Method for combining ethylene glycol monoethyl ether with ternary composite metal oxide as catalyst

A ethylene glycol monoethyl ether and ternary compound technology, which is applied in the preparation of ethers and ethers from alkylene oxides, can solve the problems of limited reserves and high prices of rare earth ions, and achieves low by-products, high selectivity and low cost. Effect

Inactive Publication Date: 2012-09-19
LIAONING OXIRANCHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, considering the high price and limited reserves of rare earth ions, we use a low-cost ternary M

Method used

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  • Method for combining ethylene glycol monoethyl ether with ternary composite metal oxide as catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Using co-precipitation method, 18.49g Mg(NO 3 ) 2 ·6H 2 O, 9.02g Al(NO 3 ) 3 9H 2 O, 1.9523gFe(NO 3 ) 3 9H 2 O was dissolved in 100mL deionized water, so that Fe in the solution 3+ / Al 3+ 0.2, stir to dissolve it for later use; configure 2.0mol L -1 100mL of NaOH solution; take a 500mL beaker, configure 100mL 0.5mol L -1 Na 2 CO 3The solution was placed in a water bath at 60°C, and the above-mentioned mixed nitrate solution and NaOH solution were slowly dropped into it under stirring, and the pH of the mixed solution was made to be 10 by controlling the dropping speed of the two. Continue stirring after the dropwise addition, crystallize at 60°C for 6h, filter and wash until neutral, and dry the obtained white solid in an oven at 120°C for 10h to obtain Mg-Al-Fe ternary hydrotalcite. After the above-mentioned Mg-Al-Fe hydrotalcite was calcined at 500°C in air for 8 hours, the obtained block was crushed to 20-40 mesh to obtain the required catalyst, which wa...

Embodiment 2

[0024] Using the catalyst MAF-1 prepared in Example 1, both ends of a 50 cm long reaction tube were filled with quartz sand, the middle of the tube was filled with 2.15 g of MAF-1, and placed in a fixed-bed reaction device. N 2 Purge the reaction tube for 10 minutes, set the pressure to 0.4MPa, and heat the reaction tube to 120°C at the same time. The reaction raw materials ethanol and ethylene oxide were respectively pumped with a flow pump at 6.0mL·h -1 and 2.1mL·h -1 The flow rate is injected into the reactor, and the product enters the receiving tank at the bottom of the device after the first-stage condensation and the second-stage condensation, and the ethylene glycol monoethyl ether product can be obtained.

Embodiment 3

[0026] Using co-precipitation method, 18.49g Mg(NO 3 ) 2 ·6H 2 O, 9.02g Al(NO 3 ) 3 9H 2 O, 9.7615gFe(NO 3 ) 3 9H 2 O was dissolved in 100mL deionized water, so that Fe in the solution 3+ / Al 3+ 1.0, stir to dissolve it for later use; configure 2.0mol L -1 100mL of NaOH solution; take a 500mL beaker, configure 100mL 0.5mol L -1 Na 2 CO 3 The solution was placed in a water bath at 60°C, and the above-mentioned mixed nitrate solution and NaOH solution were slowly dropped into it under stirring, and the pH of the mixed solution was made to be 10 by controlling the dropping speed of the two. Continue stirring after the dropwise addition, crystallize at 60°C for 6h, filter and wash until neutral, and dry the obtained white solid in an oven at 120°C for 10h to obtain Mg-Al-Fe ternary hydrotalcite. After the above-mentioned Mg-Al-Fe hydrotalcite was calcined at 500°C in air for 8 hours, the obtained block was crushed to 20-40 meshes to obtain the required catalyst, which...

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Abstract

A method for combining ethylene glycol monoethyl ether in a fixed bed reactor with ethanol and ethylene oxide as raw materials and ternary composite metal oxide as a catalyst is disclosed. The catalyst is prepared by roasting a Mg-Al-Fe type ternary hydrotalcite precursor. The composition of the precursor is (MgO)15(Al2O3)2.5(Fe2O3)x, wherein the x in the formula is 0.25-2.5. By means of the method, ethylene oxide conversion rate can reach 92.97%, and ethylene glycol monoethyl ether selectivity can reach 86.75%. Simultaneously the method resolves the problem in the prior art that a product is wide in molecular weight distribution and the catalyst and the product are difficult to separate, and greatly improves product quality and production efficiency.

Description

technical field [0001] The present invention relates to a kind of method of synthesizing ethylene glycol monoethyl ether, more specifically, the present invention relates to the method for synthesizing ethylene glycol monoethyl ether product on fixed-bed reactor with ternary composite metal oxide as catalyst. Background technique [0002] Ethylene glycol monoethyl ether produced by the reaction of ethylene oxide (EO) and absolute ethanol is a general-purpose solvent with excellent performance, with low freezing point, good mutual solubility and permeability, strong diffusion force, excellent solubility and dilution It is widely used in coatings, inks, adhesives, printing and dyeing, spices, medicine, cleaning and hydraulic transmission, etc. In addition, as an intermediate of ethylene glycol ether acetate, the market demand is also increasing with ethylene glycol The growth of alcohol ether acetate is increasing year by year. Catalysts used in the synthesis of alcohol ether...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/03B01J23/745
Inventor 纪敏朱建民刘兆滨张亚丽董振鹏周立明
Owner LIAONING OXIRANCHEM INC
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