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Preparation method of PTA (pure terephthalic acid) with flame-retardant function

A functional and flame retardant modifier technology, applied in the field of PTA preparation, can solve the problems affecting polyester mechanics, poor mutual fusion, single PTA product, etc., to improve production efficiency and product quality, promote growth, and increase output. Effect

Inactive Publication Date: 2018-07-27
ZHEJIANG MODERN TEXTILE IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned method has following shortcoming: because PTA and ethylene glycol, flame-retardant additive directly synthesize polyester after mixing, the interaction time of flame-retardant additive and polyester is shorter, mutual integration is relatively poor, synergistic effect is not sufficient enough, therefore can not be able to Give full play to the flame retardancy of flame retardant additives, and also affect the overall functions and quality effects of polyester mechanics
Therefore, the PTA product has always been single and almost unchanged

Method used

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  • Preparation method of PTA (pure terephthalic acid) with flame-retardant function

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A preparation method of PTA with flame retardant function, comprising the following steps:

[0038] 1) In parts by mass, 1 part of magnesium aluminum spinel, 1.3 parts of basic magnesium sulfate whiskers, 0.3 parts of nickel-iron spinel, 14 parts of 20wt% salicylic acid aqueous solution, 6 parts Mix oxyfluoric acid aqueous solution with a concentration of 10wt%, grind it with a liquid-phase high-energy ball mill (60°C, 2.5h), and then move it to a titanium-lined hydrothermal reactor for reaction (175°C, 2.5MPa, 11h) , then atomized and separated and dried, calcined (525°C, 4h), cooled to room temperature, then ground in a ball mill for 3h, moved to a stirred plasma reactor, and carried out radio frequency plasma treatment with nitrogen as a carrier gas (pressure 50Pa, power 55W, time 8min), then add it to 9 parts of 30wt% organic silicon ethanol solution, ultrasonically disperse (70°C, 1.5h), filter, fully wash with absolute ethanol, and then heat and dry , and passed ...

Embodiment 2

[0045] A preparation method of PTA with flame retardant function, comprising the following steps:

[0046] 1) In parts by mass, 0.8 parts of magnesium aluminum spinel, 1.6 parts of basic magnesium sulfate whiskers, 0.2 parts of nickel-iron spinel, 16 parts of 18wt% salicylic acid aqueous solution, 4 parts Aqueous hydrofluoric acid solution with a concentration of 12wt% was mixed, ground with a liquid-phase high-energy ball mill (50°C, 3h), and then moved to a titanium-lined hydrothermal reactor for reaction (150°C, 3MPa, 12h), and then Atomization separation and drying, calcination treatment (500°C, 5h), cooling to room temperature, grinding treatment in a ball mill for 2h, moving to a stirred plasma reactor, nitrogen as carrier gas, radio frequency plasma treatment (pressure 40Pa, power 80W, time 10min), then added to 8 parts of 32wt% organic silicon ethanol solution, ultrasonically dispersed (60°C, 2h), filtered, fully washed with absolute ethanol, then heated and dried, and...

Embodiment 3

[0053] A preparation method of PTA with flame retardant function, comprising the following steps:

[0054] 1) In parts by mass, 1.2 parts of magnesium aluminum spinel, 1.0 parts of basic magnesium sulfate whiskers, 0.4 parts of nickel-iron spinel, 12 parts of salicylic acid aqueous solution with a concentration of 22wt%, 8 parts The oxyfluoric acid aqueous solution with a concentration of 8wt% was mixed, ground with a liquid-phase high-energy ball mill (70°C, 2h), and then moved to a titanium-lined hydrothermal reactor for reaction (200°C, 2MPa, 10h), and then Atomization separation and drying, calcination treatment (550°C, 3h), cooling to room temperature, grinding treatment in a ball mill for 4h, moving to a stirred plasma reactor, nitrogen as carrier gas, radio frequency plasma treatment (pressure 60Pa, power 30W, time 5min), then added to 10 parts of 32wt% organic silicon ethanol solution, ultrasonically dispersed (80°C, 1h), filtered, fully washed with absolute ethanol, t...

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Abstract

The invention relates to the technical field of PTA (pure terephthalic acid) materials, and discloses a preparation method of PTA with a flame-retardant function. The preparation method comprises thefollowing steps: mixing a salicylic acid aqueous solution, a hypoflorous acid aqueous solution, magnesia-alumina spinel, alkali magnesium sulfate whisker and nickel iron spinel, grinding the mixture by a high energy liquid ball grinder, performing calcination, grinding by the ball grinder, performing radio frequency plasma treatment, performing ultrasonic dispersion in an organic silicone ethanolsolution, and performing filtration, washing, drying and sieving to prepare flame retardant powder; mixing acetic acid and deionized water, adding a sodium hexametaphosphate aqueous solution and the flame retardant powder, performing beating evenly, fusing a product with CTA slurry, performing crystallization three times, and performing washing, solid-liquid separation, steam drying and hydrogenation refining to prepare PTA. A flame-retardant modifier is added to the PTA preparation process, so that PTA has a flame-retardant function, and a synthetic material is prepared from PTA, interactiontime between the modifier and a substrate is long, the fusion degree is good, the synergistic effect is sufficient, and flame retardancy and mechanical properties of the synthetic material can be significantly enhanced.

Description

technical field [0001] The invention relates to the technical field of PTA materials, in particular to a preparation method of PTA with flame-retardant function. Background technique [0002] PTA is called pure terephthalic acid in Chinese and Pure terephthalic acid in English, or PTA for short. PTA is the lower-end product of petroleum. Purified terephthalic acid is made of p-xylene as raw material and acetic acid as solvent. Under the action of catalyst, it is oxidized in liquid phase to produce crude terephthalic acid, which is then refined by hydrogenation, crystallized and separated. , dried to obtain PTA. PTA is one of the important bulk organic raw materials, widely used in various aspects of the national economy such as light industry, agriculture, electronics, construction, adhesives, herbicides, fibers, plastics, etc. Most of the PTA in the world is used to produce polyester Synthetic material, PTA is an important raw material for synthetic polyester chips, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08K9/04C08K9/02C08K7/08C08K3/22
Inventor 凌荣根
Owner ZHEJIANG MODERN TEXTILE IND RES INST
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