A method for producing isoborneol

Abstract

The invention provides an isoborneol production method which is carried out in a reinforced radial flow reaction system (IRR) composed of a liquid flow reinforced immersed fixed bed reactor. The isoborneol production method comprises the following steps: mixing the raw materials and a composite solvent by adopting a certain quantity of composite solid acid catalyst according to a certain ratio, wherein camphene and water are used as the raw materials; carrying out hydration reaction in an IRR reaction-separation system to obtain an isoborneol product. The reaction temperature is 40-90 DEG C, the mass of the catalyst is 15-50% of the total mass of the firstly-filled liquid material, the ratio of the camphene to the water to the composite solvent is 1:(0.15-2):(0.5-4), the reaction pressure is 0.1-0.3MPa, and the reaction standing time is 40-70min. After the reacted materials are separated and subjected to ion exchange, the solvent and the unreacted materials are returned to the reactor, and the product is stored. The isoborneol production method has the advantages that the industrial reliability is good, the per-pass conversion rate of the camphene is high, the isoborneol is good in selectivity, and the energy consumption per unit product is only about 60% of that of the traditional fixed bed process.

Description

field of invention [0001] The invention relates to a method for producing isoborneol. Background technique [0002] Isoborneol, also known as isoborneol, is a white translucent crystal with a special odor. It is an isomer of borneol, and its molecular formula is C 10 h 18 O, molecular weight 154.25, melting point 208-214°C. Isoborneol is an intermediate in the synthesis of camphor, and it is also widely used in the fields of spices and medicine. [0003] At present, the synthesis method of isoborneol in industry mainly contains two kinds of processes: indirect method and direct method: [0004] The first is the esterification reaction of amphene and acetic acid to generate isoborneol acetate, which is then saponified to generate isoborneol; the second is the direct hydration of amphene under the action of an acidic catalyst to generate isoborneol. The indirect method is relatively mature, but the process is complicated and the consumption of raw materials is high; althou...

AI Technical Summary

Problems solved by technology

[0005] Chinese patent CN1408696A discloses a method for preparing isoborneol by one-step hydration of sulfuric acid as a catalyst, using a stirred tank reactor. This method simplifies the synthesis steps and reduces the amount of raw materials used, but due to the strong corrosion of sulfuric acid, the material of the equipment The requirements are high, and the subsequent separation is difficult, which is easy to cause pollution to the environment

Although this method has a higher conversion rate of camphene and the selectivity of isoborneol, the reaction time is long, the energy consumption is high, and the structure and composition of natural mordenite are greatly affected by the place of production, and the instability and fluctuation of its performance will lead to production is difficult to stabilize

In addition, the continuous separation and circulation reactor needs to add a large amount of solvent, the operation is complicated, the reaction time is long, and the actual production cost of the industry will be relatively high.

[0008] Chinese patent CN101973851A discloses a method for synthesizing isoborneol using synthetic molecular sieves as a catalyst. A fixed bed reactor is used to react at a reaction temperature of 120-180°C. The conversion rate of camphene is 80%-90%, and that of isoborneol is The selectivity is 73.3%-86.4%. This method does not use solvents, which is environmentally friendly and reduces the difficulty of separation in the downstream section. However, the reaction temperature is high, the selectivity is low, and the industry will also cause high production costs.

[0009] In addition, Chinese patent CN203112713U also discloses a reaction device for producing isoborneol by hydration of amphene. Compared with the traditional amphene hydration reaction and separation device, the device adds a membrane separation device between the fixed bed reactor and the separation system. , the device can concentrate the reaction liquid, increase the content of isoborneol, and reduce the subsequent energy consumption, but because the product mixture usually contains a small amount of fine catalyst particles, they are very easy to cause blockage to the separation membrane material and components, so the industrial practice Trouble occurs when applying

Images