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Method for synthesizing guaiacol

A technology of guaiacol and catechol, applied in chemical instruments and methods, dehydration of hydroxyl-containing compounds to prepare ethers, metal/metal oxide/metal hydroxide catalysts, etc., can solve large environmental pollution and useless substances , Vanillin quality impact and other issues

Active Publication Date: 2007-12-05
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods of domestic industrialization are mainly anthranil (ethyl) ether method and catechol-chloroethyl (methane) method, but these two methods all have high production costs, large environmental pollution and production process Shortcomings such as a large amount of useless substances, and the chlorine in the catechol-chloroethyl (methane) method raw material also has a greater impact on the quality of the product vanillin

Method used

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  • Method for synthesizing guaiacol
  • Method for synthesizing guaiacol
  • Method for synthesizing guaiacol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The catalyst of the present invention is ammonium metatungstate supported on silica, prepared by traditional impregnation method, a certain amount of ammonium metatungstate aqueous solution (or other active component aqueous solution) is impregnated in the formed 40-60 mesh commercial carbon dioxide On silicon particles, dry, and bake at 533-733K for 3 hours. The content of tungsten is 7.9% of the total mass of the catalyst (based on tungsten content).

Embodiment 2

[0033] The catalyst of the invention is used for the gas-solid phase alkylation reaction of catechol and methanol to synthesize guaiacol.

[0034] The device used in the reaction is shown in Figure 1, among the figure 1 nitrogen cylinder, 2 steady flow valves, 3 rotameters, 4 and 7 thermocouples, 5 and 8 reaction tubes, 6 and 10 heating furnaces, 9 catalyst beds, 11 Collection bottles, 12 cold traps, 13 and 14 programmed temperature controllers, 15 SY-04 sampling pumps.

[0035] During the reaction, the reaction temperature is 533K, the flow rate is 0.5mL / h, the catalyst is 1.4g, and the ratio of catechol to methanol is 1 / 5 (mol).

Embodiment 3

[0045] The lifetime of the catalyst was investigated as described in Example 2.

[0046] Test result analysis example 1

[0047] Table 1 has listed comparative example 1-6 and the catalytic activity comparison that the prepared catalyst of embodiment 1 carries out by embodiment 2, visible C, SiO 2 and TiO 2 When used as a carrier, the activity is higher, among which SiO 2 The activity is the best when used as a carrier.

[0048] Table 1 Reaction performance of ammonium metatungstate supported on different carriers

[0049]

[0050] m cat =1.4g, catechol / methanol=1 / 5 (mol), flow velocity=0.5mL / h, reaction temperature=533K, reaction time=3-4h; W content=7.9wt.%

[0051] Test result analysis example 2

[0052] Table 2 lists the catalytic activity comparisons of the catalysts prepared in Comparative Examples 7-10 and Example 1 according to Example 2. It can be seen that the activity is the best when the tungsten loading is 7.9%.

[0053] Table 2 SiO 2 Reaction pe...

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Abstract

The present invention is process of synthesizing guaiacol, and relates to the application of catalyst in catalytically synthesizing guaiacol through the solid phase alkylation reaction between catechol and methanol. The catalyst has active component of ammonium metatungstate, sodium tungstate, ammonium molybdenum, ammonium biphosphate, ammonium phosphate, ammonium chromate or silicotungstic acid; and carrier of active carbon, SiO2, ZnO, Al2O3, TiO2, BaCO3 or CaO; and active component supporting amount of 2.1-30.2 wt%. The process of synthesizing guaiacol has catalytic reaction temperature of 533-573 K, the molar ratio between catechol and methanol of 1 / 7-1 / 2.5, and catalyst amount of 0.84-2.8 weight portions. During the process, the mixed solution of catechol and methanol is fed to the pre-heater in the flow rate of 0.3-2ml / hr, gasified and reacted catalytically at the temperature of 533-573 K.

Description

technical field [0001] The invention relates to a synthesis method of guaiacol, in particular to the application of a catalyst in the gas-solid phase alkylation reaction of catechol and methanol to catalyze the synthesis of guaiacol. Background technique [0002] O-alkoxyphenol is an important fine chemical intermediate, especially guaiacol (also known as o-hydroxyanisole or o-methoxyphenol) and ethyl wood phenol (also known as o-hydroxyanisole or o-ethoxy Phenol) is an important fine chemical intermediate in industries such as spices, medicine, agriculture, and dyes. [0003] Among many applications, the most important use of guaiacol and ethyl xylin is in the synthesis of vanillin. Vanillin is a precious broad-spectrum high-grade spice. As a spice additive, it is favored by the international spice industry for its small amount of addition and unique aroma. Its demand is increasing at a rate of 10% per year. Become a tight chemical. Vanillin is also widely used in fixati...

Claims

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Application Information

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IPC IPC(8): C07C41/09C07C43/23B01J23/30B01J23/28B01J27/16B01J27/18
Inventor 张文祥贾明君陈继新朱小梅郭双龙邹秀晶苑冰李雪梅王芳盛光
Owner BC P INC CHINA NAT PETROLEUM CORP
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