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A kind of method and equipment for preparing cyclopentanol under supercritical condition

A supercritical, cyclopentanol technology, used in alcoholysis preparation, carboxylate preparation, chemical instruments and methods, etc., to achieve the effect of promoting reaction, improving conversion rate and high atom utilization rate

Active Publication Date: 2021-01-15
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In view of the above problems, the present invention provides a new method suitable for industrialized preparation of cyclopentanol, which overcomes the shortcomings of the prior art indirect hydration method that needs to use concentrated sulfuric acid or other expensive catalysts, while ensuring a higher yield

Method used

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  • A kind of method and equipment for preparing cyclopentanol under supercritical condition
  • A kind of method and equipment for preparing cyclopentanol under supercritical condition
  • A kind of method and equipment for preparing cyclopentanol under supercritical condition

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Experimental program
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Effect test

Embodiment 1

[0054] Experimental device diagram as figure 1 Shown, wherein, high-pressure metering pump 1 is connected with preheater 4, passes into acetic acid aqueous solution A in supercritical pipeline reactor 7; Pass into cyclopentene B in device 7. The high-pressure metering pump 3 is connected to the preheater 6, and the methanol C is heated and mixed with the reaction product at the outlet of the supercritical pipeline reactor 7, and then passed into the supercritical pipeline reactor 8 for reaction. The supercritical pipeline reactor The outlet of 8 is connected to the condenser 9 and the pressure controller 10 in turn, and the other end of the pressure controller 10 sends the material into a processing device (such as a rectifying device) for separation and purification. The operation process is as follows:

[0055] Turn on the high-pressure metering pump 1, pump 90% acetic acid aqueous solution A (mass percentage concentration) with a constant flow rate of 5.49ml / min, turn on t...

Embodiment 2-7

[0057] According to embodiment 1, by changing the flow rate of pump 1 and 3, to change the mol ratio of methyl alcohol, acetic acid and cyclopentene, keep conditions such as residence time, preheater and reactor temperature and reverse pressure constant, after reaction finishes Obtain the following results (Table 1):

[0058] Table 1, the influence of raw material ratio on reaction

[0059]

[0060] The results in Table 1 show that under the excess flow rate ratio of methanol and acetic acid, cyclopentene has a good conversion rate and selectivity, and the increase in the amount of methanol can improve the selectivity to a certain extent, but the amount reaches a certain level After that, the effect on conversion and selectivity is no longer obvious.

Embodiment 8-11

[0062] According to embodiment 1, only change the residence time of reaction, keep conditions such as the flow rate of pump, preheater and reactor temperature and reverse pressure constant, obtain following result (table 2) after reaction finishes:

[0063] Table 2. Effect of residence time on reaction

[0064] Example Residence time / min a

Cyclopentene conversion / % Cyclopentanol selectivity / % 8 10 73.34 96.32 9 15 85.07 96.05 10 25 92.25 93.62 11 30 92.18 92.06

[0065] a Both tube reactors 7 and 8 have the same residence time, which refers to the residence time of a single tube reactor.

[0066] The results in Table 2 show that increasing the residence time increases the conversion of cyclopentene and the selectivity to cyclopentanol.

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Abstract

The invention discloses a method for preparing cyclopentanol in supercritical condition and a device for the same. The method comprises the following steps of taking cyclopentene and an acetic acid aqueous solution as raw materials, in a pipeline reactor, enabling reactants to react to produce cyclopentyl acetate in the supercritical condition, next, enabling the cyclopentyl acetate to generate anester exchange reaction with methanol in the supercritical condition to produce the cyclopentanol, wherein a conversion ratio of the cyclopentanol can reach 92 percent or above; the selectivity of the cyclopentanol reaches 95 percent or above. According to the method, other solvents and catalysts except water do not need to be added; a main by-product methyl acetate produced in a reaction processcan be directly sold to increase profit; further, residual water and methanol can be recovered and used in the same way, and the method has the characteristics of greenness, environmental friendliness, no pollution, high selectivity and the like.

Description

technical field [0001] The invention relates to a method for preparing cyclopentanol by indirect hydration, in particular to a method for preparing cyclopentanol by indirect hydration under supercritical conditions. Background technique [0002] Cyclopentanol is a colorless viscous liquid, soluble in ethanol, slightly soluble in water, and has an aromatic smell. It is mainly used in the production of medicines, dyes and spices. It is an indispensable raw material for the drug cyclopentathiazine for high blood pressure and the new non-barbiturate intravenous anesthetic ketamine, and can also be used as a solvent in the synthesis of drugs and spices. [0003] In nature, cyclopentanol only exists in a small amount of plants and its content is low, so it is difficult to extract. Among many synthesis methods of cyclopentanol, the pyrolysis technology of adipic acid and its derivatives is relatively mature, accounting for more than 90% of the world's total production. The basic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/04C07C69/14C07C29/128C07C35/06C07C67/28B01J19/18B01J19/24
CPCB01J19/1818B01J19/242C07C29/1285C07C67/04C07C67/28C07C69/14C07C35/06Y02P20/54
Inventor 王钰高统海毛建拥彭志国李观兵潘映霞周俊瑶
Owner ZHEJIANG NHU CO LTD