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Continuous production method for isobornyl methacrylate

A technology of isobornyl methacrylate and methacrylic acid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of high prices of borneol and isobornyl, reduced value of atomic utilization, and environmental pollution Large and other problems, to achieve the effect of high utilization rate of raw materials, reduction of side reactions, and low reaction temperature

Inactive Publication Date: 2018-08-17
安徽联化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the shortcomings of borneol and isoborneol with high prices and few sources, there is also a by-product H 2 On the one hand, the generation of O or methanol leads to a decrease in the use value of atoms; on the other hand, the release of methanol will cause greater environmental pollution, and the generation of water will increase the moisture content in the product

Method used

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  • Continuous production method for isobornyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Such as figure 1 Shown, a kind of continuous production method of isobornyl methacrylate comprises the following steps: (1) methacrylic acid and refined camphene are dropped into reactor, dissolve at room temperature, and add a certain amount of polymerization inhibitor after completely dissolving Agent and catalyst, heated to 60 degrees Celsius to react, no heat is released during the reaction, after 3 hours of reaction, stop the reaction, filter and recover the catalyst to obtain the reaction mixture, temporarily store the reaction mixture in the semi-finished temporary storage tank;

[0022] (2) In the treated reaction mixture, add a polymerization inhibitor, then pump it into a short-path still and steam excess methacrylic acid and unreacted camphene under a negative pressure of 0.01MPa. Collect the distillate at 113-120°C under 0.6kPa, then wash the distillate through water to remove the acid liquid in it, and control the acidity of the product at 0.05, which is is...

Embodiment 2

[0027] Produce isobornyl methacrylate with the method of embodiment 1, difference is only: methacrylic acid and amphene react 4h at 50 ℃, the mass ratio of methacrylic acid and amphene is 5:11, catalyst ferric chloride The addition amount of the polymerization inhibitor ZJ-705 is 0.2wt% of the total weight of methacrylic acid and amphene, and the addition amount of the polymerization inhibitor ZJ-705 is 0.3wt% of the total weight of methacrylic acid and amphene.

Embodiment 3

[0029] Isobornyl methacrylate is produced by the method of Example 1, the difference is only: methacrylic acid and amphene are reacted at 70°C for 2h, the mass ratio of methacrylic acid and amphene is 9:11, and the catalyst ferric chloride The addition amount of the polymerization inhibitor ZJ-705 is 0.4wt% of the total weight of methacrylic acid and amphene, and the addition amount of the polymerization inhibitor ZJ-705 is 0.5wt% of the total weight of methacrylic acid and amphene.

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Abstract

The invention discloses a continuous production method for isobornyl methacrylate. The method comprises the following steps: (1) putting methacrylic acid and camphene into a reaction kettle, after themethacrylic acid and the camphene are completely dissolved at room temperature, adding a polymerization inhibitor and a catalyst, performing a reaction, and performing filtration to obtain a reactionmixed liquid; (2) replenishing a polymerization inhibitor into the reaction mixed liquid, performing distillation to obtain unreacted methacrylic acid and camphene under negative pressure of 0.01-0.05 MPa, and collecting a fraction at the temperature of 113-120 DEG C and pressure of 0.6 kPa to obtain the isobornyl methacrylate; (3) putting the unreacted methacrylic acid and camphene into a secondary reaction kettle, performing a reaction, and performing filtration to obtain a secondary reaction mixed liquid; and (4) performing the step (2) and the step (3) on the secondary reaction mixed liquid repeatedly in sequence to realize continuous production of the isobornyl methacrylate. The method disclosed by the invention has the advantages of having a high utilization ratio of raw materials,reducing loss of the raw materials, improving a conversion rate of the raw materials, and improving product quality.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, more specifically to a continuous production method of isobornyl methacrylate. Background technique [0002] Isobornyl methacrylate is a special ester of methacrylic acid. It has carbon-carbon double bonds and special isobornyl alkoxy groups. It has a higher T value than hydroxyalkyl acrylate and can be polymerized with many other monomers to form properties. Excellent polymer, also because of its large refractive index, can be used as optical resin. [0003] The main synthetic route of isobornyl methacrylate is the isobornyl route. The isoborneol route uses isoborneol as a raw material and includes direct esterification and transesterification. Due to the shortcomings of borneol and isoborneol with high prices and few sources, there is also a by-product H 2 On the one hand, the generation of O or methanol leads to a reduction in the utilization value of atoms; on the other h...

Claims

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Application Information

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IPC IPC(8): C07C67/04C07C69/54
CPCY02P20/584C07C67/04C07C2602/42C07C69/54
Inventor 蒋梅芳
Owner 安徽联化新材料有限公司
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