Preparation method of borneol

A production method and borneol technology, which are applied in chemical instruments and methods, preparation of organic compounds, preparation of oxygenated compounds, etc., can solve problems such as harm to workers' health, pollution of the environment by gasoline vapor, loss of people's lives and properties, etc. The effect of reducing material explosion factors, reducing labor intensity and improving production environment

Inactive Publication Date: 2011-06-22
金木集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To this end, enterprises need to invest a lot of manpower, material resources, energy and financial resources to strengthen the ventilation of the crystallization chamber and control the concentration of combustible gases. Once out of control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1, a kind of preparation method of borneol, it comprises the following steps:

[0023] (1) Esterification reaction

[0024] 1. Preparation of catalyst: Take 10kg of titanium dioxide and dry it at 150°C for 6 hours, then lower it to room temperature, then soak it in ferrous sulfate hydrochloric acid aqueous solution for 24 hours, stir it into a sauce and dry it at 90°C , and then dried at a temperature of 200° C. for 24 hours, and the prepared hydrated titanium dioxide catalyst was ready for use.

[0025] 2. Esterification of a_pinene with oxalic acid

[0026] Put 300kg of a_pinene, 9kg of hydrated titanium dioxide catalyst, and 63kg of anhydrous oxalic acid into a 500L reaction tank with stirring, heating device and thermometer, heat up to 50°C, stir for 3.5 hours, then heat up to 60°C, and react for 0.5 hours , heated up to 90°C, and reacted for 0.5 hours. Then filter, the catalyst that is filtered out can be used continuously, and the liquid esterified p...

Embodiment 2

[0038] Embodiment 2, a kind of preparation method of borneol, it comprises the following steps:

[0039] (1) Esterification reaction

[0040] 1. Preparation of catalyst: Take 10kg of titanium dioxide and dry it at 145°C for 6.25 hours, then lower it to room temperature, put it into ferrous sulfate hydrochloric acid aqueous solution and soak it for 23.5 hours, stir it into a sauce and dry it at 80°C , and then dried at a temperature of 190° C. for 24 hours, and the prepared hydrated titanium dioxide catalyst was ready for use.

[0041] 2. Esterification of a_pinene with oxalic acid

[0042] Put 300kg of a_pinene, 9kg of hydrated titanium dioxide catalyst, and 63kg of anhydrous oxalic acid into a 500L reaction tank with stirring, heating device and thermometer, heat up to 53°C, stir for 3 hours, then heat up to 63°C, and react for 0.5 hours , heated up to 87°C, and reacted for 0.5 hours. Then filter, the catalyst that is filtered out can be used continuously, and the liquid est...

Embodiment 3

[0054] Embodiment 3, a kind of preparation method of borneol, it comprises the following steps:

[0055] (1) Esterification reaction

[0056] 1. Preparation of catalyst: Take 10kg of titanium dioxide and dry it at 155°C for 6.5 hours, then lower it to room temperature, then soak it in ferrous sulfate hydrochloric acid aqueous solution for 24.5 hours, stir it into a sauce and dry it at 100°C , and then dried at a temperature of 210° C. for 24 hours, and the prepared hydrated titanium dioxide catalyst was ready for use.

[0057] 2. Esterification of a_pinene with oxalic acid

[0058] Put 300kg of a-pinene, 9kg of hydrated titanium dioxide catalyst, and 63kg of anhydrous oxalic acid into a 500L reaction tank with stirring, heating device and thermometer, heat up to 47°C, stir for 3.5 hours, then heat up to 57°C, and react for 0.5 hours , heated up to 93°C, and reacted for 0.5 hours. Then filter, the catalyst that is filtered out can be used continuously, and the liquid esterif...

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PUM

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Abstract

The invention discloses a preparation method of borneol, which comprises the following steps: preparing a titanium dioxide hydrate catalyst; putting 300 parts of alpha-pinene, 9 parts of titanium dioxide hydrate catalyst and 63 parts of anhydrous oxalic acid into a reaction tank, wherein a stirring and heating device and a thermometer are arranged in the reaction tank; heating to 47-53 DEG C, stirring for 3-4 hours, heating to 57-63 DEG C, reacting for 0.5 hour, heating to 87-93 DEG C, and reacting for 0.5 hour; filtering, wherein the catalyst which is filtered out can be used for subsequent production; washing the liquid esterified substance, which is filtered out, with water, evaporating to remove light oil, and saponifying the evaporated borneol; and after carrying out primary crystallization and secondary crystallization by using a 70-80% ethanol solution, carrying out centrifugal drying, and airing to obtain the finished product. By using ethanol instead of gasoline, the invention lowers the production cost, reduces the environmental pollution and conforms to the industrial policy in China. Meanwhile, the invention shortens the production cycle, lowers the production cost and the labor intensity of the workers, and enhances the labor productivity.

Description

1. Technical field [0001] The invention relates to a method for making ice flakes. 2. Background technology [0002] The current borneol is generally prepared by esterifying a-pinene, boric acid and oxalic acid, and then washing with water, steaming light oil, saponifying brain steaming, coarse crystallization, fine crystallization and drying in the air. The esterification reaction uses boric anhydride as a catalyst to carry out the esterification reaction with a-pinene and oxalic acid. The esterification time is long, requiring 15 hours, the production cycle is long, and the temperature control is extremely strict. Once out of control, improper handling is very serious. It is easy to cause fire and explosion. In the crystallization purification process of crude crystallization and fine crystallization, 120# gasoline is used as the solvent, and the ratio of gasoline to crude brain is 1:1 and 1:1.2, and the two crystallization time is 9 days. High-grade gasoline has high po...

Claims

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Application Information

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IPC IPC(8): C07C35/30C07C27/02C07C27/26B01J21/06
CPCY02P20/584
Inventor 孙国廉钮立强
Owner 金木集团有限公司
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