Non-drying preparation method of ethylene glycol antimony

A technology of ethylene glycol antimony and drying method, which is applied to the preparation of metal alcohols, the separation/purification of hydroxyl compounds, organic chemistry, etc., and can solve the problem of difficult further improvement of product whiteness and brightness, high price of heavy metal inhibitors, and product hue value. There are problems such as influence, to achieve the effect of saving heavy metal inhibitors, reducing the cost of decolorization and impurity removal, and eliminating unsafe factors

Active Publication Date: 2011-05-18
益阳市华昌锑业催化剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the simultaneous use of activated carbon and heavy metal inhibitors for decolorization and impurity removal, there are the following problems: first, the removal of impurities by heavy metal inhibitors has an impact on the hue value of the product, and it is difficult to further improve the whiteness and brightness of the product; second, the process control is more difficult , the stability of product quality is poor; the third is that heavy metal inhibitors are expensive, resulting in higher production costs; the fourth is that the output is high and the consumption of ethylene glycol is large; the fifth is that the heavy metal impurity content of antimony trioxide is relatively low. , and then aggravate the removal of impurities by metal inhibitors, the effect of improving the removal of impurities is not obvious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: First put 1800kg of ethylene glycol into the reaction tank, heat up to 80°C, then put in 300kg of antimony trioxide, start stirring, 90 rpm, and pass 8kg / cm2 after 10 minutes 2 When the temperature in the tank reaches 100°C, start the vacuum system to keep the negative pressure in the tank at -0.099-0.089mpa. The production volume is ≤120 liters, and the reaction time is 3.5 hours. After the reaction is completed, according to 1% of the input weight of antimony trioxide, add medical activated carbon decolorizer, keep it for 10-15 minutes, and carry out circulation filtration at 150°C. After the reaction, the material is output from the reaction tank, and returns to the same reaction tank through the filter and pipeline, and then filters the ethylene glycol antimony liquid again with another filter to further remove the impurities leaked in the circulating filtration After filtration, cool slowly at 30°C for 30 minutes, then quench with cooling water below 20°...

Embodiment 2

[0017] Embodiment 2: first 1700kg ethylene glycol is dropped into retort, heating 100 ℃, then drop into 275kg antimony trioxide, start stirring, 100 rev / mins, pass through 9kg / cm after 8 minutes 2 When the temperature in the tank reaches 100°C, start the vacuum system to maintain the negative pressure in the tank -0.09mpa, control the temperature in the reaction tank at 141°C-145°C, keep the boiling point of the mixed liquid at all times, and control the output ≤90 liters, the reaction time is 3.2 hours, after the reaction, add activated carbon decolorizer according to 1.5% of the weight of antimony trioxide input, keep it for 10 minutes, carry out circulation filtration under the condition of 150 ℃, and remove the material after the reaction from the reaction Tank output, through the filter and pipeline and then back to the same reaction tank, and then filter the ethylene glycol antimony liquid again with another filter to further remove the impurities leaked in the circulatin...

Embodiment 3

[0018] Embodiment 3: first 1650kg ethylene glycol is dropped into reaction tank, heating 110 ℃, then drop into 250kg antimony trioxide, start to stir, 100 rev / mins, after 9 minutes, pass through 10kg / cm Steam heating, when tank After the temperature reaches 100°C, start the vacuum system to keep the negative pressure in the tank at -0.098~-0.080mpa, control the temperature in the reaction tank at 145°C~150°C, keep the boiling point of the mixed liquid at all times, and control the production volume to ≤70 liters. The reaction time was 2.8 hours. After the reaction was finished, 2.5% of the weight was added by antimony trioxide. Add medical activated carbon decolorizing agent, preferably medical activated carbon decolorizing agent, keep for 12 minutes, carry out circulation filtration at 150°C, output the material after the reaction from the reaction tank, pass through the filter and pipeline and return to the same Reaction tank, and then use another filter to filter the ethyle...

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PUM

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Abstract

The invention provides a non-drying preparation method of ethylene glycol antimony, and relates to a preparation method of antimony-containing compound catalyst which is used in polyester polycondensation reaction. The preparation method is characterized by comprising the following steps: adding antimony trioxide and ethylene glycol in a reaction tank to be subjected to esterification dehydrationreaction, wherein the weight ratio of the antimony trioxide to ethylene glycol is 1:(6-7), the temperature in the reaction tank is 135-150 DEG C and the pressure ranges from minus 0.10MPa to minus 0.08MPa; after the reaction, adding a single activated carbon decolouring impurity-removing reagent in the reaction tank for decolouring and impurity removal, then performing circulating filtration, andthen filtering again; and then conveying filtrate to a crystallizing tank, crystallizing the filtrate, performing centrifuge dripping, and then directly performing inspection and packaging. In the method provided by the invention, washing and drying are not required, and the chelate structure of the product is not damaged; and the single activated carbon decolouring impurity-removing reagent is used, thus the effects of decolouring and impurity removal are good, the hue value of the product is high, the loss of ethylene glycol is less, the stability of the product quality is good, the operation is simple, and the production cost is low.

Description

technical field [0001] The invention relates to a preparation method of an antimony compound catalyst used for polycondensation reaction of polyester. Background technique [0002] Most of the existing ethylene glycol antimony production methods adopt drying process, such as Chinese patent, application date 2001.11.20, application number is a kind of ethylene glycol antimony preparation method of 01134185, with excessive ethylene glycol Alcohol and antimony trioxide undergo lipidation dehydration reaction in the temperature range of 120°C to 180°C, filter, cool and crystallize, recrystallize with ethylene glycol, and directly remove ethylene glycol by heating and drying under reduced pressure. Due to the drying process, part of the Sb 2 (OCH 2 CH 2 O) 3 The chelating structure of the ethylene glycol is destroyed and reduced to antimony trioxide, which not only increases the consumption of antimony trioxide, but also affects the catalytic effect of ethylene glycol antimon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/28C07C29/70C07C29/74C08G63/86
Inventor 刘谏文刘晓阳刘坚固
Owner 益阳市华昌锑业催化剂有限公司
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