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Catalytic hydrogenation synthesis method for prenyl alcohol

A technology of isopentenol and hydrogenation catalysis, which is applied in the direction of chemical instruments and methods, isomerization preparation, hydroxyl compound preparation, etc., can solve the problems of shortening reaction time, reducing production cost, pollution, etc., and achieves shortening reaction time, The effect of reducing production cost and increasing reaction yield

Inactive Publication Date: 2015-12-23
SHANDONG CHENGTAI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] For above-mentioned defect, the object of the present invention is to provide a kind of hydrogenation catalytic synthesis method of prenol, which can improve the reaction yield and the selectivity of prenol, solve the corrosion and pollution problems that acid catalysis exists, shorten reaction time, reducing production costs

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] The invention provides a hydrogenation catalytic synthesis method of prenol, which comprises the following steps:

[0027] a. Under the action of a solid base catalyst, add paraformaldehyde with a concentration of 93%-97% and tert-butanol as a solvent to the reactor, and then inject nitrogen into the reactor to replace the air in the reactor, and then to the reactor Isobutylene is added to the mixture, after stirring, the reaction temperature is controlled at 180°C to 220°C, the reaction is continued for 3 to 5 hours, and then the cooling discharge distillation is performed;

[0028] b. Collect the prenol obtained by distillation;

[0029] c. Add the 3-methyl-3-butene-l-alcohol obtained by distillation into a fixed bed reactor, and at a temperature of 50℃~100℃, use Se and Ce promoted silica gel supported Pd catalyst to add Hydrogen catalyzed reaction to produce prenol.

[0030] Preferably, the temperature in step c is 70°C.

[0031] Preferably, the reaction kettle is a stainles...

Embodiment 2

[0038] Under the action of a solid catalyst, 95% paraformaldehyde and tert-butanol as a solvent are added to the reactor, nitrogen is injected into the reactor to replace the air in the reactor, and isobutylene is added to the reactor. When the reaction temperature is controlled at 200°C, the reaction is continued for 3 hours to 5 hours, and then the cooling discharge distillation is performed; the isopentenol obtained by the distillation is collected; the 3-methyl-3-butene obtained by the distillation is collected -l-alcohol is added to a fixed-bed reactor, and at a temperature of 50°C, a silica gel supported Pd catalyst promoted by Se and Ce is used to perform a hydrogenation catalytic reaction to obtain prenol.

[0039] Prenol is prepared by the above method. The 3-methyl-3-butene-1-alcohol obtained by distillation is added to a fixed bed reactor. At a temperature of 50°C, the reaction yield is 60%. The enol selectivity is 90%. The reaction yield and the selectivity of prenol...

Embodiment 3

[0041] Under the action of a solid catalyst, 95% paraformaldehyde and tert-butanol as a solvent are added to the reactor, nitrogen is injected into the reactor to replace the air in the reactor, and isobutylene is added to the reactor. When the reaction temperature is controlled at 200°C, the reaction is continued for 3 hours to 5 hours, and then the cooling discharge distillation is performed; the isopentenol obtained by the distillation is collected; the 3-methyl-3-butene obtained by the distillation is collected -l-alcohol is added to a fixed-bed reactor, and at a temperature of 100°C, a silica gel supported Pd catalyst promoted by Se and Ce is used to carry out a hydrogenation catalytic reaction to obtain prenol.

[0042] Prenol is prepared by the above method, and 3-methyl-3-butene-1-alcohol obtained by distillation is added to a fixed bed reactor. At a temperature of 100°C, the reaction yield is 58%. The enol selectivity is 88%. The reaction yield and the selectivity of pr...

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Abstract

The invention provides a catalytic hydrogenation synthesis method for prenyl alcohol. The method comprises the following steps: under the action of a solid base catalyst, adding paraformaldehyde with a concentration of 93 to 97% and tert-butyl alcohol used as a solvent into a reaction vessel, injecting nitrogen into the reaction vessel to replace air in the reaction vessel, then adding isobutene into the reaction vessel, carrying out stirring, then carrying out a continuous reaction at 180 to 220 DEG C for 3 to 5 h and carrying out cooling, discharging and distillation; collecting prenyl alcohol obtained after distillation; and adding 3-methyl-buten-l-ol into a fixed-bed reactor and carrying out catalytic hydrogenation at 50 to 100 DEG C under the catalysis of a silica gel-loaded Pd catalyst promoted by Se and Ce so as to prepare prenyl alcohol. Thus, the method provided by the invention can improve reaction yield and selectivity of prenyl alcohol, overcomes the problems of corrosion and pollution existing in acidic catalysis, shortens reaction time and reduces production cost.

Description

Technical field [0001] The invention relates to the technical field of a synthetic method of prenol, in particular to a method for the hydrogenation catalytic synthesis of prenol. Background technique [0002] Prenol, namely 3-methyl-2-butene-l-alcohol, molecular weight 86.13, density 0.848g / mL (25℃), boiling point 140℃, flash point 43℃, vapor pressure 1.4mmHg (20℃) , It is a colorless and transparent liquid. [0003] Isopentenol is mainly used to synthesize high-efficiency and low-toxic pesticide pyrethroids, polycarboxylic acid water reducer raw materials TPEG, vitamin E, vitamin A, and perfume products citral, etc. With the continuous research on the synthesis of isopentenol With maturity and continuous deepening of application development, the scope of its application in pesticides will continue to expand, and market demand will also rise sharply. Isopentenol is the raw material for the synthesis of pyrethroid, an important precursor of methyl bentine acid. Usually prenol an...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/38B01J27/057
CPCC07C29/38B01J27/0573C07C29/56C07C33/025C07C33/03
Inventor 张国华姜立新李源明张培丽宋峰
Owner SHANDONG CHENGTAI CHEM IND
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