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Composite PTA preparation method

A technology of aqueous solution and fluoboric acid, applied in the direction of single-component polyester rayon, etc., can solve the problems of insufficient synergistic effect, side reactions, and poor mutual fusion, so as to improve the overall function and quality effect, improve the dispersion and Compatibility, the effect of promoting the growth of oxide crystals

Inactive Publication Date: 2018-09-04
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, the above method has the following disadvantages: since the polyester is directly synthesized after the polymerization of PTA and ethylene glycol, the interaction time between the anti-aging additive and the polyester is relatively short, the mutual fusion is poor, and the synergistic effect is not sufficient, so the anti-aging additive cannot be fully utilized. Anti-aging properties, and will also produce many side reactions, affecting the overall functions and quality effects of polyester mechanics
[0005] The key and core of modified polyester and its products is modified PTA, and there is no report on how to develop PTA with anti-aging function. For PTA products, at present, the preparation of PTA is mainly considered from the purification process, that is, to reduce The content of impurities such as carboxybenzaldehyde reduces the influence of such impurities on the reaction of PTA in the subsequent polycondensation reaction, and almost no consideration is given to the development of some new PTA varieties for some special occasions, such as the preparation of modified products with special functions. material etc.
Therefore, the PTA product has always been single and almost unchanged, and there has been no introduction of refined products and special products.

Method used

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  • Composite PTA preparation method

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Effect test

Embodiment 1

[0065] A preparation method of composite PTA, comprising the steps of:

[0066] (1) By mass parts, 1.25 parts of zinc molybdate, 1.25 parts of cerium oxide, 6 parts of mass fraction are 20% fluoroboric acid aqueous solution, 0.5 parts of graphene oxide, 0.5 parts of tin oxide, 0.2 parts of Titanium oxide and 10 parts of perchloric acid aqueous solution with a mass fraction of 2% are fully mixed, ground at 50°C for 3 hours with a high-energy ball mill, and then moved to a hydrothermal reactor lined with titanium, and then heated at 190°C, 3MPa Down treatment for 7 hours, cooling and filtering, calcining at 525°C for 4.5 hours, cooling to room temperature, grinding in a ball mill for 3.5 hours, moving to a stirred plasma reactor, using nitrogen as a carrier gas at 45Pa, 65W power RF plasma treatment for 8 minutes, then added to 12.5 parts of 30% organic silicon ethanol solution, ultrasonically dispersed at 70°C for 2 hours, filtered, fully washed with absolute ethanol, then heat...

Embodiment 2

[0071] A preparation method of composite PTA, comprising the steps of:

[0072] (1) In parts by mass, 1 part of zinc molybdate, 1.5 parts of cerium oxide, 8 parts of mass fraction of 15% fluoroboric acid aqueous solution, 0.4 part of graphene oxide, 0.6 part of tin oxide, 0.3 part of Titanium oxide and 8 parts of perchloric acid aqueous solution with a mass fraction of 1% are fully mixed, ground at 55°C for 2 hours with a high-energy ball mill, and then moved to a hydrothermal reactor lined with titanium, and then heated at 200°C, 2MPa Down treatment for 8 hours, cooling and filtering, calcining at 530°C for 5 hours, cooling to room temperature, grinding in a ball mill for 3 hours, moving to a stirred plasma reactor, using nitrogen as a carrier gas, and performing radio frequency plasma at 40Pa and 80W power The body was treated for 6 minutes, and then added to 15 parts of ethanol solution of organic silicon with a mass fraction of 40%, ultrasonically dispersed at 80°C for 1 h...

Embodiment 3

[0077] A preparation method of composite PTA, comprising the steps of:

[0078] (1) In parts by mass, 1.5 parts of zinc molybdate, 1 part of cerium oxide, 4 parts of mass fraction of 30% fluoroboric acid aqueous solution, 0.6 parts of graphene oxide, 0.4 parts of tin oxide, 0.1 part of Titanium oxide and 12 parts of perchloric acid aqueous solution with a mass fraction of 2% are fully mixed, ground at 45°C for 4 hours with a high-energy ball mill, then moved to a hydrothermal reaction kettle lined with titanium, and then heated at 180°C, 4MPa Down treatment for 6 hours, cooling and filtering, calcining at 520°C for 4 hours, cooling to room temperature, grinding in a ball mill for 4 hours, moving to a stirred plasma reactor, using nitrogen as a carrier gas, and performing radio frequency plasma at 50Pa and 50W power The body was treated for 10 minutes, and then added to 10 parts of ethanol solution of organic silicon with a mass fraction of 20%, ultrasonically dispersed at 60°C...

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Abstract

The invention relates to a composite PTA preparation method. The method comprises the following steps: 1) mixing zinc molybdate, cerium oxide, a fluorboric acid aqueous solution, graphene oxide, tin oxide and titanium oxide, and a perchloric acid aqueous solution and grinding a mixture, and then performing a hydro-thermal reaction and steps of filtering, calcining, plasma processing, and organosilicon modification to prepare composite age-proof powder; and 2) mixing acetic acid and water, adding a sodium hexametaphosphate aqueous solution and the composite age-proof powder obtained in the step1), and beating the materials for dispersing to obtain the composite age-proof agent, fusing the composite age-proof agent with crude terephthalic acid slurry, performing crystallization and solid-liquid separating, washing the material, and performing steps of drying, beating, and solid-liquid separating to obtain composite PTA. The prepared product has obvious age proof effect.

Description

technical field [0001] The invention belongs to the technical field of PTA varieties, and in particular relates to a preparation method of composite PTA. 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 typical reaction pressure is 0.6-1.6MPa, the temperature is 160-200°C,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08K9/00C08K9/06C08K3/24C08K3/22C08K3/38C08K3/04D01F6/92D01F1/10
Inventor 范艳苹胡克勤凌荣根李琪杨晓静
Owner ZHEJIANG MODERN TEXTILE IND RES INST
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