Magnesium-aluminum-zirconium solid catalyst for embedded synthesis of alkoxy alcohol ether ester in one step

A technology for synthesizing alkoxy alcohol ethers and solid catalysts, applied in physical/chemical process catalysts, preparation of organic compounds, organic chemistry, etc., can solve problems such as poor product performance, high energy consumption, high material consumption, and long process flow. Achieve the effects of easy separation, high selectivity, and easy separation and recovery

Active Publication Date: 2014-07-16
JIANGSU YIDA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the process of synthesizing alkoxy alcohol ether ester compounds includes two steps. First, alcohol and alkylene oxide react to form alcohol ether compounds. After the product is purified, it is reacted with carboxylic acid compounds to obtain the required alcohol ether ester. The process flow Long, high energy consumption and material consumption, complex product separation and treatment in the production process, poor product performance, and high product cost

Method used

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  • Magnesium-aluminum-zirconium solid catalyst for embedded synthesis of alkoxy alcohol ether ester in one step
  • Magnesium-aluminum-zirconium solid catalyst for embedded synthesis of alkoxy alcohol ether ester in one step

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a three-necked flask equipped with a stirrer, a reflux condenser was installed. Dissolve 9.3g of magnesium chloride hexahydrate, 10.8g of aluminum nitrate nonahydrate, and 1.2g of zirconium nitrate pentahydrate with 41.2g of deionized water, and add them to a three-necked flask. Dissolve 3.2g of potassium hydroxide, 7.8g of Dissolve potassium carbonate, quickly add potassium hydroxide and potassium carbonate solution into the three-necked flask, and stir vigorously. After reacting for half an hour, crystallize at 70°C for 6 hours, then suction filter to obtain a solid precipitate, and wash with deionized water 4 times, each water consumption is 100mL, placed in a constant temperature drying oven at 100 ℃ and dried until constant weight. The dried solid was ground and calcined in a muffle furnace at 500° C. for 5 h to obtain a magnesium-aluminum-based composite metal oxide solid catalyst.

[0018] This catalyst is used to catalyze the ethoxylation reaction of ethyl a...

Embodiment 2

[0020] The basic preparation method is the same as in Example 1, except that the salt solution added to the three-necked flask has only magnesium chloride and aluminum nitrate.

[0021] This catalyst is used to catalyze the ethoxylation reaction of ethyl acetate with raw material ratio EA:EO=3:1, the conversion rate of ethylene oxide is 50.92%, the yield rate of CAC is 23.12%, and the yield rate of DCAC is 14.70%. .

Embodiment 3

[0023] The basic preparation method is the same as in Example 1, except that the mixed salt solution added to the three-necked flask is magnesium chloride, aluminum nitrate and zinc nitrate.

[0024] This catalyst is used to catalyze the ethoxylation reaction of ethyl acetate with a molar ratio of raw materials EA:EO=2:1, the conversion rate of ethylene oxide is 39.36%, the yield rate of CAC is 18.64%, and the yield rate of DCAC is 11.33% %.

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Abstract

The invention relates to a magnesium-aluminum-zirconium solid complex metal oxide catalyst, which can be used for obtaining alkoxy alcohol ether ester by catalyzing one-step embedding reactive synthesis of epoxy ethane (propane) and carboxylic ester to carry out. The catalyst is characterized in that soluble magnesium salt, aluminium salt and zircon salt can be prepared into a solution with certain concentration through deionized water, a certain amount of precipitator is dissolved by deionized water and mixed with the prepared magnesium-aluminum-zirconium solution, under vigorous stirring condition, crystallization is performed for a certain period of time at the temperature of 40-100 DEG C, then precipitate is filtered out, soluble salt attached to the precipitate is washed by deionized water, drying is performed until constant weight is realized, and then the product is roasted in a muffle furnace so that the magnesium-aluminum-zirconium solid complex metal oxide catalyst is prepared. The magnesium-aluminum-zirconium solid complex metal oxide catalyst has the advantages of double acid-base active sites, easiness in separation, environmental protection, high efficiency and the like; the catalyst can catalyze one-step reactive synthesis carboxylic ester and alkyleneoxide, is high in catalyst activity and selectivity, and is easily recyclable and reused.

Description

technical field [0001] The invention relates to a catalyst for catalyzing the one-step synthesis of alcohol ether esters, in particular to a magnesium-aluminum-zirconium composite oxide solid catalyst with acid-base dual active sites, which is used to catalyze the ring-opening and intercalation of ethylene oxide into ethyl acetate In the ester bond of the ester, one-step reaction synthesizes ethylene glycol ethyl ether acetate. The invention belongs to the technical fields of catalyst preparation and fine chemicals. Background technique [0002] Amphiphilic chemicals produced with ethylene oxide and propylene oxide as basic raw materials have become an important part of the development of high value-added downstream products of alkylene oxide. Alkoxylation is the key to the production of polyoxyalkylene fine chemicals. An important method, wherein glycol ether and glycol ether ester compounds are one of the important derivatives of epoxy compounds. [0003] At present, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10C07C67/29C07C69/16
Inventor 刘准朱煜郭登峰赵会晶曹惠庆张静
Owner JIANGSU YIDA CHEM
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