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Catalyzing and decoloring integrated method for synthesizing environment-friendly plasticizer triethylhexyl (2-propylheptyl) citrate

An environmentally friendly plasticizer, citric acid three technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid esters, etc., can solve the problem of deep color of target products, low product yield, and many side reactions And other problems, to achieve the effect of shortening the production cycle, simplifying the operation, and good thermal stability

Inactive Publication Date: 2013-04-10
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many problems in the catalytic method of concentrated sulfuric acid, such as serious corrosion of equipment, many side reactions, such as alcohol and alcohol intramolecular dehydration into alkene, intermolecular dehydration into ether, and sulfuric acid ester, resulting in dark color of the target product. Activated carbon for decolorization
A large amount of activated carbon will adsorb the product, resulting in a decrease in the yield of the product

Method used

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  • Catalyzing and decoloring integrated method for synthesizing environment-friendly plasticizer triethylhexyl (2-propylheptyl) citrate
  • Catalyzing and decoloring integrated method for synthesizing environment-friendly plasticizer triethylhexyl (2-propylheptyl) citrate
  • Catalyzing and decoloring integrated method for synthesizing environment-friendly plasticizer triethylhexyl (2-propylheptyl) citrate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 Catalyst immobilized preparation

[0026] Using a high-concentration p-toluenesulfonic acid solution as the active center precursor to immobilize the activated carbon to prepare a heterogeneous catalyst: Weigh 10g of powdered activated carbon, wash it with deionized water until neutral, activate it at 120°C for 2h, and soak it in 70g of activated carbon with a mass fraction of 50 % of p-toluenesulfonic acid aqueous solution, immobilized at room temperature for 35 hours, filtered, and dried to constant weight to obtain p-toluenesulfonic acid immobilized on activated carbon, abbreviated as C-pTSA, as a heterogeneous catalyst.

Embodiment 2

[0027] Embodiment 2 prepares three (2-propyl heptyl) citrates

[0028] Add 4.2kg of citric acid monohydrate, 11.7kg of 2-propylheptanol (the molar ratio of citric acid monohydrate to 2-propylheptanol is 1:3.7), 0.126kg of catalyst, and stir to raise the temperature to 110℃ ~150°C, the reaction time is 4h, and the esterification rate reaches 99.6%; the crude product is dealcoholized by vacuum distillation, the temperature is 140°C~150°C, and the vacuum degree is 0.09MPa. After the alcohol is no longer released, the catalyst is filtered out, and the filtrate is re- Carry out neutralization alkali washing and water washing. Neutralization alkali washing uses 5% sodium bicarbonate and 1% sodium hydroxide aqueous solution at a temperature of 50 ° C ~ 70 ° C. Water washing uses deionized water or distilled water at a temperature of 60 ℃~90℃; and finally dry to obtain the colorless product tris(2-propylheptyl) citrate.

Embodiment 3

[0029] Embodiment 3 prepares three (2-propyl heptyl) citrates

[0030] Add 4.2kg of citric acid monohydrate, 12.6kg of 2-propylheptanol (the molar ratio of citric acid monohydrate to 2-propylheptanol is 1:4.0), and 0.105kg of heterogeneous catalyst in the reaction kettle, stir and heat up to the temperature 110°C~150°C, reaction time 6h, the esterification rate reached 99.7%; the crude product was dealcoholized by vacuum distillation, the temperature was 140°C~150°C, and the vacuum degree was 0.09MPa. After the alcohol was no longer released, the catalyst was filtered out. The filtrate is then subjected to neutralization and alkali washing and water washing. The neutralization and alkali washing uses 5% sodium bicarbonate and 1% sodium hydroxide aqueous solution at a temperature of 50°C to 70°C, and deionized water or distilled water is used for water washing. The temperature is 60°C~90°C; finally, it is dried to obtain the colorless product tris(2-propylheptyl) citrate.

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Abstract

A catalyzing and decoloring integrated method for synthesizing environment-friendly plasticizer triethylhexyl (2-propylheptyl) citrate belongs to the technical field of chemical synthesis. The method comprises: taking p-toluenesulfonic acid as an active central body, immobilizing the p-toluenesulfonic acid on an active carbon to prepare a heterogeneous catalyst, taking citric acid monohydrate or anhydrous citric acid and 2-propyl heptanol as main reaction materials, using the heterogeneous catalyst for catalyzing and decoloring, taking cyclohexane as a water carrying agent, stirring and raising the temperature to 110-150 DEG C to conduct an esterification reaction, reducing the pressure and distilling to remove excess ethanol after the reaction is over, separating the heterogeneous catalyst from a reaction system, filtering the catalyst, and neutralizing, washing with alkali, washing with water and drying a crude product, so as to obtain a finished product of the triethylhexyl (2-propylheptyl) citrate. The selected raw materials are easy to get and cheap, high in catalytic activity, good in selectivity, and high in esterification yield; the used catalyst can be recycled and is not obviously corrosive; the method integrates catalyzing and decoloring, is simple in operation and is economic and environment-friendly; in addition, the obtained product is free from toxic, good in plasticity and thermal stability and small in mobility, and is not easy to volatilize.

Description

technical field [0001] The catalytic decolorization integrated synthesis of environmentally friendly plasticizer tris(2-propylheptyl) citrate belongs to the technical field of chemical synthesis. Specifically relates to a non-toxic, good plasticizing performance, good thermal stability, non-volatile, small migration of citrate plasticizers. Its preparation method is to use anhydrous or monohydrate citric acid and 2-propylheptanol to synthesize citric acid tris(2- Propylheptyl) ester, and then dealcoholize the resulting crude product under reduced pressure, filter, neutralize and alkali wash, wash with water, and dry to realize the integrated process of catalytic decolorization to obtain a colorless oily product. Background technique [0002] Plasticizers have long been dominated by phthalates such as dioctyl phthalate (DOP). However, these products are difficult to meet the requirements of environmental protection in terms of many properties, especially hygiene and low tox...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08C07C67/48
CPCY02P20/584
Inventor 蒋平平叶媛园冷炎秦晓洁
Owner JIANGNAN UNIV
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