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Method and device for preparing ethylene glycol antimony through microwave reaction

A technology of ethylene glycol antimony and microwave reaction, which is applied to the preparation of metal alcohols, chemical instruments and methods, chemical/physical/physicochemical processes using energy, etc., can solve the problems of long time and high energy consumption, and achieve short reaction time , low energy consumption, increase the effect of full contact

Active Publication Date: 2016-07-06
锡矿山闪星锑业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a method and device for preparing ethylene glycol antimony by microwave reaction with low energy consumption and short reaction time in view of the defects of long time and high energy consumption in the existing ethylene glycol antimony synthesis

Method used

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  • Method and device for preparing ethylene glycol antimony through microwave reaction
  • Method and device for preparing ethylene glycol antimony through microwave reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The microwave reaction of the present embodiment prepares the method for ethylene glycol antimony, comprises the following steps:

[0053] In a 0.5L microwave reactor equipped with a microwave heating device, a condensing reflux device, and a stirrer, add 300 mL of ethylene glycol and 150 g of antimony trioxide at a liquid-solid ratio of ethylene glycol to antimony trioxide of 2:1, Start the microwave heating device, the microwave frequency is 2450MHz, the stirring speed is controlled at 30 rpm, the reaction temperature is controlled at 140-145°C, and the temperature of the outlet gas of the condensation reflux device is controlled at 90-100°C; when the mixture in the reactor reaches the controlled temperature, During heat preservation reaction 15 minutes, at this moment, reaction material is clear and transparent, adds activated carbon 1.2g, then heat preservation and stirring 10 minutes, filter and obtain clear filtrate; Filtrate enters crystallization tank, carries ou...

Embodiment 2

[0064] In a 10L microwave reactor equipped with a microwave heating device, a condensing reflux device, and a stirrer, according to the liquid-solid ratio of ethylene glycol and antimony trioxide 3:1, add 7500 mL of ethylene glycol and 2500 g of antimony trioxide respectively, and start Microwave heating device, the microwave frequency is 2450MHz, the stirring speed is controlled at 50 rpm, the reaction temperature is controlled at 155-160°C, and the temperature of the outlet gas of the condensation reflux device is controlled at 100-110°C; when the mixture in the reactor reaches the controlled temperature, keep warm When reacting for 25 minutes, at this time, the reaction material was clear and transparent, and 12.5 g of activated carbon was added, and then it was incubated and stirred for 10 minutes, and filtered to obtain a clear filtrate; Vacuum drying to obtain ethylene glycol antimony product 3531.0g, its quality index is: whiteness 93.6%, Sb56.78%, As0.0015%, Pb0.0006%, ...

Embodiment 3

[0067] In a 10L microwave reactor equipped with a microwave heating device, a condensing reflux device, and a stirrer, according to the liquid-solid ratio of ethylene glycol and antimony trioxide at 4:1, add 7200 mL of ethylene glycol and 1800 g of antimony trioxide respectively, and start Microwave heating device with a microwave frequency of 2450MHz; control the stirring speed to 70 rpm, control the reaction temperature to 170-175°C, and control the outlet gas temperature of the condensation reflux device to 110-120°C; when the mixture in the reactor reaches the controlled temperature, keep warm When reacting for 40 minutes, at this moment, the reaction material was clear and transparent, and 12.6 g of activated carbon was added, and then it was incubated and stirred for 10 minutes, and filtered to obtain a clear filtrate; Vacuum drying to obtain 2514.8g of ethylene glycol antimony product, its quality index is: whiteness 93.7%, Sb57.12%, As0.0013%, Pb0.0007%, Cu0.0004%, Fe0....

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Abstract

Provided are a method and device for preparing ethylene glycol antimony through a microwave reaction. The method comprises the following steps of 1, reaction synthesis, wherein the raw materials of antimonous oxide and ethylene glycol are put into a microwave reaction kettle provided with a microwave heating device, a reflux condensation device and a stirrer according to the solid-to-liquid ratio of 1:(2-10), the microwave heating device is started, the reaction temperature and reaction time are controlled, and the temperature of gas at the outlet of the reflux condensation device is controlled; 2, purification and decoloration; 3, cooling crystallization, 4 drying, wherein an ethylene glycol antimony product is obtained; 5, mother liquid distillation, wherein obtained ethylene glycol mother liquid is added into a microwave distillation kettle provided with a microwave heating device, the temperature of a distillation outlet is controlled, ethylene glycol is distilled out and returns back for use, and distillation residues are recycled. The invention further discloses the device for preparing ethylene glycol antimony through the microwave reaction. The method for preparing ethylene glycol antimony through the microwave reaction has the advantages that the heating speed is high, the reaction time is short, the conversion ratio is high, the direct yield of final products is high, the productivity is high, the cost is low and the like.

Description

technical field [0001] The invention relates to a preparation method and device of ethylene glycol antimony, in particular to a method and device for preparing ethylene glycol antimony by microwave reaction. Background technique [0002] Ethylene glycol antimony, the chemical formula is Sb 2 (OCH 2 CH 2 o) 3 , with a relative molecular weight of 423.66 and a theoretical antimony content of 57.5%, is a new type of catalyst in the polycondensation process of polyethylene terephthalate (PET). Due to the excellent catalytic effect, antimony ethylene glycol has become an upgraded product of antimony trioxide and antimony acetate in the antimony-based catalysts in the polyester catalytic process. [0003] In the production process of ethylene glycol antimony, the reaction of ethylene glycol and antimony trioxide to synthesize ethylene glycol antimony is the key process in the whole process. The speed of the synthesis reaction process directly affects the speed of the entire p...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/70B01J19/12
CPCB01J19/126B01J2219/1206C07C29/70C07C31/202
Inventor 金承永单桃云廖光荣金涛刘鹊鸣邓卫华
Owner 锡矿山闪星锑业有限责任公司
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