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Triisononyl citrate compound and preparation method thereof

A technology of citric acid tri-compound, which is applied in the field of tri-isononyl citrate compound and its preparation, can solve the problems of poor low temperature resistance, high volatility, poor extraction resistance and the like, and achieves low wear resistance and volatility. Small, good plasticizing effect

Active Publication Date: 2016-04-06
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at the defects of tri-n-nonyl citrate, and the technical problems such as high volatility, poor low-temperature resistance, and poor extraction resistance of low-carbon alcohol ester plasticizers of citric acid. Improvements were made and a citrate ester compound with a new structure was invented: triisononyl citrate, whose structure is shown in the following formula

Method used

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  • Triisononyl citrate compound and preparation method thereof
  • Triisononyl citrate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of novel load heteropolyacid catalyst:

[0037] 1) Ultrafine SiO 2 Carrier pretreatment: take a certain amount of particle size is 3μm, specific surface area is 220m 2 Soak the ultrafine silicon dioxide per gram with 2mol / L dilute hydrochloric acid for 4 hours, wash it with deionized water, dry it under an infrared lamp, and bake it in a muffle furnace at 500°C for 2.5 hours;

[0038] 2) PO 4 3- -RuO 4 2- / SiO 2 Catalyst preparation: immerse the carrier treated in step 1) in 4mol / L sodium ruthenate solution, filter and dry after 6 hours, then immerse it in a phosphoric acid solution with a mass fraction of 50%, and heat it in a water bath to 50 ℃, after 4 hours, filter, dry, roast and wash with water to remove the soluble substances in the catalyst, and put it in a desiccator for later use;

[0039] Preparation of triisononyl citrate:

[0040] 1) Add 192.14g of citric acid, 504.88g of isononyl alcohol, 55.76g of cyclohexane and 0.96g of ca...

Embodiment 2

[0044] The preparation method of novel load heteropolyacid catalyst:

[0045] 1) Ultrafine SiO 2 Carrier pretreatment: take a certain amount of particle size is 4μm, specific surface area is 189m 2 Soak the ultrafine silica per gram with 2mol / L dilute hydrochloric acid for 6 hours, wash it with deionized water, dry it under an infrared lamp, and bake it in a muffle furnace at 500°C for 3.3 hours;

[0046] 2) PO 4 3- -RuO 4 2- / SiO 2 Catalyst preparation: immerse the carrier treated in step 1) in 4mol / L sodium ruthenate solution, filter and dry after 6 hours, then immerse it in a phosphoric acid solution with a mass fraction of 40%, and heat it in a water bath to 50 ℃, after 4 hours, filter, dry, roast and wash with water to remove the soluble substances in the catalyst, and put it in a desiccator for later use;

[0047] Preparation of triisononyl citrate:

[0048] 1) Add 192.14g of citric acid, 663.55g of isononyl alcohol, 81.29g of cyclohexane and 4.03g of catalyst in...

Embodiment 3

[0052] The preparation method of novel load heteropolyacid catalyst:

[0053] 1) Ultrafine SiO 2 Carrier pretreatment: take a certain amount of particle size is 5μm, specific surface area is 170m 2 Soak / g of ultrafine silica with 2mol / L dilute hydrochloric acid for 8 hours, wash it with deionized water, dry it under an infrared lamp, and bake it in a muffle furnace at 500°C for 4 hours;

[0054] 2) PO 4 3- -RuO 4 2- / SiO 2 Catalyst preparation: immerse the carrier treated in step 1) in a 4mol / L sodium ruthenate solution, filter and dry after 6 hours, then immerse it in a phosphoric acid solution with a mass fraction of 45%, and heat it in a water bath to 50 ℃, after 4 hours, filter, dry, roast and wash with water to remove the soluble substances in the catalyst, and put it in a desiccator for later use;

[0055] Preparation of triisononyl citrate:

[0056] 1) Add 192.14g of citric acid, 778.95g of isononyl alcohol, 106.82g of cyclohexane and 6.92g of catalyst into a t...

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Abstract

The invention provides a triisononyl citrate compound and a preparation method thereof; the preparation method comprises preparation of a loaded heteropoly acid catalyst and preparation of triisononyl citrate; the invention belongs to the citric acid plasticizer field. The preparation method comprises the steps: esterifying citric acid and isononyl alcohol under the action of a catalyst at the temperature of 110-170 DEG C to synthesize triisononyl citrate with the reaction time of 1-3 hours, during reaction, taking cyclohexane as a water carrying agent, after the completion of the reaction, cooling the solution to 50-80 DEG C, filtering to obtain the catalyst, recycling and reusing, and carrying out reduced pressure dealcoholization, alkali washing and water washing to be neutral; and adding activated carbon, carrying out adsorption decolorization, drying, and thus obtaining the product triisononyl citrate. The catalyst used in the method has high catalytic activity and high repeated utilization rate, the purity of the obtained product is high, and the shortcomings that a conventional citric acid low-carbon alcohol ester plasticizer has high volatility, poor low-temperature resistance, poor extraction resistance and the like are overcome.

Description

technical field [0001] The invention relates to a triisononyl citrate compound and a preparation method thereof, belonging to the technical field of citric acid plasticizers. Background technique [0002] In recent years, the demand for plasticizers in my country's industry is increasing, which mainly depends on the rapid development of the plastics industry. Plasticizer, also known as plasticizer, is an additive added to plastic, resin or elastomer materials to increase the softness of the material or to liquefy the material. It can improve the processing type, plasticity, flexibility, Stretch or expand. More than 80% of the plasticizers used by my country's plastic manufacturers are phthalate plasticizers represented by dioctyl phthalate (DOP, or DEHP). This type of plasticizer is highly volatile and migratory, and is a carcinogen. In 2012, many domestic brands of liquor were found to contain excessive plasticizers, prompting people to pay close attention to the environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/18
CPCY02P20/584C07C69/704B01J27/1856B01J27/188C07C67/08
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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