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Technique for preparing octadecyl acrylate with fusion esterification method

A technology of octadecyl acrylate and acrylic acid, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of easy removal of product water, complicated post-treatment process, short reaction time, etc. The effect of reducing post-processing cost, fast reaction rate and short reaction time

Inactive Publication Date: 2008-09-24
SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of technology that adopts melting esterification to prepare stearyl acrylate, this technology does not use entrainer, has fast reaction rate, high reaction selectivity, short reaction time, high yield of ester, easy to form It has the advantages of easy detachment of water and other advantages, avoiding the complicated and difficult post-treatment process caused by the use of organic solvents in the existing production process, and realizing the clean production of high-grade acrylate

Method used

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  • Technique for preparing octadecyl acrylate with fusion esterification method
  • Technique for preparing octadecyl acrylate with fusion esterification method
  • Technique for preparing octadecyl acrylate with fusion esterification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 74.7g of n-octadecanol and 0.81g of inhibitor hydroquinone into a 500ml four-neck flask equipped with a thermometer, agitator and reflux condenser, heat to 60°C to melt them all, then add 24.5g of acrylic acid and 1g of catalyst p-toluenesulfonic acid, stir and mix evenly; heat the mixture under the condition of 90-110°C to reflux for about 2.5 hours, then install a water separator for dehydration, after separating out more water, heat up to Continue the heat preservation reaction at 135°C for 2.5 hours. When the amount of water released is observed to be equivalent to the theoretical value, the esterification reaction is considered to be basically completed. Stop heating at this time, and remove unreacted acrylic acid and residual water by distillation under reduced pressure; then pour the product into a beaker, and wash off residual p-toluenesulfonic acid, hydroquinone and a small amount of it with a 5% sodium hydroxide aqueous solution. Acrylic, then washed sever...

Embodiment 2

[0030] Add 76.8g of isostearyl alcohol (isostearyl alcohol) and 0.72g of polymerization inhibitor phenothiazine into a 500ml four-neck flask equipped with a thermometer, agitator and reflux condenser, and heat it to 60°C to make it completely melt , and then sequentially add 26.5 g of acrylic acid and 1 g of catalyst p-toluenesulfonic acid, stir and mix evenly. Heat the mixture under the condition of 80-120°C for 3 hours, and then install a water separator for dehydration; after separating out more water, raise the temperature to 140°C and continue the heat preservation reaction for 2 hours. When the values ​​are equivalent, the esterification reaction is considered to be basically complete. Heating was stopped, and unreacted acrylic acid and residual water were distilled off under reduced pressure. Then pour the product into a beaker, wash off residual p-toluenesulfonic acid, hydroquinone and a small amount of acrylic acid with 5% potassium hydroxide aqueous solution, and th...

Embodiment 3

[0032] Add 78.2g of isostearyl alcohol (isostearyl alcohol) and 0.90g of inhibitor hydroquinone into a 500ml four-neck flask equipped with a thermometer, agitator and reflux condenser, and heat to 60°C to make it all melt Then, add 25.5 g of acrylic acid and 1 g of catalyst p-toluenesulfonic acid in sequence. The mixture was first heated to reflux at 90-120°C for about 2 hours, and then installed with a water separator for dehydration. After more water was separated, the temperature was raised to 140°C to continue the heat preservation reaction for 3 hours; When the values ​​are equivalent, the esterification reaction is considered to be basically complete. Heating was stopped, and unreacted acrylic acid and residual water were distilled off under reduced pressure. Then pour the product into a beaker, wash off residual p-toluenesulfonic acid, hydroquinone and a small amount of acrylic acid with 5% sodium hydroxide aqueous solution, and then wash with water several times until...

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Abstract

The present invention provides a method used for preparing octadecyl acrylate through melt esterification. In the method, inhibitor with 0.3 to 0.8 percent of the weight of the octadecanol is added into the octadecanol and is heated so as to be completely melted; acrylic acid with 1.2 to 1.5 times of the molar weight of the octadecanol and a catalyst with 0.5 to 1.2 percent of the weight of the octadecyl are added orderly and mixed; the mixture is heated to be at the temperature between 60 DEG C and 120 DEG C for 2 to 3 hours for reflux reaction; water generated in the reaction is separated; the mixture is continuously heated to be at the temperature between 130 DEG C and 140 DEG C, and reacts for 2 to 4 hours at the constant temperature; the acrylic acid that can not completely react and the residual water are removed through vacuum distillation; the reaction products are washed by caustic alkali aqueous solution and then by water to be neutral; finally the products are treated through vacuum drying for 6 to 8 hours at the temperature of 40 DEG C; thus the waxy solid octadecyl acrylate can be prepared. The method has the advantages of high reaction rate, high reaction selectivity, short reaction time, high yield of the ester, easy separation of the water that is generated in the reaction, and so on. No azeotropic agent is used in the reaction. Thus the method avoids the serious pollution caused by toxic solvents and belongs to the clean production process.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a synthesis method of a higher ester of acrylic acid-stearyl acrylate, in particular to a process for preparing stearyl acrylate by a melt esterification method. Background technique [0002] Octadecyl acrylate is an important organic chemical raw material. Octadecyl acrylate is an acrylic functional monomer obtained by the reaction of acrylic acid and stearyl alcohol under the action of an acidic catalyst. Its freezing point is 24°C. It has the characteristics of low toxicity and low viscosity. It is insoluble in water and soluble in general organic solvents. . The main application of octadecyl acrylate is as plasticizer, adhesive, fiber treatment agent, paper finishing agent, lubricating oil additive, leveling agent, etc. [0003] At present, the methods for preparing stearyl acrylate mainly include transesterification and solvent esterification. The transesterification metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
Inventor 俞燕龙杨帆陈士龙
Owner SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP