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Preparation method for cycloolefin anhydride plasticizer

A technology of cycloalkene acid anhydrides and plasticizers, which is applied in the field of preparation of cycloalkene acid anhydride plasticizers, can solve the problems of application limitations and poor miscibility, and achieve the effect of good miscibility

Inactive Publication Date: 2009-12-30
ZHENJIANG UNION CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although benzene-based plasticizers have not been found to be toxic to the human body, due to their symmetrical molecular structure and non-polarity, their miscibility with PVC is poor, and they are easy to precipitate in the case of high additions in PVC emulsified powder systems. , so there are certain limitations in its application

Method used

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  • Preparation method for cycloolefin anhydride plasticizer
  • Preparation method for cycloolefin anhydride plasticizer
  • Preparation method for cycloolefin anhydride plasticizer

Examples

Experimental program
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Embodiment Construction

[0015] Embodiments of the inventive method comprise the following steps:

[0016] Step 1: Add 2.6 parts of isononyl alcohol and 1 part of 1,2,3,6-tetrahydrophthalic anhydride into the reaction kettle, heat up to 160-180°C while stirring, and carry out the monoesterification reaction;

[0017] Step 2: When the temperature rises to 160-180°C, add 200ppm tetraisopropyl titanate and 300ppm antioxidant. The antioxidant can be selected from known antioxidant ingredients, such as phosphite antioxidant, secondary One or more of phosphoric acid or hindered phenol antioxidants;

[0018] The third step: continue to heat up to 225°C, hold the temperature for 2 to 5 hours to carry out the double esterification reaction, reduce the acid value to below 0.3mgKOH / g, add alkali to neutralize to less than 0.05mgKOH / g;

[0019] Step 4: Lower the temperature to 210-215°C, and dealcoholize under reduced pressure for 1.5 hours;

[0020] Step 5: Cool down to 95-98°C, add 5% pure water to kill the c...

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Abstract

The invention relates to a preparation method for a cycloolefin anhydride plasticizer, which comprises the following steps: firstly, adding 2 to 4 portions of isononyl alcohol and one portion of 1,2,3,6-tetra hydro phthalic anhydride into a reaction kettle for mono-esterification reaction; secondly, increasing the temperature to between 160 and 180 DEG C, and adding a catalyst; thirdly, continuously increasing the temperature to 225 DEG C, and performing di-esterification reaction; fourthly, reducing the temperature to between 210 and 215 DEG C, and performing dealcoholization under reduced pressure for 1 to 2 hours until the alcohol-containing mass percent is less than 0.05 percent; fifthly, reducing the temperature to between 85 and 98 DEG C, adding pure water sterilizing tetraisopropyl titanic acid ester which accounts for 2 to 5 percent of the reaction product in the kettle, fully reacting the mixture, and increasing the temperature to between 100 and 110 DEG C for decompression dehydration; and sixthly, adding activated carbon and diatomite for decoloration and filtration to obtain a finished product. The obtained product does not contain a benzene ring structure, thereby having environmental-friendliness and non-toxic effect on a human body. Through practical detection, compared with the conventional product, the product has better solubility with a PVC system.

Description

technical field [0001] The invention relates to the manufacture of an additive used in plastic production, in particular to a preparation method of a cycloalkene acid anhydride plasticizer. Background technique [0002] In the prior art, Chinese patent application CN1824688 discloses a phthalate polyester plasticizer: poly-1,2-propylene glycol phthalate, poly-1,3-butylene phthalate and ortho-phthalate Poly-1,4-butylene phthalate products; this type of product is produced by polymerization of phthalic anhydride and corresponding diols, 2-ethylhexanol with tetra-n-butyl titanate as a catalyst be made of. Chinese patent application CN101157615 discloses a production method of plasticizer diisononyl phthalate. [0003] Chinese patent application CN101245009 discloses a kind of manufacture method of dioctyl terephthalate plasticizer, and it comprises that the polyester waste cloth after cleaning, drying is chopped, puts into reactor; Add octanol and anhydrous ethyl alcohol to r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/75C07C67/08C08K5/12
Inventor 曹锋
Owner ZHENJIANG UNION CHEM IND
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