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Method for catalytically synthesizing isobornyl methacrylate by activated carbon supported stannic chloride

A technology of isobornyl methacrylate and methacrylic acid is applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. Overcome the effects of high price, low moisture content and low cost

Inactive Publication Date: 2010-10-20
NANJING FORESTRY UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The current existing synthetic method of isobornyl (meth)acrylate is to adopt purified solid amphene as a raw material direct esterification method. On the one hand, solid amphene is expensive, inconvenient to feed, needs to be broken and pre-dissolved, and is difficult to measure; On the other hand, in the camphene distillation process, because the high-purity camphene is easy to block the pipeline, the distillation process is complicated
[0011] On the one hand, the catalysts currently used are difficult to recover, and there are various disadvantages, and processes such as water washing or even alkali washing are usually required in the aftertreatment process, so it is difficult to prepare isobornyl (meth)acrylate with low moisture content and high purity. product

Method used

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  • Method for catalytically synthesizing isobornyl methacrylate by activated carbon supported stannic chloride
  • Method for catalytically synthesizing isobornyl methacrylate by activated carbon supported stannic chloride
  • Method for catalytically synthesizing isobornyl methacrylate by activated carbon supported stannic chloride

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Experimental program
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Embodiment 1

[0018] 135.00g camphene (purity is 74.1%, 0.735mole) and 82.18g methacrylic acid (0.954mole) are pre-mixed and then added to a 500mL four-necked flask equipped with a thermometer, condenser and mechanical stirrer, followed by adding 17.4g Activated carbon supports tin tetrachloride catalyst and 1.2753g of phenothiazine. After the material is kept at 40°C for 1 hour, the temperature is raised to 60°C, and the reaction is carried out at constant temperature in a water bath for 6h, followed by detection by gas chromatography. After the reaction solution was filtered to remove the catalyst, 0.5g Na 2 CO 3 After stirring for 20 minutes, distill under reduced pressure to distill off unreacted camphene and excess methacrylic acid, and collect fractions at 113-120°C / 6mm Hg. The product yield is 77.4%, the reaction selectivity is 94.3%, and the ester content is 99.5%.

Embodiment 2

[0020] 135.00g camphene (purity is 74.1%, 0.735mole) and 88.50g methacrylic acid (1.028mole) (the molar ratio of camphene and methacrylic acid is 1: 1.4) is mixed in advance, dissolves at room temperature, waits to dissolve completely Finally, it was added to a 500mL four-necked flask equipped with a thermometer, a condenser and a mechanical stirrer, and then 22.3g of activated carbon-supported tin tetrachloride catalyst and 0.9425g of phenothiazine were added. After the material was kept at 40°C for 1 hour, the temperature was raised to 50°C, and the reaction was carried out in a constant temperature water bath for 7 hours, followed by detection by gas chromatography. Add 0.6g Na 2 CO 3 And stir for 20min, steam unreacted camphene and excess methacrylic acid under reduced pressure, collect 113~120 ℃ / 6mm Hg fraction, be isobornyl methacrylate, product yield 83.9%, reaction selection The property is 95.3%, and the ester content is 99.3%.

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Abstract

The invention provides a method for catalytically synthesizing isobornyl methacrylate by activated carbon supported stannic chloride, which is characterized by using isomerized solution obtained by isomerizing alpha-pinene by metatitanic acid as the raw material and using the activated carbon supported stannic chloride as a catalyst, directly esterifying the isomerize solution, the activated carbon supported stannic chloride and (methyl) acrylic acid without additional solvents, filtering the esterified solution to remove the catalyst and then directly distilling the esterified solution without washing to obtain isobornyl acrylate (methyl). The method has the following advantages: the isomerized solution can be directly esterified without being purified and the esterified solution is directly distilled without being washed to obtain isobornyl acrylate (methyl). The synthetic method has the advantages of low energy consumption, low environmental pollution, good isomerization and esterification reaction selectivity, high yield and the like.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing isobornyl methacrylate supported by activated carbon with tin tetrachloride. It belongs to the field of fine chemical technology. Background technique [0002] Isobornyl acrylate and isobornyl methacrylate are abbreviated as IBOA and IBOMA, and their scientific name is 1,7,7-trimethyl-bicyclo[2.1.1]-2-heptyl (meth)acrylate. It is a colorless and transparent liquid, insoluble in water, with extremely low vapor pressure at room temperature and mild odor. It is a very useful special monomer. Due to its unique bridged ring structure, the (meth)acrylate has special physical and chemical properties: low viscosity, high boiling point, low surface tension (low shrinkage), high glass transition temperature, low chroma, high refractive index , Good hydrophobicity, good compatibility with various resins, solvents, pigments and fillers, low toxicity, non-flammable. (Meth)isobornyl acrylate can mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/04B01J27/135
Inventor 王石发汪建新李好瑾徐晓维巍柏松
Owner NANJING FORESTRY UNIV
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