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Preparation method of ethylene glycol antimony

A technology of ethylene glycol antimony and ethylene glycol, applied in the field of preparation of ethylene glycol antimony, can solve problems such as insufficient solubility, and achieve the effects of ensuring filtration effect, reducing steam energy consumption, and reducing reaction temperature

Active Publication Date: 2014-03-05
HUNAN CHENZHOU MINING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solubility of the product produced by this method is not enough, the b value is often above 4.0, and the L value is below 90

Method used

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  • Preparation method of ethylene glycol antimony
  • Preparation method of ethylene glycol antimony
  • Preparation method of ethylene glycol antimony

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Laboratory research and development

[0047] According to the technical process of the present invention, the sample produced in the laboratory has carried out product analysis, and the determination of each process parameter has passed through some comparative experiments, and the process is as follows:

[0048] 1. Product sample analysis

[0049] The product sample was qualitatively analyzed with an infrared spectrometer, and the infrared absorption spectrum of the product was shown in figure 1 shown. Depend on figure 1 Analysis shows that 1085, 1038cm -1 C—O stretching vibration peaks, 2939, 2872cm -1 for CH 2 C—H stretching vibration peak, 1461cm -1 for CH 2 The bending vibration peak of , indicating the presence of ethylene glycol groups in the product; and the reactant Sb 2 o 3 It can be seen from the comparison of the infrared absorption spectra that Sb 2 o 3 Has been converted to antimony glycol.

[0050] 2. Analysis of factors affecting yield and qu...

Embodiment 2

[0075] (2) Industrial production

[0076] According to the various process parameters determined above, the weight ratio of feeding materials is 4~7:1 (ethylene glycol: antimony trioxide), the vacuum degree of the reactor is -0.05~-0.07MPa, the reaction temperature is 120~150℃, and the produced water volume is 150 ~300kg / ton Sb 2 o 3 , The dosage of activated carbon is 2~6kg / ton of Sb 2 o 3 , Cooling and crystallization temperature 35-25°C, centrifugal drying rotation speed 800-1200 rpm, continuous production for 15 days, a total of 15 tons of antimony trioxide was invested, 21.3 tons of ethylene glycol antimony was produced, and 12.1 ethylene glycol was consumed tons, 90kg of activated carbon, 17 tons of bituminous coal, and several other materials. The statistics are as follows:

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Abstract

The invention discloses a preparation method of ethylene glycol antimony. The method comprises the following steps of: feeding antimonous oxide and ethylene glycol into a sealed reaction kettle according to the mass ratio of 1 to (4-7), and heating the antimonous oxide and the ethylene glycol to 120-150 DEG C to react for 1-3 hours at a pressure is -0.05MPa to -0.07MPa; adding active carbon to decolor the reaction liquid and remove impurities of the reaction liquid for 15-30 minutes after the reaction is finished; filtering the cleaned reaction liquid by a 200-400 mesh filter screen to obtain feed liquid; cooling the feed liquid to 35-25 DEG C to crystallize; and drying crystallized solid for 15-25 minutes in an centrifugal machine with 800-1200 r / min. The method is short in reaction time, short in flow and low in cost, and the ethylene glycol antimony prepared by the method is high in content and good in chromaticness, and can be widely applied to industrial production.

Description

technical field [0001] The invention relates to a preparation method of ethylene glycol antimony, which belongs to the field of catalyst synthesis. Background technique [0002] Antimony glycol, chemical formula Sb 2 (OCH 2 CH 2 O) 3 , relative molecular weight 423.5, theoretical antimony content 57.5%. Its main purpose is as a new type of catalyst used in the production process of polyester (PET). During the polycondensation reaction of polyester, it can activate the relevant functional groups of the reactants and promote the reaction. It is used in the production of polyester Bottle-level slices, textile slices and membrane-level slices, etc. Because ethylene glycol antimony has less impurity content, is easily soluble in ethylene glycol and has no toxicity, its performance is better than antimony trioxide and antimony acetate. At present, the annual production capacity of polyester in the world has exceeded 80 million tons, and the global consumption of antimony for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/28C07C29/70
Inventor 王晶杨第武彭蛟龙
Owner HUNAN CHENZHOU MINING CO LTD
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