Non-drying preparation technology of ethylene glycol antimony

A technology of ethylene glycol antimony and preparation process, which is applied in the directions of metal alcohol preparation, organic chemistry, etc., can solve the problems of increasing production cost and safety cost, increasing consumption of antimony trioxide, affecting the catalytic effect of ethylene glycol antimony, and the like, Achieve the effect of eliminating unsafe factors, eliminating drying process and improving production environment

Inactive Publication Date: 2011-10-26
安化县文威化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of antimony trioxide in the product is 57.28~57.89%. The above prior art has a drying process without exception, and part of the Sb will be made during the drying process. 2 (OCH 2 CH 2 O) 3 The chelating structure of the product is destroyed and reduced to antimony trioxide, so that the content of antimony trioxide in the product exceeds the theoretical value (57.47%), the prior art 1 reaches 57.6%, and the prior art 2 reaches 57.52% %, prior art 3 has reached 58.5%, and prior art 4 has reached 57.89%. Because the product contains antimony trioxide, it not only increases the consumption of antimony trioxide, but also reduces the catalytic effect of antimony glycol. influences
In addition, in the prior art, there is a washing process. Except that the prior art 3 uses ethylene glycol for washing (ie, ethylene glycol recrystallization), the washing liquid used in the rest is methanol with high toxicity, low boiling point, and flammability. or ethanol, increasing production costs and safety costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0010] Example 2 First put 1850kg of ethylene glycol into the reaction tank, heat it to 100°C, then put in 280kg of antimony trioxide, start stirring, 100 rpm, and pass through 9kg / cm2 after 8 minutes 2 When the temperature in the tank reaches 100°C, start the vacuum system to keep the negative pressure in the tank at -0.06~-0.05mpa, control the temperature in the reaction tank at 141°C~145°C, and keep the boiling point of the mixture all the time. Control the production volume to ≤200 liters, and the reaction time is 3.8 hours. After the reaction is completed, carry out circulation filtration at 145°C, then slowly cool the ethylene glycol antimony liquid at 35°C for 30 minutes, and then use cooling water below 20°C Rapid cooling, cooling time 3.8 hours, to make it completely crystallized, the crystals enter the centrifugal dryer for drying, the mother liquor is returned to use after treatment, and the dried ethylene glycol antimony directly enters the quality inspection and pa...

Embodiment 3

[0011] Example 3 First put 1950kg of ethylene glycol into the reaction tank, heat it to 110°C, then put in 300kg of antimony trioxide, start stirring, 100 rpm, and pass 10kg / cm2 after 9 minutes 2 When the temperature in the tank reaches 100°C, start the vacuum system to keep the negative pressure in the tank at -0.06~-0.05mpa, and control the temperature in the reaction tank at 145°C~150°C, and keep the boiling point of the mixture all the time. Control the extraction volume to ≤200 liters, and the reaction time is 4 hours. After the reaction, carry out circulation filtration at 150°C, then slowly cool the ethylene glycol antimony liquid at 40°C for 30 minutes, and then use cooling water below 20°C Rapid cooling, cooling time 3.8 hours, to make it completely crystallized, the crystals enter the centrifugal dryer for drying, the mother liquor is returned to use after treatment, and the dried ethylene glycol antimony directly enters the quality inspection and packaging process. ...

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PUM

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Abstract

The invention which provides a non-drying preparation technology of ethylene glycol antimony relates to a preparation method of an antimony-containing compound catalyst for a polyester polycondensation reaction. The preparation method, which comprises the following steps: treating excessive ethylene glycol and diantimony trioxide as raw materials, carrying out esterification and dehydration under heating and negative pressure conditions, and filtering and cooling to crystallize, is characterized in that: cooled and crystallized crystals are directly subjected to quality inspection and packing after being dried by a centrifugation drier. In the invention, procedures of drying and washing are omitted, so the damage to ethylene glycol antimony chelates Sb2(OCH2CH2O)3 caused by drying is avoided, and usage of high toxic, flammable and explosive methanol and ethanol is avoided, thereby the production environment is improved, unsafe factors are eliminated, the technology is simplified and the safety cost is reduced; and simultaneously products of the technology of the present invention have 54% to 55% of antimony, the content of antimony is controlled below a theoretical value, and diantimony trioxide is eliminated in the products, so the catalytic performance of the products is improved, the dissolving temperature is reduced, a b value and an L value are improved, and raw material consumption is reduced.

Description

[0001] This application is a divisional application, original application date: 2007.6.26, application number: 200710035237.3, invention name: Preparation method of crystalline ethylene glycol antimony technical field [0002] The invention relates to a non-drying preparation method of an antimony compound catalyst used in polycondensation reaction of polyester. Background technique [0003] Ethylene glycol antimony is the third generation polyester catalyst after antimony trioxide and antimony acetate. There are many ways to prepare ethylene glycol antimony, such as Chinese patent, application date 99.4.16, application number 99114156.3, a high-purity ethylene glycol antimony preparation method (abbreviated as prior art 1), is based on excessive ethylene glycol Alcohol and antimony trioxide undergo lipidation dehydration reaction in the temperature range of 120-180°C, filter, cool, crystallize, and recrystallize with ethylene glycol, wash with alcohol to remove ethylene gly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/28C07C29/70
Inventor 刘谏文刘晓阳
Owner 安化县文威化工有限公司
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