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Preparation method of dihydric alcohol titanium

A technology of titanium diol and diol, applied in the field of preparation of titanium diol, can solve the problems of high anhydrous degree, difficult operation and high equipment requirements, achieve less harsh reaction conditions, simplify technological process, The effect of reducing process energy consumption

Pending Publication Date: 2022-02-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on the anhydrous degree of the system, corrosive gas hydrogen chloride is generated during the reaction process, the operation is difficult, the process is complicated, the manufacturing cost is high, and the equipment requirements are high

Method used

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  • Preparation method of dihydric alcohol titanium
  • Preparation method of dihydric alcohol titanium
  • Preparation method of dihydric alcohol titanium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 19g (0.1mol) TiCl to the flask 4 , 112.5g (2.5mol) formamide, stir evenly, dropwise add 12.4g (0.2mol) ethylene glycol at room temperature, control the rate of addition, so that the reaction temperature does not exceed 50 ° C, and white solids are constantly formed during the reaction. After the dropwise addition, continue to stir the reaction until the raw material titanium tetrachloride remains less than 1%. After the reaction is finished, cool to normal temperature, filter and separate the white solid product, wash thoroughly with water whose temperature does not exceed 15°C until there is no chloride ion in the washing solution, then wash with acetone, and dry at 60°C to obtain the titanium ethylene glycol catalyst. The rate is 95.6%.

[0035] The titanium content in the ICP test catalyst is 28.49%.

Embodiment 2

[0037] Add 19g (0.1mol) TiCl to the flask 4 , 135g (3mol) formamide, stir evenly, add 15.2g (0.2mol) 1,3-propanediol dropwise at room temperature, control the rate of addition, so that the reaction temperature does not exceed 60 ° C, white solids are constantly formed during the reaction, drop After the addition is complete, continue to stir the reaction until the raw material titanium tetrachloride remains less than 1%. After the reaction, cool to normal temperature, filter to obtain a white solid, and wash the white product solid with a large amount of water (not exceeding 20° C.) until there is no chloride ion in the washing liquid. Then wash the white solid with acetone, and dry the white solid at no more than 60° C. to obtain titanium propylene glycol with a yield of 96.2%.

[0038] The titanium content in the ICP test catalyst is 24.50%.

Embodiment 3

[0040] Add 19g (0.1mol) TiCl to the flask 4 , a mixed solution of formamide-ethyl acetate containing 112.5g (2.5mol) of formamide (the volume ratio of formamide / ethyl acetate is 60:40), stir evenly, and add 12.4g (0.2mol) of ethylene glycol dropwise at room temperature , Control the rate of addition so that the reaction temperature does not exceed 50°C, and white solids are continuously generated during the reaction. After the dropwise addition, continue to stir the reaction until the raw material titanium tetrachloride remains less than 1%. After the reaction is finished, cool to normal temperature, filter and separate the white solid product, wash thoroughly with water whose temperature does not exceed 15°C until there is no chloride ion in the washing solution, then wash with acetone, and dry at 60°C to obtain the titanium ethylene glycol catalyst. The rate is 95.7%.

[0041] The titanium content in the ICP test catalyst is 28.52%.

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Abstract

The invention discloses a preparation method of dihydric alcohol titanium. The dihydric alcohol titanium has a structure as shown in a formula (I) which is described in the specification. In the formula (I), n is equal to 2 or 3. According to the preparation method, an alkaline solvent method is adopted, titanium tetrachloride and dihydric alcohol react in an alkaline solvent, a product is directly separated out after the reaction is completed, and a pure product is obtained through separation and purification. The method can effectively adsorb acid mist, and is simple and convenient to operate, high in controllability, high in product yield and excellent in product hydrolysis resistance.

Description

technical field [0001] The invention relates to a method for preparing titanium glycolate, in particular to a method for preparing titanium glycolate with good acid mist adsorption effect and easy operation. Background technique [0002] Butylene terephthalate (PBT), polyethylene terephthalate (PET) and polytrimethylene terephthalate (PTT) are widely used in various fields of production and life, such as fibers, bottles, films And engineering plastics, etc., because polyester fiber is cheap and good, polyester fiber is the fastest growing among the three major synthetic fibers. The catalysts used to produce PET are mainly antimony, germanium and titanium series catalysts, and the antimony catalysts mainly include antimony acetate and antimony glycol. Antimony catalysts have moderate reactivity and low price, and the produced polyester has excellent performance. However, antimony is a heavy metal. In the production of antimony catalysts, PET production and post-processing su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C08G63/85
CPCC07F7/003C08G63/85
Inventor 仲军实李金平戴志彬王玉合朱兴松夏峰伟常玉周倩
Owner CHINA PETROLEUM & CHEM CORP
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