catalyst is high and stable in catalytic activity, environment-friendly and consistent with the concept of green chemistry; the conversion rate of the 2,3-butanediol and the selectivity of the methyl ethyl ketone are high.

Description

technical field [0001] The invention relates to the technical field of catalytic chemistry, and mainly relates to a preparation method and application of a composite catalyst. Background technique [0002] Methyl ethyl ketone, commonly known as methyl ethyl ketone (MEK), is a good organic solvent with moderate boiling point, outstanding solvency, good stability, fast volatilization rate, low viscosity and low toxicity. As a very important industrial solvent, methyl ethyl ketone can be used as an organic solvent for nitrocellulose, vinyl resin, polyurethane, phenolic resin, alkyd resin, ink, coating, adhesive, pharmaceutical production, and dewaxing of lubricating oil. . In addition, the α-methyl active hydrogen and carbonyl contained in methyl ethyl ketone can undergo various chemical reactions, so methyl ethyl ketone is also an organic synthesis intermediate and fine chemical raw material, and can be used as an anti-peeling agent and antioxidant for paints and fragrances. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46C07C49/10C07C45/52
Inventor 张雄福王爽刘海鸥戴建英修志龙
Owner DALIAN UNIV OF TECH