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Method for preparing hybridized p-xylene

A technology of p-xylene and xylene mother liquor, which is applied in the manufacture of fire-resistant and flame-retardant filaments, single-component copolyester artificial filaments, etc., can solve the problems of lack of research and development of refined products and special products, and single products. To achieve the effect of improving the overall function and quality, deep integration, and improving the overall function and quality

Inactive Publication Date: 2018-07-31
ZHEJIANG MODERN TEXTILE IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the product of p-xylene has always been single and almost unchanged, and there has been no research and development of refined products and special products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A preparation method of hybrid p-xylene, comprising the steps of:

[0045] (1) the concentration of 82% by weight is 4wt% fluorosulfonic acid solution, 22% concentration is 4wt% fluorophosphoric acid solution and 1.5% magnesium aluminum spinel, 7% aluminum hydroxide whisker and 1.2 % Mg-Zn spinel is uniformly mixed, moved to a hydrothermal reactor, continuously stirred and reacted for 4 hours at a temperature of 120°C and a pressure of 0.3MPa, and then cooled naturally under stirring, and liquid was carried by a liquid-phase high-energy ball mill at 50°C Grinding for 2.5 hours, filtering, calcining at 510°C for 5 hours, fully washing with deionized water, drying in vacuum at 93°C, grinding with a ball mill for 4 hours, and passing through a 250-mesh sieve to obtain a flame retardant hybrid agent;

[0046] (2) p-xylene is added successively with p-xylene weight as 9% acetic acid, 5% sodium hypophosphite, 1.5% o-xylene, 0.9% ethylamine co-solvent and 5% by ( 1) The prepa...

Embodiment 2

[0050] A preparation method of hybrid p-xylene, comprising the steps of:

[0051] (1) 60% concentration by weight is 4wt% fluorosulfonic acid solution, 6% concentration is 4wt% fluorophosphoric acid solution and 0.5% magnesium aluminum spinel, 3% aluminum hydroxide whisker and 0.5% % Mg-Zn spinel is uniformly mixed, moved to a hydrothermal reactor, continuously stirred and reacted for 5 hours at a temperature of 130°C and a pressure of 0.2MPa, and then cooled naturally under stirring, and carried liquid with a liquid-phase high-energy ball mill at 45°C Grinding for 3 hours, filtering, calcining at 500°C for 6 hours, fully washing with deionized water, drying in vacuum at 90°C, grinding with a ball mill for 5 hours, and passing through a 200-mesh sieve to obtain a flame retardant hybrid agent;

[0052] (2) p-xylene is added successively with p-xylene weight as 8% acetic acid, 3% sodium hypophosphite, 1% o-xylene, 0.8% ethylamine cosolvent and 4% by ( 1) The prepared flame reta...

Embodiment 3

[0056] A preparation method of hybrid p-xylene, comprising the steps of:

[0057] (1) the concentration of 90% by weight is 5wt% fluorosulfonic acid solution, 35% concentration is 3wt% fluorophosphoric acid solution and 2% magnesium aluminum spinel, 15% aluminum hydroxide whisker and 2 % magnesium-zinc spinel is uniformly mixed, moved to a hydrothermal reactor, and continuously stirred and reacted for 3 hours at a temperature of 110°C and a pressure of 0.4MPa, and then cooled naturally under stirring, and a liquid-phase high-energy ball mill was used to carry liquid at 55°C Grinding for 2 hours, filtering, calcining at 520°C for 4 hours, fully washing with deionized water, vacuum drying at 95°C, grinding with a ball mill for 3 hours, and passing through a 200-mesh sieve to obtain a flame retardant hybrid agent;

[0058] (2) p-xylene is added successively with p-xylene weight as 10% acetic acid, 6% sodium hypophosphite, 2% o-xylene, 1% ethylamine co-solvent and 3% by ( 1) The ...

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Abstract

A method for preparing hybridized p-xylene comprises the steps of: mixing a fluorosulfonic acid solution and a fluorophosphoric acid solution with magnesium aluminate spinel, aluminum hydroxide whiskers and magnesium zinc spinel, performing a hydrothermal reaction, grinding, filtering, calcining, washing and drying to obtain a flame retardant hybridizer; mixing p-xylene, acetic acid, sodium hypophosphite, o-xylene, an ethylamine cosolvent, a potassium hydrogen phosphate dispersion, and the obtained flame retardant hybridizer, grinding, filtering and dispersing to obtain a hybridized p-xylene mother liquor; adding the obtained hybridized p-xylene mother liquor in a form of spraying into the p-xylene to prepare the hybridied p-xylene. The product prepared by the method has an excellent flameretardant function.

Description

technical field [0001] The invention belongs to the technical field of developing new varieties of p-xylene, and in particular relates to a preparation method of hybrid p-xylene. Background technique [0002] Dimethylbenzene is a colorless transparent liquid; it is a product in which two hydrogens on the benzene ring are replaced by methyl groups, and there are three isomers of ortho, meta and para. Of the three xylene isomers, para-xylene has the largest commercial market. Para-xylene (para-xylene), which can be abbreviated as "PX", is a derivative of benzene, an important chemical raw material, a colorless liquid, and becomes a flaky or columnar crystal at low temperature, insoluble in water, soluble in ethanol, ether, Benzene, acetone, flammable. P-xylene is a basic organic raw material, of which about 80% is used for the preparation of terephthalic acid and synthetic materials. These synthetic materials are widely used in engineering plastics, construction materials, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/183C08K7/08C08K3/22D01F6/84D01F1/07
Inventor 陶仁中李琪韩文娟胡超胡克勤张芳
Owner ZHEJIANG MODERN TEXTILE IND RES INST
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