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Method for preparing guaiacol

A technology of guaiacol and reaction, which is applied in the field of guaiacol preparation, can solve the problems of difficult development of matching technology, high price of catechol, expensive life of catalyst, etc., to achieve improved product selectivity and low cost , The effect of low production cost

Active Publication Date: 2014-04-09
WANHUA CHEM GRP CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the price of catechol is high, the catalyst is expensive and has a short life, and it needs to be regenerated frequently, and it is difficult to develop supporting technologies
There are difficult problems in the existing production process of guaiacol, so a greener and more efficient solution is urgently needed

Method used

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  • Method for preparing guaiacol
  • Method for preparing guaiacol
  • Method for preparing guaiacol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]Preparation of supported solid acid catalyst: dissolving stannous chloride and / or niobium oxalate, bismuth nitrate, zirconium nitrate in 0.05mol / L dilute nitric acid solution respectively to obtain active component solution, the mass concentration of above-mentioned active component solution is 10 %, prepare aluminum nitrate into an aqueous solution with a mass concentration of 30%, mix the active component solution and aluminum nitrate solution evenly according to the ratio in Table 1, stir, and slowly add 25% ammonia water with the same mass as the active component solution at 70°C As a precipitating agent, it was added dropwise for 1 hour. After the dropwise addition, it was filtered and washed until the pH of the washing liquid was neutral, dried, and roasted at 773K for 6 hours. Catalyst raw powders loaded with different active components and different loads are prepared. The molded catalyst was obtained by extruding, and the active components and contents of the ca...

Embodiment 2

[0047] Dehydrogenation catalyst preparation:

[0048] Using the method of excessive volume impregnation, add a certain amount of light silicon dioxide and 300g water to the 5L round bottom flask, gradually add nickel nitrate, K 2 CO 3 , stannous chloride, stirred at 80°C for 3h, dried at 120°C for 12h after stirring, roasted at 400°C for 6h, extruded into a 3*3mm columnar catalyst, packed into a fixed bed reactor, 350°C, H 2 After reduction for 6 hours, the activated catalyst was obtained. The specific composition of the obtained dehydrogenation catalyst is shown in Table 2.

[0049] Table 2 Composition of different dehydrogenation catalysts

[0050]

[0051]

Embodiment 3

[0053] Ring-opening reaction of epoxycyclohexane alcohol: put epoxycyclohexane and methanol in a certain proportion, respectively, through the In a fixed-bed reactor for decomposing the catalyst, the reaction is continued under the protection of an inert gas. After the reaction is completed, methanol is distilled off under reduced pressure at a pressure of 0.2 bar, and o-methoxycyclohexanol is obtained at the bottom of the kettle; o-methoxycyclohexanol Dehydrogenation reaction: o-methoxycyclohexanol is diluted with nitrogen and passed through the 2 The fixed-bed reactor of activated dehydrogenation catalyst bed, the crude product adopts batch rectification process under normal pressure, and the theoretical plate number of rectification tower is 30, and first rectification extracts a small amount of by-product components, and the temperature of tower still 200°C, tower top temperature 170°C, pressure 0.1MPa, reflux ratio 1:1, to obtain a small amount of cyclohexanone, o-methoxy...

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Abstract

The invention discloses a method for preparing guaiacol. The method comprises two steps of firstly, putting cyclohexene oxide and methyl alcohol into a fixed bed reactor with supported solid acid catalyst according to a certain proportion, continuously reacting under inert gas protection so as to obtain o-methoxyl cyclohexanol; secondly, diluting the o-methoxyl cyclohexanol with inert gas, then passing through a dehydrogenation catalyst bed activated by H2, rectifying a coarse product so as to obtain the guaiacol. The method has the characteristics that the raw material has low cost, atom economy is high, yield of the product is high, and the separation technology is simple.

Description

technical field [0001] The invention relates to a preparation method of guaiacol, in particular to a two-step process for catalyzing the reaction of epoxycyclohexane and methanol and further dehydrogenating to prepare guaiacol. Background technique [0002] Guaiacol, also known as o-hydroxyanisole, o-hydroxyanisol, and methylcatechol, is an important fine chemical intermediate in industries such as spices, medicine, agriculture, and dyes. body. [0003] The biggest use of guaiacol is to produce vanillin, which is a precious broad-spectrum high-grade spice, which can be widely used as a deodorant, flavor-changing agent and flavoring agent in cosmetics, soaps, cakes, candies, beverages , tobacco and baked goods industries. [0004] As an important intermediate in organic synthesis, guaiacol can also be used to produce potassium guaiacol sulfonate, an expectorant and antitussive agent, and 5-nitroguaiacol sodium, a high-efficiency plant growth regulator. [0005] In addition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/18
CPCC07C41/03C07C41/18C07C2601/14C07C43/23C07C43/196
Inventor 陈海波李俊平李静黎源华卫琦丁建生
Owner WANHUA CHEM GRP CO LTD
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