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Preparation method of composite metal oxide and synthesis method of alcohol ether carboxylate

A technology of alcohol ether carboxylate and composite metal, which is applied in the preparation of composite metal oxide and the field of composite metal oxide catalyzed synthesis of alcohol ether carboxylate, can solve the problem of product limitation and the like, so as to improve the reaction activity and catalytic activity Enhanced, reduced aggregation time effect

Active Publication Date: 2015-06-17
武汉奥克化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The research group of Professor Fang Yun of Jiangnan University [Shen Yongan, Fang Yun, Wang Yiyou et al. 2005, 22(9): 712-714; X.M.Xia, Y.A.Shen, S.R.Ji, et al.J.Chem.Technol.Biotechnol.2007 ,82:47–50.], using self-made hydrotalcite catalysts to synthesize ethylene glycol ethyl ether acetate, but the synthesized products are limited to oligomeric alcohol ether carboxylates

Method used

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  • Preparation method of composite metal oxide and synthesis method of alcohol ether carboxylate
  • Preparation method of composite metal oxide and synthesis method of alcohol ether carboxylate
  • Preparation method of composite metal oxide and synthesis method of alcohol ether carboxylate

Examples

Experimental program
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Effect test

Embodiment 1

[0041] 1. Catalyst Preparation

[0042] Weigh 192 grams of Mg(NO 3 ) 2 ·6H 2 O crystals and 141 g of Al(NO 3 ) 3 9H 2 O crystals were dissolved in 1 liter of deionized water to form Al(NO 3 ) 3 and Mg(NO 3 ) 2 mixed solution. Put 0.9mol / L Na 2 CO 3 300ml of the solution was added to the above mixed solution. Add 2.25mol / L NaOH solution dropwise into the mixed solution to adjust the pH value of the solution to 10±0.5. Continue to stir the mixed solution at room temperature for about 5-6 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight. For the XRD spectrum of the sample, see figure 1 Figure A.

[0043] Take 10 grams of the dried sample, add it to 400 mL of 0.0025 g / mL lauric acid in isopropanol solution, boil and reflux for about 2 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight. The XRD spectrum pattern of the compound obtained, see figure 1 Figure B. Finally, it was calcined a...

Embodiment 2

[0051] 1. Preparation of composite metal oxide catalysts

[0052] Weigh 192 grams of Mg(NO 3 ) 2 ·6H 2 O crystals, and 47 grams of Al(NO 3 ) 3 9H 2 O crystals were dissolved in 1 liter of deionized water to form Al(NO 3 ) 3 and Mg(NO 3 ) 2 mixed solution. Put 0.9mol / LNa 2 CO 3 Add 300mL of the solution into the above mixed solution, and then add 2.25mol / L NaOH solution dropwise into the mixed solution to adjust the pH value of the solution to 10±0.5. Continue to stir the mixed solution at room temperature for about 5-6 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight.

[0053] Take 10 grams of the dried sample, add it to 500 mL of 0.002 g / mL stearic acid in isopropanol solution, boil and reflux for about 4 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight . Finally, it was calcined at 250° C. for 5 hours in a muffle furnace to obtain the final composite metal oxide catalyst.

[0054...

Embodiment 3

[0061] 1. Catalyst preparation

[0062] Weigh 77g Mg(NO 3 ) 2 ·6H 2 O crystals, 19g Al(NO 3 ) 3 9H 2 O crystals and 41 g FeCl 3 ·6H 2 O was dissolved in 1 liter of deionized water to form Al(NO 3 ) 3 , Mg(NO 3 ) 2 and FeCl 3 mixed solution. Put 0.9mol / L Na 2 CO 3300ml of the solution was added to the above mixed solution. Add 2.25mol / L NaOH solution dropwise into the mixed solution to adjust the pH value of the solution to 10±0.5. Continue to stir the mixed solution at room temperature for about 5-6 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight.

[0063] Take 10 grams of the dried sample, add it to 400 mL of 0.0025 g / mL lauric acid in isopropanol solution, boil and reflux for about 2 hours, then filter with suction, wash until neutral, and dry in an oven at 80°C overnight. Finally, it was calcined at 300° C. for 5 hours in a muffle furnace to obtain the final composite metal oxide catalyst.

[0064] 2. Preparation o...

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Abstract

The invention relates to a preparation method of a composite metal oxide. The preparation method comprises the following steps of 1, composite metal hydroxide preparation, 2, reaction of the composite metal hydroxide and fatty acid, and 3, roasting of the treated compound at a temperature of 300 DEG C or less. The invention also relates to a catalytic synthesis method of alcohol ether carboxylate. The catalytic synthesis method utilizes the composite metal oxide as a catalyst. The preparation method of the composite metal oxide utilizes fatty acid to realize modification and utilizes a roasting temperature far below the existing technology roasting temperature. The composite metal oxide has obviously strong activity in catalytic oxyalkylation, is suitable for alcohol ether carboxylate synthesis, and has wide and easily controlled product polymerization degree distribution. The synthesis method increases alcohol ether carboxylate product types and simplifies a preparation technology.

Description

technical field [0001] The invention relates to the field of inorganic metal oxide catalysts, in particular to a method for preparing a composite metal oxide and a method for catalyzing the synthesis of alcohol ether carboxylates by the composite metal oxide prepared by the preparation method. Background technique [0002] The scale development of my country's alcohol ethers first began in the mid-1990s, when the production of glycol ethers was the main focus. It can cause blood lesions and fetal malformations. Foreign developed countries and regions began to restrict its production and use, and replaced them with propylene glycol ethers or ester ethers. With the technical support of Dow Chemical in the United States and some domestic scientific research institutions, domestic enterprises began to produce propylene glycol ether and alcohol ether carboxylate solvents with low toxicity and similar physical and chemical properties to glycol ethers [Feng Zhaolin. Modern Chemicals...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J23/745C07C67/26C07C69/16C08G65/26
Inventor 朱建民刘兆滨董振鹏周立明张金昌孟岩
Owner 武汉奥克化学有限公司
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