Method for preparing functional preset purified terephthalic acid

A refined terephthalic acid, pre-set technology, applied in the manufacture of fire-retardant and flame-retardant filaments, single-component copolyester rayon, etc., can solve the problems of single terephthalic acid product, property and personal safety, No consideration of purified terephthalic acid and other issues, to achieve the effect of improving dispersibility and compatibility, reducing impact, good overall function and quality effect

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

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Problems solved by technology

However, these synthetic materials using petroleum as raw materials are flammable materials, which have caused serious safety hazards to people's property and personal safety. Therefore, it is of great significance to develop special purified terephthalic acid for the synthesis of flame-retardant materials.
[0004] The key and core of modified polyester and its products are modified PTA, and in the existing literature, the preparation of purified terephthalic acid is mainly considered from the purification process, that is, to reduce the content of impurities such as p-carboxybenzaldehyde, reduce In the subsequent polycondensation reaction of purified terephthalic acid, the impact of this impurity on the reaction is hardly considered. The development of some new varieties of purified terephthalic acid is applied to some special materials, such as the preparation of modified materials with special functions, etc.
Therefore, the product of purified terephthalic acid has always been single, and almost unchanged

Method used

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  • Method for preparing functional preset purified terephthalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] A kind of preparation method of functional preset purified terephthalic acid, comprises the steps:

[0067] (1) In parts by mass, 0.3 parts of silicon carbide whiskers, 0.15 parts of nickel-aluminum spinel and 1.4 parts of dawsonite whiskers are added to 14 parts of 3% perchloric acid aqueous solution, Mix 3.5 parts of phosphorous acid aqueous solution with a mass fraction of 3%, grind at 70°C for 2.5 hours with a liquid-phase high-energy ball mill, then move to a titanium-lined hydrothermal reactor, and process at 175°C and 2.5MPa 11h, then atomized and separated and dried, calcined at 525°C for 4h, cooled to room temperature, then ground in a ball mill for 3h, moved to a stirred plasma reactor, and carried out radio frequency at 50Pa and 55W with nitrogen as the carrier gas Plasma treatment for 7 minutes, then added to 16 parts of organic silicon ethanol solution with a mass fraction of 30%, ultrasonically dispersed at 65°C for 1.5 hours, filtered, fully washed with a...

Embodiment 2

[0072] A kind of preparation method of functional preset purified terephthalic acid, comprises the steps:

[0073] (1) In parts by mass, 0.4 parts of silicon carbide whiskers, 0.1 parts of nickel-aluminum spinel and 1.8 parts of dawsonite whiskers are added to 10 parts of 4% perchloric acid aqueous solution, Mix 5 parts of phosphorous acid aqueous solution with a mass fraction of 2%, grind at 80°C for 2h with a liquid-phase high-energy ball mill, then move to a titanium-lined hydrothermal reactor, and treat at 200°C and 3MPa for 10h, Then atomize, separate and dry, calcinate at 500°C for 5 hours, cool to room temperature, grind in a ball mill for 4 hours, move to a stirred plasma reactor, use nitrogen as a carrier gas, and conduct radio frequency plasma at 40Pa and 80W power Treat for 10 minutes, then add to 12 parts of 30% organic silicon ethanol solution, ultrasonically disperse at 70°C for 1 hour, filter, wash thoroughly with absolute ethanol, heat and dry, and pass through...

Embodiment 3

[0078] A kind of preparation method of functional preset purified terephthalic acid, comprises the steps:

[0079] (1) In parts by mass, 0.2 parts of silicon carbide whiskers, 0.2 parts of nickel-aluminum spinel and 1.0 parts of dawsonite whiskers are added successively to 18 parts of perchloric acid aqueous solution with a mass fraction of 2%, Mix 2 parts of phosphorous acid aqueous solution with a mass fraction of 4%, grind it with a liquid-phase high-energy ball mill at 60°C for 3h, then move it to a titanium-lined hydrothermal reactor, and treat it at 150°C and 2MPa for 12h. Then atomize, separate and dry, calcinate at 550°C for 3 hours, cool to room temperature, grind in a ball mill for 2 hours, move to a stirred plasma reactor, use nitrogen as a carrier gas, and conduct radio frequency plasma at 60Pa and 30W power Treat for 5 minutes, then add to 20 parts of organic silicon ethanol solution with a mass fraction of 20%, ultrasonically disperse at 60°C for 2 hours, filter,...

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Abstract

A method for preparing a functional preset purified terephthalic acid comprises the following steps: (1) mixing and rinding a silicon carbide whisker, nickel aluminum spinel, a dawsonite whisker, a perchloric acid aqueous solution and a phosphorous acid aqueous solution, after hydrothermal reaction, atomizing, separating, drying, calcining, re-grinding, performing plasma treatment, silicone modification, and filtration, washing, and drying to obtain a preset flame retardant; (2) mixing acetic acid, water, a sodium hexametaphosphate aqueous solution and the preset flame retardant obtained in the step (1), beating and dispersing to obtain a special modifying liquid, fusing the special modifying liquid with crude terephthalic acid slurry, crystallizing, performing solid-liquid separation, washing, drying, beating, performing solid-liquid separation again, and hydrorefining to obtain the preset purified terephthalic acid. The product prepared by the method has good effects such as flame retardance.

Description

technical field [0001] The invention belongs to the technical field of purified terephthalic acid variety development, and in particular relates to a method for preparing functionally preset purified terephthalic acid. Background technique [0002] PTA (Pure terephthalic acid) is purified terephthalic acid. PTA is the lower-end product of petroleum, usually p-xylene is used as raw material, acetic acid is used as solvent, and under the action of catalyst, it is oxidized in liquid phase to generate crude terephthalic acid, which is then refined by hydrogenation, crystallized, separated, and dried to obtain PTA. . For example, patents US5723656, US006307099 and US4241220 etc. have described a typical production process of purified terephthalic acid. First, the raw material p-xylene is dissolved in an acetic acid solvent containing a cobalt-manganese-bromine catalyst, and air or oxygen-enriched is passed through to oxidize to generate crude terephthalic acid (CTA). The typic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/183C08K9/00C08K9/04C08K7/00C08K7/10C08K3/22D01F6/84D01F1/07
CPCC08G63/78C08G63/183C08K3/22C08K7/00C08K7/10C08K9/00C08K9/04C08K2003/2227C08K2003/2293D01F1/07D01F6/84
Inventor 李琪庞学松范艳苹凌荣根张芳
Owner ZHEJIANG MODERN TEXTILE IND RES INST
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