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Method for producing semi-dulling titanium series polyester

A titanium-based polyester and semi-matte technology, which is applied in the production of semi-matte titanium-based polyester, can solve the problems of decreased catalyst activity, reduced diethylene glycol generation and degradation reaction, and inability to prepare viscous polyester.

Active Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the catalyst are: the antimony-based catalyst contains heavy metals and pollutes the environment; the polymer is gray
[0007] Titanium dioxide has an effect on the activity of titanium-based polyester catalysts. If titanium dioxide and titanium catalysts are added to the reaction system, the catalyst activity will decrease, and polyester with acceptable viscosity cannot be prepared within the same polycondensation time.
US6699545 ​​and WO2008008836 disclose the addition of zinc p-toluenesulfonate to polyester prepolymers, which can shorten the time of solid-state polycondensation and reduce the generation and degradation of diethylene glycol, but sulfonic acid or sulfonate compounds are used in semi-dull titanium series The preparation of polyester has not been reported

Method used

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  • Method for producing semi-dulling titanium series polyester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of Catalyst A

[0046] Add 12.4 grams (0.2 mol) of ethylene glycol in the reactor that stirrer, condenser and thermometer are equipped with, slowly drop into reactor 28.4 grams (0.1 mol) tetraisopropyl titanate, separate out white precipitate, After reacting at 70°C for 2 hours, the product was centrifuged, and the residue was washed with distilled water three times, and the product was vacuum-dried at 70°C to obtain a white powdery substance.

[0047] Place the dried white powdery substance in a reactor with a stirrer, a condenser and a thermometer, add 50 grams of ethylene glycol, 32 grams of 25% aqueous sodium hydroxide solution (0.2 moles), magnesium acetate tetrahydrate 21.4 gram (0.1 mole), 21 grams (0.1 mole) of citric acid monohydrate, and 14 grams (0.1 mole) of trimethyl phosphate were reacted for 2 hours at a reaction temperature of 150° C. to obtain a nearly colorless homogeneous liquid, which was catalyst A.

[0048] Preparation of polyester

...

Embodiment 2

[0052] Catalyst A was placed under strong sunlight and irradiated continuously for 3 months. No change in the color and appearance of the catalyst was found. The catalytic performance was tested again. The results are shown in Table 1.

Embodiment 3

[0054] Catalyst A was placed in the room without being protected from light for one and a half years, and no change in the color and appearance of the catalyst was found. The catalytic performance was tested again, and the results are shown in Table 1.

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Abstract

The invention relates to a method for producing semi-dulling titanium series polyester, mainly solving the problem that titanium pigment has an inhibition effect on the activity of a titanium series polyester catalyst in the traditional production process. The method comprises the following steps: carrying out esterification reaction on dicarboxylic acid and alkylene diol used as raw materials inthe presence of a titanium series polyester catalyst; adding titanium pigment as a dulling agent; and then carrying out polycondensation reaction in vacuum so as to obtain a polyester product. The used titanium series polyester catalyst comprises reaction products of the following materials: (A) a titanium compound having a general formula of Ti (OR)4, wherein R is alkyl having 1-10 carbon atoms;(B) dihydric alcohol having 2-10 carbon atoms; (C) at least one metal compound of IA in an element periodic table; (D) at least one metal compound of IIA, IB, IIB, VIIB and VIII in the element periodic table; (E) at least one fatty organic acid selected from organic acids; and (F) at least one phosphate compound selected from phosphorus compounds. Sulfoacid or a sulfonate compound is used as a cocatalyst and has a formula of RSO3M, wherein R is alkyl or substituted aryl having 1-20 carbon atoms, and M is hydrogen, or one of IA, IIA, IB, IIB, VIIB and VIII in the element periodic table. Through the technical scheme, the problem in the traditional production is well solved, and the method can be used for industrial production of polyesters.

Description

technical field [0001] The present invention relates to a method for producing semi-dull titanium series polyester. Background technique [0002] Polyethylene terephthalate (hereinafter referred to as polyester) is an important industrial raw material. Due to its various excellent properties, it can be widely used in fibers, bottles, films and other materials. It is the largest variety of synthetic fibers. It also has very important uses in engineering plastics and other industrial fields. [0003] Catalyst is an important link in the polyester production process. At present, the polyester catalysts with more industrial production and research are mainly three series of catalysts: antimony, germanium and titanium. Among them, antimony series catalysts are most commonly used in polyester industrial equipment ( Including antimony trioxide, antimony acetate and antimony glycol, etc.), at present, more than 90% of polyesters in the world are produced by antimony-based catalysts,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/87C08G63/83C08K3/22
Inventor 周文乐熊金根章瑛虹郁剑乙张俊
Owner CHINA PETROLEUM & CHEM CORP