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Phosphate ester substance and its preparation method, polyester resin containing phosphate ester substance and its preparation method

A polyester resin, phosphoric acid ester-containing technology, applied in the direction of phosphorus organic compounds, chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, etc. The haze of the ester resin increases and the hue of the polyester resin is not good, so as to achieve the effect of improving the heat resistance and speed

Inactive Publication Date: 2021-01-22
FAR EASTERN NEW CENTURY COPRRATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It also revealed that when phosphoric acid is used, as the amount of phosphoric acid increases, the time of polycondensation reaction will also increase, and it is easy to generate antimony phosphate, which will cause the haze of polyester resin to increase
The U.S. patent also discloses that phosphate triester can be used, but phosphate triester cannot effectively inhibit the degradation reaction of polyester resin, the hue of polyester resin is still poor, and the rate of solid state polymerization cannot be effectively improved. In addition, for polyester There is no significant effect on the heat resistance of the resin during secondary processing

Method used

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  • Phosphate ester substance and its preparation method, polyester resin containing phosphate ester substance and its preparation method
  • Phosphate ester substance and its preparation method, polyester resin containing phosphate ester substance and its preparation method
  • Phosphate ester substance and its preparation method, polyester resin containing phosphate ester substance and its preparation method

Examples

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preparation example Construction

[0041] The preparation method of the phosphate ester substance comprises the following steps of phosphorylating the compound represented by the formula (A) with the phosphating agent to obtain the compound selected from the compound represented by the formula (I), the formula ( II) Phosphate ester substances of the compounds shown or a combination of the above.

[0042]

[0043] In said formula (A), R 1 and R 2 Independently represent C 2 to C 4 straight chain alkylene or C 3 to C 4 Branched chain alkylene. The C 2 to C 4 straight chain alkylene and the C 3 to C 4 The branched alkylene group is as described above, so it will not be repeated. Preferably, R 1 and R 2 Independently represent C 2 straight-chain alkylene.

[0044]A specific example of the compound represented by the formula (A) is, but not limited to, bis-ethylene terephthalate [bis(2-hydroxyethyl)terephthalate]. The source of said bis-ethylene terephthalate is, for example, commercially available...

preparation example 1

[0062] [Preparation Example 1] Phosphate ester substance

[0063] First add 100 ml of solvent (1,2-dichloroethane, 1,2-dichloroethane) to a reaction flask, then add 15.05 g (0.105 mol) of pentaquinone in the reaction flask under an ice-bath environment Phosphorus oxide (P 2 o 5 ). After phosphorus pentoxide was uniformly dispersed in the solvent, in the reaction flask, adding successively a total amount of 29.9g (0.118mol) of bis-ethylene terephthalate (manufacturer model: Tokyo Chemical Industry CO. B3429). Next, the temperature of the reaction bottle was raised to 80° C. by gradually increasing the temperature, so that bis-ethylene terephthalate and phosphorus pentoxide were phosphorylated. After the phosphorylation reaction was carried out for 3 hours, in the reaction flask, add 2wt% deionized water [the calculation basis of the deionized water consumption is: (weight+two pentoxide of ethylene glycol terephthalate) Phosphorus weight)×2%], and the phosphorylation reacti...

Embodiment 1

[0067] [Example 1] Polyester resin containing phosphate ester substance

[0068] Add 345.8g (2.083mole) of terephthalic acid and 161.49g (2.605mole) of ethylene glycol into a 1-liter reactor, at 260°C and 2kg / cm 2 The esterification reaction of terephthalic acid and ethylene glycol is carried out under the condition of nitrogen pressure. When the conversion rate of the esterification reaction reaches more than 80%, add the phosphoric acid ester material of Preparation Example 1 that has been dispersed in ethylene glycol in advance and that the consumption is 0.034g, and 300ppm of antimony trioxide (Sb 2 o 3 ) to obtain a mixture. The mixture was reacted at 270 to 275° C., and after 135 minutes of reaction, a polyester resin containing phosphoric acid ester was obtained (theoretical phosphorus content in the polyester resin containing phosphoric acid ester was 11.14 ppm).

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Abstract

A phosphate ester substance is selected from the compound represented by formula (I), the compound represented by formula (II) or a combination thereof. The definition of each substituent in formula (I) and formula (II) is as described in the specification and claims. The phosphate ester substance is suitable for the preparation of polyester resin, and the preparation method of polyester resin comprises the following steps: providing a mixture containing catalyst, phosphate ester substance and dicarboxylate component, wherein the dicarboxylate component has at least one A dicarboxylate-based substance; reacting the mixture to obtain a polyester resin containing a phosphate ester substance. Phosphate ester substances can not only prevent the polyester resin containing phosphate ester substances from degrading during the polycondensation process, but also increase the rate of solid state polymerization. In addition, the secondary processing heat resistance of polyester resins containing phosphate substances is significantly better than that of polyester resins that do not contain phosphate substances.

Description

technical field [0001] The invention relates to a phosphoric ester substance and a preparation method thereof. The phosphoric ester substance is an additive used in preparing polyester resins. The phosphoric ester substance relates to a phosphoric ester substance with a specific structure. The invention also relates to a method for preparing polyester resin using the phosphoric acid ester substance, and the obtained polyester resin. Background technique [0002] The existing polyester resin preparation method will add a metal-containing catalyst in the polycondensation reaction to accelerate the rate of the polycondensation reaction. However, such a metal-containing catalyst will cause the polyester resin to undergo a degradation reaction, making the polyester resin in the polycondensation process. Medium degradation, and then cause the molecular weight of the obtained polyester resin to be insufficient and have the problem of poor hue. [0003] In order to solve the above ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09C08G63/692
CPCC07F9/091C08G63/6926C08G63/85C08G63/80C08K5/523C08L67/02C07F9/12C08G63/82
Inventor 黄德仁郑莘卉
Owner FAR EASTERN NEW CENTURY COPRRATION