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Preparation process of benzoic ether plasticizer through solid acid catalysis

A solid acid catalyst, benzoate technology, applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry and other directions, can solve problems such as unfavorable large-scale production, high cost of raw materials, hidden safety hazards, etc., and achieve a green production process. Environmental protection, good catalytic activity, and the effect of eliminating the generation of waste water

Inactive Publication Date: 2017-05-10
GUANGZHOU YINTIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under the catalysis of anhydrous potassium carbonate, diethylene glycol ester and benzoate are transesterified to obtain diethylene glycol dibenzoate (publication number CN101987819 A). This method adopts transesterification, which needs to be added in batches Boiling agent, high raw material cost
Using tetravalent titanium oxide, SnO, and ZnO metal oxide compound as a catalyst to catalyze the esterification reaction of diethylene glycol and benzoate (publication number CN101376631 A) to generate diethylene glycol dibenzoate and sulfuric acid or titanate as the production method of catalyst, this method avoids the neutralization water washing process after the end of the reaction, and solves the problem of little or no sewage in the plasticizer production process, but the method uses peroxide ( Hydrogen peroxide and sodium peroxycarbonate complex) and activated carbon adsorption for decolorization and purification, peroxide is explosive under heated conditions
This brings safety hazards to production and is not conducive to mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] Catalyst preparation

[0017] A certain amount of La 2 0 3 Dissolve in 3.0mol·L-1 dilute hydrochloric acid to form La 3+ solution, and then measure TiC1 according to a certain volume ratio 4 with La 3+ The solution was mixed with NH 4 ·HO[w(NH 3 )=12%] hydrolyzed until the solution is alkaline, control the pH value at 8-9, the precipitation is complete, after standing for 24h, carry out suction filtration, and continuously wash with distilled water until the precipitation does not have Cl-exist (with 0.1mol L-1 AgNO 3 inspection), dried at 110°C and ground into fine powder. Then soak the powder in dilute H with a concentration of 1.0 mol L-1 2 SO 4 for 24 hours, then suction filtered, dried in a drying oven at 110°C, activated by roasting at 550°C for 4 hours, cooled and placed in a desiccator for later use.

Embodiment 1

[0019] Add benzoic acid (122.12g, 1mol), alcohol ester dodecane (240.3g, 1.1mol) and catalyst 0.072g into a 1000ml four-neck flask, raise the temperature to 180°C, add water-carrying agent n-butyl ether, and maintain the reaction temperature After reacting for 10 hours at 180-190°C, GC showed that the acid reaction was complete, stop heating, cool down to room temperature, filter, rectify under reduced pressure, recover alcohol ester dodeca and water-carrying agent, and obtain dodecyl alcohol benzoate. Yield: 91.5%, content: 99.1%.

Embodiment 2

[0021] Add benzoic acid (122.12g, 1mol), ethylene glycol (28.21g, 0.45mol) and catalyst 0.045g into a 1000ml four-neck flask, heat up to 160°C, add water-carrying agent cyclohexane, and maintain the reaction temperature at 150 -160°C, after 6 hours of reaction, GC showed that the alcohol reaction was complete, stop heating, pass nitrogen to recover the acid and water-carrying agent, cool down to room temperature, filter, and rectify under reduced pressure to obtain ethylene glycol dibenzoate. Yield: 96.5%, content: 99.3%.

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Abstract

The invention discloses a preparation process of a benzoic ether plasticizer through solid acid catalysis. A preparation method of the preparation process is characterized in that benzoic acid and alcohol are used as raw materials and directly take reaction to generate a benzoic ether compound under the catalysis of a water-carrying agent and a catalyst. Compared with sulfuric acid, a used catalytic system has the advantages that better catalytic activity is realized on toluenesulfonic acid and sodium hydrogen sulfate, so that the catalyst consumption is low; in addition, a loading type solid acid catalyst is used, so that the catalyst separation can be realized through direct filtering after the reaction is finished; the catalyst can be repeatedly used; the production process is simpler; in addition, the generation of waste water can be basically avoided; the production process achieves the green and environment-friendly effects.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of fine chemical products, in particular to a preparation process of a solidified acid-catalyzed benzoate plasticizer. Background technique [0002] Plasticizers are the most widely used additives in the processing and production of PVC and other plastics. Without plasticizers, PVC will become very hard and brittle, which cannot meet the softness or flexibility requirements of plastic products in production and life. Plasticizers in my country are widely used and have a large output. Nearly 80% of the plasticizers are phthalates, such as DOP and DBP. Due to the potential carcinogenic effect of DOP, its use is restricted in the United States and other countries. my country also has relevant regulations restricting the use of phthalate plasticizers. [0003] Benzoate is a new type of environmentally friendly plasticizer developed in my country in recent years. It has good compati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/78B01J27/053
CPCC07C67/08B01J27/053C07C69/78
Inventor 杨海玉黄春龙姜鹏楚庆岩谢丽青
Owner GUANGZHOU YINTIAN NEW MATERIAL CO LTD
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