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Method of preparing tetrahydrobicyclo pentadiene by continuous hydrogenation of bicyclopentadiene

A technology of tetrahydrodicyclopentadiene and dicyclopentadiene is applied in the field of continuous hydrogenation of dicyclopentadiene to produce tetrahydrodicyclopentadiene, and can solve the problem of reducing the yield of target product, catalyst deactivation and cooling uniformity Restrictions and other problems, to achieve the effects of easy reaction, improved reaction yield, and uniform temperature

Inactive Publication Date: 2007-02-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of installing a heat exchange device in the hydrogenation reactor is used to remove the heat of reaction generated during the hydrogenation of (bis)cyclopentadiene. The disadvantage is that the uniformity of cooling in the reactor is limited to a certain extent.
It is speculated that there is still a local excessive temperature rise in the catalyst bed, which causes partial catalyst deactivation, which will reduce the yield of the target product

Method used

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  • Method of preparing tetrahydrobicyclo pentadiene by continuous hydrogenation of bicyclopentadiene
  • Method of preparing tetrahydrobicyclo pentadiene by continuous hydrogenation of bicyclopentadiene
  • Method of preparing tetrahydrobicyclo pentadiene by continuous hydrogenation of bicyclopentadiene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~8

[0017] The process flow of each embodiment of the present invention is shown in the drawings. The reactor 1 is a fixed bed reactor, and a venturi ejector 2 is installed on the top of the reactor. The raw material dicyclopentadiene M1, the solvent M2 and the external circulation reaction liquid M4 enter the raw material blending tank for mixing. The liquid phase material from the raw material blending tank and the raw material hydrogen M3 are fully mixed and atomized into a mist-like gas-liquid mixture in the Venturi injector 2 and then pass through the fixed-bed catalyst bed for hydrogenation reaction. The reaction liquid from the reactor enters the reaction liquid storage tank 4, and then passes through the external circulation heat exchanger for heat exchange and cooling. The cooled reaction liquid is divided into two parts, one is the external circulation part M4, the other is the discharge M5, M4 returns to the raw material blending tank 3, and M5 enters the product storage ta...

Embodiment 9

[0020] Except that cyclopentane is used as the solvent, the rest are the same as in Examples 1-8, and other process conditions are listed in Table 1.

Embodiment 10

[0022] Except that cyclohexane is used as the solvent, the rest are the same as in Examples 1-8, and other process conditions are listed in Table 1.

[0023] The reaction results of each example are shown in Table 2.

[0024] DCPD / solvent

(weight ratio)

DCPD / H 2

(mol ratio)

Reaction pressure

(MPa)

temperature reflex

(℃)

Catalyst load

(hr -1 )

M5 / M4

(weight ratio)

Example 1

1∶5

1∶3.7

1.2

182

2.0

1∶5

Example 2

1∶6

1∶3.2

1.2

165

2.5

1∶5

Example 3

1∶7

1∶3.2

0.9

120

2.5

1∶6

Example 4

1∶8

1∶4.3

1.5

139

2.5

1∶8

Example 5

1∶8

1∶3.4

1.2

154

2.5

1∶7

Example 6

1∶8

1∶5.0

1.2

122

3.5

1∶8

Example 7

1∶8

1∶3.0

1.2

110

4.0

1∶8

Example 8

1∶10 ...

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PUM

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Abstract

The continuous dicyclopentadiene hydrogenating process to prepare tetrahydro dicyclopendiene is one continuous catalytic hydrogenation reaction of the mixture of dicyclopentadiene, solvent and hydrogen in a fixed bed catalyst bed. The catalyst includes gamma-Al2O3 as carrier and Pa as active component. The solvent is any one of cyclopentane, n-hexane, cyclohexane, benzene, toluene, cyclohexane, ethanol, methanol, and tertiary butyl alcohol. The reacted liquid is discharged partially and externally circulated partially with the weight ratio being 1 to 5-12, and the externally circulated liquid after being cooled is mixed with dicyclopentadiene material and solvent before being mixed with hydrogen in venturi ejector, atomized into gas-liquid mixture and reacted in the catalyst bed. The catalyst load is 2.0-4.0 / hr accounted in liquid phase material, and the reacted heat is transferred via external circulation. The present invention has high tetrahydro dicyclopendiene.

Description

Technical field [0001] The invention relates to a method for preparing tetrahydrodicyclopentadiene by hydrogenating dicyclopentadiene. Background technique [0002] Tetrahydrodicyclopentadiene is a solid high-energy fuel with excellent performance. Based on it, a series of valuable dicyclopentadiene derivatives with tricyclodecane structure can be prepared. After the isomerization of tetrahydrodicyclopentadiene into hanging tetrahydrodicyclopentadiene, it can be used as an excellent liquid high-energy fuel, which has important uses in the aerospace field; reaction under different isomerization conditions can obtain another A kind of isomer-adamantane, adamantane has a wide range of uses and extremely high added value, so it is known as a new generation of fine chemical raw materials. In the prior art, the method of producing tetrahydrodicyclopentadiene by hydrogenation of dicyclopentadiene has the most industrial application prospects. Since the hydrogenation reaction of dicyclop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/15C07C5/03
Inventor 周飞郭世卓范存良顾超然
Owner CHINA PETROLEUM & CHEM CORP
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