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A kind of triisononyl citrate compound and preparation method thereof

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

Active Publication Date: 2017-12-26
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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  • A kind of triisononyl citrate compound and preparation method thereof
  • A kind of triisononyl citrate compound and preparation method thereof
  • A kind of triisononyl citrate compound and preparation method thereof

Examples

Experimental program
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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) 192.14g citric acid, 504.88g isononyl alcohol, 55.76g hexanaphthene and 0.96g catalyst are joi...

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) 192.14g citric acid, 663.55g isononyl alcohol, 81.29g hexanaphthene and 4.03g catalyzer are joined in t...

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 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) 192.14g citric acid, 778.95g isononyl alcohol, 106.82g hexanaphthene and 6.92g catalyst are joined in the there-...

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Abstract

The invention provides a triisononyl citrate compound and a preparation method thereof, including the preparation of a loaded heteropolyacid catalyst and the preparation of triisononyl citrate, belonging to the field of citric acid plasticizers. Under the action of catalyst, citric acid and isononyl alcohol are esterified into triisononyl citrate at 110~170℃. The reaction time is 1~3 hours. During the reaction, cyclohexane is used as water carrier. After the reaction is completed, the Cool the solution to 50-80°C, filter to obtain the catalyst, recycle and reuse, dealcoholize under reduced pressure, wash with alkali, and wash with water until neutral; add activated carbon for adsorption decolorization, and dry to obtain the product triisononyl citrate. The catalyst used in the method has high catalytic activity, high reutilization rate, high purity of the obtained product, and overcomes the disadvantages of high volatility, poor low-temperature resistance, and poor extraction resistance of existing citric acid low-carbon alcohol ester plasticizers.

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 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 environment...

Claims

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Application Information

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