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Hexa-hydrogen phthalate compound and preparation thereof

A technology of phthalate and phthalate alcohol, which is applied in the field of hexahydrophthalate compound and its preparation, can solve the problem of small molecular weight, plasticization efficiency containing benzene ring, healthy human body hazards, etc.

Inactive Publication Date: 2009-01-14
NANYA PLASTICS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Food packaging materials made of DEHA plasticizers are restricted because DEHA is suspected of being harmful to human health; and food packaging materials made of diisononyl adipate (DINA) plasticizers, although due to molecular weight The improvement of the plasticizer in the film improves the migration, but the adhesion of the film decreases
[0005] In the prior art, U.S. Patent US3110603 discloses a benzoic acid dibasic ester compound, which has good compatibility with PVC resin, but contains benzene rings in its structure and has low plasticization efficiency
And publication number WO2005023926 discloses a kind of diethylene glycol ester plasticizer, and its composition is to use the raw material such as benzoic acid to make with the way of excess acid, but also contains benzene ring on the structure and molecular weight is small, easy to volatilize when processing

Method used

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  • Hexa-hydrogen phthalate compound and preparation thereof
  • Hexa-hydrogen phthalate compound and preparation thereof
  • Hexa-hydrogen phthalate compound and preparation thereof

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preparation example Construction

[0024] The preparation method of the hexahydrophthalate compound of the present invention comprises the first stage of esterification reaction, the second stage of esterification reaction, neutralization and washing steps, distillation steps, drying and water removal steps and filtration and purification steps:

[0025] The first stage of esterification reaction:

[0026] In order to obtain an excellent plasticizer effect, when carrying out the first stage of esterification reaction, use C 4 ~C 12 Dibasic alcohol and hexahydrophthalic anhydride are used as raw materials, and in the presence of a catalyst, they are put into a reactor with stirring and a condenser for esterification; wherein, the molar excess of dibasic alcohol is 0.1% to 20%; The amount of catalyst added is 0.1wt% to 3.0wt% based on the total weight of the reactants, and the catalyst type can be acidic (such as p-toluenesulfonic acid, etc.) or organometallic (such as tetraisopropyl titanate, etc.), but Cataly...

Embodiment 1

[0049] The reaction raw materials are 0.5 mole of hexahydrophthalic anhydride, 1.15 mole of diethylene glycol, 1.0 g of catalyst TIPT (tetraisopropyl titanate) and 34.0 g of xylene are simultaneously fed into the attached magnet for stirring and condensation In the four-necked flask of the reactor, the reaction temperature is 160°C to 180°C, and the reaction time is 5 hours. During the reaction, moisture must be removed. After the reaction is below the acid value of 3mgKOH / g, 0.96 moles of 2-ethylhexanoic acid (2 -EHA), the reaction temperature is 160°C-230°C, the reaction time is 5 hours, and the esterification reaction is completed after the acid value is below 5mgKOH / g. After the reaction is completed, the reaction liquid is neutralized with an aqueous solution of alkali metal hydroxide, and then washed with water, distilled, dried to remove water, and purified by filtration to obtain a hexahydrophthalate compound with a good hue.

[0050] Use the obtained hexahydrophthalat...

Embodiment 2

[0053] The reaction raw materials are 0.5 mole of hexahydrophthalic anhydride, 1.05 mole of triethylene glycol, 1.0 g of catalyst TIPT (tetraisopropyl titanate) and 34.0 g of xylene are simultaneously fed into the attached magnet for stirring and condensation In the four-necked flask of the reactor, the reaction temperature is 160°C to 180°C, and the reaction time is 5 hours. During the reaction, moisture must be removed, and 0.97 moles of 2-ethylhexanoic acid (2-ethylhexanoic acid (2- EHA), the reaction temperature is 160°C-230°C, the reaction time is 5 hours, and the esterification reaction is completed after the acid value is below 5mgKOH / g. After the reaction is completed, the reaction solution is neutralized with an aqueous solution of alkali metal hydroxide, and then washed with water, distilled, dried to remove water, and purified by filtration to obtain a hexahydrophthalate compound with good color.

[0054] Use the obtained hexahydrophthalate compound as the plasticiz...

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Abstract

The invention relates to hexahydrophthalic acid ester compound used for preparing the plasticizer without phthalic acid and benzoic acid, which can not cause damage to the organism and the environment. The invention adopts the preparation method that firstly, the esterifying reaction is performed to hexahydrophthalic anhydride and diatomic alcohol and catalyzator, after acid radical is removed, the hexahydrophthalic acid ester alcohol is synthetized, then monoprotic acid is added into the synthetized hexahydrophthalic acid ester alcohol to continue the esterificating reaction, and finally, the hexahydrophthalic acid ester compound is produced.

Description

technical field [0001] The present invention relates to a hexahydrophthalate compound and a preparation method thereof, in particular to the use of the obtained hexahydrophthalate compound, which can be used as resin processing such as polyvinyl chloride, cosmetics or medical supplies. Plasticizers are used. Background technique [0002] Plasticizers can provide the processability, flexibility, and electrical insulation of resins during the processing of polyvinyl chloride and other resins, and plasticizers have a swelling effect and can be dissolved in resins to form a homogeneous phase. Compared with the resin before adding the plasticizer, it can effectively reduce the processing temperature of the thermoplastic material, make the resin easy to be subjected to thermal flow molding, increase elasticity and reduce hardness, etc. [0003] The plasticizers with the largest amount currently used are dioctyl phthalate (Di-2-ethylhexyl phthalate, DOP) and diisononyl phthalate (...

Claims

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Application Information

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IPC IPC(8): C08K5/12C08L27/06C07C69/753
Inventor 谢嵩岳冯殿润许汉卿刘阳涂
Owner NANYA PLASTICS CORP
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