A kind of preparation method of cyclohexyl methacrylate

A technology of methacrylic acid and cyclohexyl ester, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low conversion rate, achieve improved conversion rate, increase conversion rate, and facilitate operation Effect

Active Publication Date: 2017-02-22
ANQING FEIKAI NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] In the process of realizing the present invention, the inventor has found that there are at least the following problems in the prior art: the existing industrial method for preparing cyclohexyl methacrylate only relies on organic solvents to take the water generated in the esterification reaction out of the reaction system, low conversion rate

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  • A kind of preparation method of cyclohexyl methacrylate

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preparation example Construction

[0043] Above-mentioned preparation method comprises the following steps:

[0044] Step (1), adding cyclohexanol, methacrylic acid, solvent, catalyst and polymerization inhibitor to the reactor;

[0045] In step (2), the reaction system obtained in step (1) is heated to a constant temperature after reflux; during the reaction, an oxygen-containing gas is introduced into the reaction system; wherein, the flow rate of the oxygen-containing gas in the late stage of the reaction is greater than that in the early stage of the reaction The flow rate of the oxygen-containing gas, the early stage of the reaction is within 5-8 hours of the beginning of the reaction, and the late stage of the reaction is 5-8 hours after the reaction to the end of the reaction;

[0046] In step (3), after the reaction is completed, the reaction system is cooled, and the cyclohexyl methacrylate product is obtained through neutralization, washing, and vacuum distillation.

[0047]The esterification reactio...

Embodiment 1

[0075] The preparation method of cyclohexyl methacrylate in the present embodiment is as follows:

[0076]Step (1), add 100.0Kg cyclohexanol, 160.0Kg methacrylic acid (the mole of cyclohexanol and methacrylic acid) successively in the reactor that thermometer, water separator, cooling tower, stirring paddle and ventilation pipe are equipped with The ratio is 1:1.8), 64.0Kg cyclohexane, 4.05Kg solid superacid 4.05Kg p-toluenesulfonic acid, 1.725Kg p-hydroxyanisole, 3.61Kg hypophosphorous acid, and add 41.6Kg cyclohexane in the water separator.

[0077] Step (2), under the atmosphere of the mixed gas of compressed air and nitrogen (compressed air: nitrogen = 1:2, volume ratio, the same below), turn on the heating device, control the reaction temperature at 70°C to reflux the reaction system; The flow rate is kept at 1.0m in the first 5 to 6 hours of the reaction 3 / h, then keep at 2.0m until the end of the reaction 3 / h; titrate the acid value with KOH standard solution to 9...

Embodiment 2

[0084] The preparation method of cyclohexyl methacrylate in the present embodiment is as follows:

[0085] Step (1), add 100.0Kg cyclohexanol, 110.0Kg methacrylic acid (the mole of cyclohexanol and methacrylic acid) successively in the reactor that thermometer, water separator, cooling tower, stirring paddle and ventilation pipe are equipped with The ratio is 1:1.3), 40.0Kg toluene, 55Kg cyclohexane, 4.05Kg solid superacid 4.05Kg p-toluenesulfonic acid, 1.725Kg copper sulfate pentahydrate, 2.51Kg p-hydroxyanisole, and add 14.2Kg toluene and 27.4Kg cyclohexane into the water separator.

[0086] Step (2), under the atmosphere of the mixed gas of compressed air and nitrogen (compressed air: nitrogen = 1:1.5), turn on the heating device, control the reaction temperature at 60°C to reflux the reaction system, and the flow rate of the mixed gas is within 5 minutes of the beginning of the reaction. ~ 6 hours to maintain at 1.0m 3 / h, then keep at 3.0m until the end of the reaction...

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Abstract

The invention discloses a preparation method of cyclohexyl methacrylate, belonging to the technical field of preparation of fine chemicals. The method comprises the following steps: adding cyclohexanol, methacrylic acid, a solvent, a catalyst and a polymerization inhibitor into a reaction kettle, heating the obtained reaction system to a reflux state, and keeping the temperature constant; introducing oxygen-containing gas into the reaction system in the reaction process, wherein the flow rate of the oxygen-containing gas in the later reaction period is greater than that of the oxygen-containing gas in the early reaction period, the early reaction period is within 5-8 hours after the reaction starts, and the later reaction period is after 5-8 hours of the reaction to the end of the reaction; and after the reaction finishes, neutralizing, washing, and carrying out reduced pressure distillation to obtain the cyclohexyl methacrylate product. According to the preparation method, different flow rates of the oxygen-containing gas are introduced in different stages of esterification reaction, and water generated in the reaction process is maximally taken out of the reaction system, thereby enhancing the conversion rate; and a simple separation purification technique can be performed to obtain the high-purity low-chroma product.

Description

technical field [0001] The invention relates to the technical field of preparation of fine chemicals, in particular to a preparation method of cyclohexyl methacrylate. Background technique [0002] Cyclohexyl methacrylate is an acrylic resin monomer, its refractive index is 1.4598, its molecular weight is 168.23, and its appearance is colorless or light yellow liquid. Polymers based on cyclohexyl methacrylate have good flexibility and very large refractive index. The main uses of cyclohexyl methacrylate are: modifier of resin for paint, raw material of resin for synthetic prism, lens and other optical materials, modifier of resin for colorant and toner, resin for adhesive, The raw material of tooth resin and the production of information recording disks. [0003] At present, the main method of industrial synthesis of cyclohexyl methacrylate is: take methacrylic acid and cyclohexanol as raw materials, carry out esterification reaction in organic solvent under the catalysis ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/54C07C67/08
CPCC07C67/08C07C67/54C07C67/62C07C69/54
Inventor 查文平谭鹏程为中吕亮王子凡
Owner ANQING FEIKAI NEW MATERIAL CO LTD
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