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Process for synthesizing organometallic antimonide

A synthesis process, organometallic technology, applied in the direction of antimony organic compounds, etc., can solve the problems of low concentration, low yield, high toxicity, etc.

Inactive Publication Date: 2010-04-14
李绍通
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Antimony trioxide not only has poor solubility and low activity, but also leads to poor color, thermal stability and spinnability of products.
The disadvantage is that the concentration range of antimony trioxide in ethylene glycol is small and the concentration is low, resulting in low yield and high cost
Dioxane is a highly toxic, flammable, explosive and volatile solvent, which increases cost and investment when used in large quantities
[0010] Although the method with the application number 01106356.4 uses carbon fiber fabrics for decolorization, the color of ethylene glycol antimony is not good, so it still needs to be washed with absolute ethanol
[0011] The method whose application number is 00110819.0 uses inert gas N2 to take out the water generated by the reaction, but the reaction solution is still blue or black, which reduces the conversion rate of antimony trioxide and affects the product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a four-necked 500Ml flask with a stirrer, thermometer, and rectification tube (connected to a vacuum pump and hydrogen and nitrogen lines) that can be heated, add 50 grams of antimony trioxide (purity 99.8%) and 200 grams of ethylene glycol (purity) 99.5%). Start the vacuum pump. When the pressure of the vacuum gauge is -0.09MPa, stop the pump and slowly turn on the nitrogen to make the pressure zero. Repeat the operation three times to replace the oxygen in the bottle as much as possible. Then open the hydrogen or the mixed gas valve of hydrogen and nitrogen to enter the gas, make the pressure 0.05MPa, heat under stirring, and control the temperature at 160-170°C, and react for 120 minutes. During the heating reaction process, the pressure is maintained at -0.06MPa~0.02MPa by supplementing hydrogen and nitrogen, and the water and other substances generated by the reaction are separated through the rectification tube, no water is discharged, and the reaction is comple...

Embodiment 2

[0031] Repeat the operation of Example 1, wherein 50 grams of antimony trichloride and 180 grams of ethylene glycol are added. After 120 minutes of reaction, the reaction solution was transparent and colorless. The vacuum was released with nitrogen, cooled to room temperature under stirring, separated and dried to obtain white crystals of antimony glycol, with an antimony content of 57.35%.

Embodiment 3

[0033] Repeat the operation of Example 1, wherein 50 grams of antimony oxychloride and 250 grams of ethylene glycol are added. After 120 minutes of reaction, the reaction solution was transparent and colorless. The vacuum was released with nitrogen, cooled to room temperature under stirring, separated and dried to obtain white crystals of antimony glycol, with an antimony content of 57.4%.

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PUM

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Abstract

This invention discloses a new synthesis technology of diatomic alcohol antimonium of organic antimonide used for polyester polycondensation. The technology uses antimonious material and diatomic alcohol to synthesize diatomic alcohol antimonium in the presence of reducing substances through reaction, filtration, crystallization and drying. The material combined with good solubility, high purity,high catalytic activity and the advantages of color, and the excessive alcohol can be recycled.

Description

Technical field [0001] The invention relates to a synthesis process of an antimony-containing organometallic compound-antimony diol, and belongs to the synthesis process field of a catalyst used for polycondensation of polyester or copolyester. Background technique [0002] At present, the polycondensation catalyst used by most polyester enterprises at home and abroad is antimony dioxide (Sb 2 O 3 ), antimony acetate and antimony diol Sb(O-R-O) 3 Sb (where R is C 2 H 4 Or C 3 H 6 Or C 4 H 8 ), applied to the production of synthetic polyester or copolyester such as DMT method and PTA method. [0003] Antimony trioxide is not only difficult to dissolve and low activity, but also leads to poor product color, thermal stability, and spinnability. Although antimony acetate improves the solubility, it has the problems of low antimony content and corrosion of equipment. [0004] The antimony diol has high solubility in the diol, and has the highest antimony content in the soluble antimony c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/90
Inventor 李绍通
Owner 李绍通
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