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A kind of method that cyclopentene hydration prepares cyclopentanol

A technology for hydration of cyclopentene and cyclopentanol, which is applied in the preparation of hydroxyl addition, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. The problems such as low rate and unfavorable industrial application can achieve the effect of improving mass transfer rate, low cost and easy operation.

Active Publication Date: 2016-08-03
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above-mentioned method for preparing cyclopentanol by cyclopentene hydration generally has low cyclopentene conversion rate and short operating period of the device.
Although in some technical schemes, the conversion rate of cyclopentene has been limited to a certain extent by adding cocatalysts and / or solvents, the operation process is complicated and the cost is high, which is not conducive to industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0017] The preparation process of titanium-based composite oxide carrier is as follows:

[0018] After preparing the mixed solution of titanium tetrachloride and aluminum nitrate, the mixed solution of titanium tetrachloride and zirconium tetrachloride, gradually drop the potassium hydroxide solution into the above mixed solution, and the reaction time is 4 hours to 20 hours to obtain a white paste Precipitate. Al 2 o 3 -TiO 2 or ZrO 2 -TiO 2 Composite oxide carrier.

[0019] Acid salt of loaded rubidium phosphotungstate (Rb 2.1 h 0.9 PW 12 o 40 ) catalyst preparation method:

[0020] Immerse the above carrier in rubidium carbonate (R b2 CO 3 ) in aqueous solution for 5 hours to 20 hours, the sample was dried at 80°C to 150°C for 3 hours to 12 hours, and then baked at 300°C to 400°C for 3 hours to 10 hours.

[0021] Dip the above roasted sample in phosphotungstic acid (H 3 PW 12 o 40 ) in an aqueous solution for 5 hours to 20 hours, dried at 80°C to 160°C for 5...

Embodiment 7

[0029] According to the method of embodiment 1, the loaded type phosphotungstic acid rubidium acid salt catalyst is prepared, and the catalyst TiO 2 The mass percentage of the titanium-based composite oxide is 40%, and the mass percentage of the active component rubidium phosphotungstic acid salt and the catalyst is 30%.

[0030] When the reaction temperature is 110°C, the reaction pressure is 3.0MPa, and the cyclopentene volume space velocity is 5.5h -1 , Cyclopentene / water (molar ratio) is 4.5:1, and the long-term activity evaluation results of running for 1200 hours are shown in Table 3.

[0031] table 3

[0032] serial number Running time / hour Cyclopentene conversion / % 1 50 39.3 2 100 38.4 3 150 39.5 4 200 37.5 5 250 39.4 6 300 38.8 7 350 39.1 8 400 38.9 9 450 39.5 10 500 38.8 11 550 39.0 12 600 37.9 13 650 39.6 14 700 38.8 15 750 39.1 16 800 38.9 17 850 39.0...

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Abstract

The invention discloses a method for preparing cyclopentanol by hydrating cyclopentene. The catalyst is a titanium-based composite oxide loaded with rubidium phosphotungstic acid salt, the reaction temperature is 90°C-200°C, and the reaction pressure is 1.0MPa- Under the condition of 7.0MPa, cyclopentene and water undergo hydration reaction through a fixed bed reactor, the volume space velocity of cyclopentene is 1.5h-1~18h-1, and the molar ratio of cyclopentene to water is 1.0~10:1 . While the conversion rate of cyclopentene and the selectivity of cyclopentanol are obviously improved, the method has the advantages of simple operation process, easy separation of follow-up products, low cost, suitable for industrial application and the like.

Description

technical field [0001] The invention relates to a method for preparing cyclopentanol by hydrating cyclopentene. Background technique [0002] Cyclopentanol is an important intermediate of fine chemical products, mainly used in the preparation of bromocyclopentane, chlorocyclopentane, etc., and can be used to manufacture antibacterial, antiallergic and other drugs. [0003] Cyclopentanol can be obtained from adipic acid through high-temperature deacidification to obtain cyclopentanone, and then through hydrogenation reaction. However, due to the large amount of pollutants and the restriction of raw material sources, this preparation method is gradually eliminated. In addition, C 5 In the distillate, cyclopentene obtained through separation is used as raw material, and cyclopentanol can also be produced through hydration reaction. There are two main methods of hydration, one is the indirect hydration process, and the other is the direct hydration process. Although the indir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C35/06C07C29/04B01J31/38
CPCB01J27/188C07C29/04C07C2601/08C07C35/06
Inventor 李花伊霍稳周吕清林刘野魏晓霞田丹
Owner CHINA PETROLEUM & CHEM CORP
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