CN215162250U - Device of cyclohexene preparation methyl cyclopentane - Google Patents

Device of cyclohexene preparation methyl cyclopentane Download PDF

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CN215162250U
CN215162250U CN202121136676.5U CN202121136676U CN215162250U CN 215162250 U CN215162250 U CN 215162250U CN 202121136676 U CN202121136676 U CN 202121136676U CN 215162250 U CN215162250 U CN 215162250U
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cyclohexene
reactor
valve
pipe
hydrogenation
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CN202121136676.5U
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陈恩之
苗迎彬
郭正谦
赵培朝
朱伸兵
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Chongqing Huafeng New Material Research Institute Co ltd
Chongqing Huafeng Polyamide Co ltd
CHONGQING HUAFON CHEMICAL CO LTD
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Chongqing Huafeng New Material Research Institute Co ltd
Chongqing Huafeng Polyamide Co ltd
CHONGQING HUAFON CHEMICAL CO LTD
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Abstract

The utility model provides a device of methyl cyclopentane is prepared to cyclohexene, including at least one cyclohexene reactor, the rectifying column, hydrogenation ware, set up the agitator in the cyclohexene reactor, the feed inlet of cyclohexene reactor is used for linking to each other with the cyclohexene source, the bin outlet of cyclohexene reactor links to each other with the rectifying column through the blow-off pipe, be equipped with first valve on this blow-off pipe, the top of the tower discharge outlet of rectifying column is through the condenser, the back flow links to each other with the flow return of rectifying column, set up the backwash pump on this back flow, set up the second valve on the back flow, and be located the low reaches of backwash pump, the liquid phase feed inlet of hydrogenation ware passes through the inlet pipe and links to each other with the back flow, be located between backwash pump and the second valve, set up the third valve on the inlet pipe, the gaseous phase feed inlet of hydrogenation ware is located the top of hydrogenation ware, the bin outlet of hydrogenation ware is located the bottom of hydrogenation ware. The utility model discloses simple structure, operating method utilize the extensive cyclohexene in source to prepare methyl cyclopentane, effectively satisfy the actual demand of enterprise.

Description

Device of cyclohexene preparation methyl cyclopentane
Technical Field
The utility model relates to a chemical industry field, in particular to device of cyclohexene preparation methyl cyclopentane.
Background
Methylcyclopentane is an organic compound and is a colorless transparent liquid at normal temperature and pressure. Mainly used as reagents and chemical synthesis raw materials.
The existing industrial production of methylcyclopentane is mainly C in the refining industry6Obtained by further catalytic reaction and rectification, has long process flow, expensive catalyst and complex reaction product.
Therefore, how to design a method for producing methylcyclopentane with simple process and mild reaction is an urgent problem to be solved by those skilled in the art.
Disclosure of Invention
The utility model aims at prior art not enough, provide a device of cyclohexene preparation methyl cyclopentane, its simple structure, operation method, the extensive cyclohexene in usable source prepares methyl cyclopentane, effectively satisfies the actual demand of enterprise.
Realize the technical scheme of the utility model is that: the utility model provides a device of cyclohexene preparation methyl cyclopentane, includes at least one cyclohexene reactor, at least one rectifying column, at least one hydrogenation ware, set up the agitator in the cyclohexene reactor, the feed inlet of cyclohexene reactor is used for linking to each other with the cyclohexene source, the bin outlet of cyclohexene reactor links to each other with the rectifying column through arranging the material pipe, is equipped with first valve on this row of material pipe, the top of the tower bin outlet of rectifying column through condenser, back flow with the backward flow mouth of rectifying column links to each other, sets up the backwash pump on this back flow, sets up the second valve on the back flow, and is located the low reaches of backwash pump, the liquid phase feed inlet of hydrogenation ware passes through the inlet pipe and links to each other with the back flow, is located between backwash pump and the second valve, sets up the third valve on the inlet pipe, the gaseous phase feed inlet of hydrogenation ware is located the top of hydrogenation ware for link to each other with the hydrogen source, the discharge outlet of the hydrogenation reactor is positioned at the bottom of the hydrogenation reactor.
Further, the rectifying towers are connected in parallel and/or in series.
Furthermore, a material outlet at the bottom of the rectifying tower is connected with a material inlet of the cyclohexene reactor through a circulating pipeline, and the circulating pipeline is provided with a circulating pump.
Furthermore, a fourth valve is arranged on the circulating pipeline and is positioned at the downstream of the circulating pump.
Preferably, the return pipe is provided with a return tank which is positioned at the upstream of the return pump.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the device for preparing methylcyclopentane from cyclohexene comprises at least one cyclohexene reactor, at least one rectifying tower and at least one hydrogenation reactor, wherein the cyclohexene reactor is used for enabling added cyclohexene to react and isomerize under the action of a molecular sieve catalyst to generate methylcyclopentene, the rectifying tower is used for separating to obtain the methylcyclopentene, and the hydrogenation reactor is used for enabling the added methylcyclopentene to react with hydrogen under the action of a hydrogenation catalyst to generate the methylcyclopentane. The stirrer is arranged in the cyclohexene reactor, and a feed inlet of the cyclohexene reactor is used for being connected with a cyclohexene source, so that the raw material cyclohexene and the molecular sieve catalyst are uniformly mixed. The discharge port of the cyclohexene reactor is connected with the rectifying tower through a discharge pipe, and the discharge pipe is provided with a first valve for discharging the generated mixture into the rectifying tower. The top discharge opening of rectifying column through condenser, back flow with the reflux opening of rectifying column links to each other, sets up the backwash pump on this back flow, sets up the second valve on the back flow, and is located the low reaches of backwash pump, and after the vapour phase methyl cyclopentane that the rectifying column separation obtained was the liquid through the condensation, partly backward flow can effectively improve the purity of the vapour phase methyl cyclopentane that the separation obtained. The liquid phase feed inlet of the hydrogenation reactor is connected with the return pipe through a feed pipe and is positioned between the return pump and the second valve, the feed pipe is provided with a third valve, and the purpose of controlling the return ratio is realized by controlling the opening degree of the second valve and the third valve. The gas phase feed inlet of the hydrogenation reactor is positioned at the top of the hydrogenation reactor and is used for being connected with a hydrogen source, the discharge outlet of the hydrogenation reactor is positioned at the bottom of the hydrogenation reactor, liquid methylcyclopentane entering the hydrogenation reactor and gaseous hydrogen react under the action of a hydrogenation catalyst to generate target product methylcyclopentane, the target product methylcyclopentane is discharged from the bottom of the hydrogenation reactor, the hydrogen is prevented from being discharged, and the production safety can be effectively ensured on the basis of obtaining the target product.
2. The discharge outlet at the bottom of the rectifying tower is connected with the feed inlet of the cyclohexene reactor through a circulating pipeline, the circulating pipeline is provided with a circulating pump, the bottom of the rectifying tower is a mixture containing cyclohexene and a molecular sieve catalyst, the mixture is injected into the cyclohexene reactor through the circulating pipeline, methyl cyclopentene can be generated in a circulating mode, the cyclohexene raw material is fully utilized, and the cost of synthesizing methyl cyclopentane in an enterprise is effectively reduced.
3. The reflux pipe is provided with a reflux tank which is positioned at the upstream of the reflux pump and used for buffering, decelerating and collecting the liquid-phase methylcyclopentene discharged from the condenser, so that the flow of the liquid-phase methylcyclopentene flowing back to the rectifying tower and discharged to the hydrogenation reactor is stable, the separation precision of the rectifying tower and the feeding precision of the hydrogenation reactor are ensured, and the purity of the separated methylcyclopentene and the conversion rate of the hydrogenation reactor are further ensured.
The applicant tests and verifies that the conversion rate of the intermediate product (methylcyclopentene) prepared from cyclohexene is 10%, the conversion rate of the intermediate product (methylcyclopentene) prepared from methylcyclopentane can reach 100%, and the purity of the obtained methylcyclopentane can reach more than 95%.
The following further description is made with reference to the accompanying drawings and detailed description.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the attached drawing, 1 is a cyclohexene reactor, 2 is a rectifying tower, 3 is a hydrogenation reactor, 4 is a stirrer, 5 is a discharge pipe, 6 is a condenser, 7 is a return pipe, 8 is a return pump, 9 is a feed pipe, 10 is a circulation pipeline, 11 is a circulation pump, 12 is a return tank, a is a first valve, b is a second valve, c is a third valve, and d is a fourth valve.
Detailed Description
The utility model discloses in, do not mark equipment, the part of concrete structure or model select for use the equipment or the part of chemical industry field conventionality usually, do not mark the connected mode that connected mode or the manufacturer's suggestion that are chemical industry field conventionality usually of concrete connected mode.
Example 1
Referring to fig. 1, the apparatus for preparing methylcyclopentane from cyclohexene includes a cyclohexene reactor 1, a rectifying tower 2, and a hydrogenation reactor 3, and according to actual requirements, the number of cyclohexene reactors is plural, and usually the number is set in parallel, the number of rectifying towers is plural, and the cyclohexene reactors may be connected in parallel and/or in series, and the number of hydrogenation reactors may also be plural, and usually the number is set in parallel. The stirrer 4 is arranged in the cyclohexene reactor 1, a feed inlet of the cyclohexene reactor 1 is used for being connected with a cyclohexene source, and in the embodiment, the feed inlet of the cyclohexene reactor is arranged at the middle lower part of the side wall of the reactor. The discharge port of the cyclohexene reactor 1 is connected with the rectifying tower 2 through a discharge pipe 5, and the discharge pipe 5 is provided with a first valve a. The top of tower bin outlet of rectifying column 2 is through condenser 6, back flow 7 with the return opening of rectifying column 2 links to each other, set up backwash pump 8 on this return flow 7, set up second valve b on the return flow 7, and be located backwash pump 8's low reaches, in order to stabilize the liquid intermediate product that the separation obtained, set up reflux drum 12 on return flow 7, be located backwash pump 8's upper reaches, in order to make full use of unreacted cyclohexene raw materials, rectifying column 2's the bin outlet at the bottom of the tower links to each other with cyclohexene reactor 1's feed inlet through circulating line 10, set up circulating pump 11 on this circulating line 10, set up fourth valve d on circulating line 10, be located circulating pump 11's low reaches. And a liquid phase feed inlet of the hydrogenation reactor 3 is connected with a return pipe 7 through a feed pipe 9 and is positioned between a return pump 8 and a second valve b, and the feed pipe 9 is provided with a third valve c. The gas phase feed inlet of the hydrogenation reactor 3 is positioned at the top of the hydrogenation reactor 3 and is used for being connected with a hydrogen source, and the discharge outlet of the hydrogenation reactor 3 is positioned at the bottom of the hydrogenation reactor 3.
Example 2
Methylcyclopentane was prepared using the apparatus of example 1, comprising the steps of:
1) adding cyclohexene (cyclohexene purity 99 wt%) and molecular sieve catalyst (volume concentration controlled at 0.25) into cyclohexene reactor, wherein the internal space of the cyclohexene reactor is 200m3The reaction temperature is controlled at 110-112 ℃, the pressure is controlled at 0.4-0.42MPa, and the cyclohexene feeding flow is controlled at 100-105m3Performing molecular rearrangement on the cyclohexene to obtain a mixed material containing a molecular sieve catalyst, the cyclohexene and the methylcyclopentene;
2) discharging the mixed material obtained in the step 1) to a rectifying tower, controlling the tower top temperature of the rectifying tower to be 35-37 ℃, the tower bottom temperature to be 60-63 ℃, controlling the opening degrees of a second valve and a third valve, condensing the separated methyl cyclopentene into liquid through a condenser, then feeding the liquid into a buffer tank, buffering, decelerating and collecting the liquid, driving a reflux pump to reflux part of the liquid methyl cyclopentene to the rectifying tower, feeding part of the liquid methyl cyclopentene into a hydrogenation reactor through a feeding pipe, and controlling the flow rate to be 9-9.5m3H, leading the reflux ratio of the rectifying tower to be 10;
3) hydrogenation through gas phase feed inletHydrogenation is carried out in a reactor, the purity of hydrogen is more than or equal to 99.9 percent, and the flow rate is 2000Nm3H is used as the reference value. Reacting methyl cyclopentene with hydrogen under the action of hydrogenation catalyst (Ni) to obtain methyl cyclopentane, discharging from the bottom of hydrogenation reactor, and controlling flow rate at 9.6-10m3The reaction temperature is 100-105 ℃, and the pressure is 1-1.2 MPa.
The applicant verifies that the conversion rate of the intermediate product (methyl cyclopentene) prepared from cyclohexene is 9%, the conversion rate of methyl cyclopentane is 100%, and the purity of the obtained methyl cyclopentane is 95-95.5%.
Example 3
Methylcyclopentane was prepared using the apparatus of example 1, comprising the steps of:
1) adding cyclohexene (cyclohexene purity 99 wt%) and molecular sieve catalyst (volume concentration controlled at 0.35) into cyclohexene reactor, wherein the internal space of the cyclohexene reactor is 200m3The reaction temperature is controlled to 130-3Performing molecular rearrangement on the cyclohexene to obtain a mixed material containing a molecular sieve catalyst, the cyclohexene and the methylcyclopentene;
2) discharging the mixed material obtained in the step 1) to a rectifying tower, controlling the tower top temperature of the rectifying tower to be 53-55 ℃, the tower bottom temperature to be 79-81 ℃, controlling the opening degrees of a second valve and a third valve, condensing the separated methyl cyclopentene into liquid through a condenser, then feeding the liquid into a buffer tank, buffering, decelerating and collecting the liquid, driving a reflux pump to reflux part of the liquid methyl cyclopentene to the rectifying tower, feeding part of the liquid methyl cyclopentene into a hydrogenation reactor through a feeding pipe, and controlling the flow rate to be 18-18.2m3H, leading the reflux ratio of the rectifying tower to be 20;
3) hydrogenation is carried out in the hydrogenation reactor through a gas phase feed inlet, the purity of the hydrogen is more than or equal to 99.9 percent, and the flow is 5000Nm3H is used as the reference value. Reacting methyl cyclopentene with hydrogen under the action of hydrogenation catalyst (Ni) to obtain methyl cyclopentane, discharging from the bottom of hydrogenation reactor, and controlling flow rate at 19.2-19.6m3The reaction temperature is 175-180 ℃, and the pressure is 1.8-2 MPa.
The applicant verifies that the conversion rate of the intermediate product (methyl cyclopentene) prepared from cyclohexene is 9.7%, the conversion rate of methyl cyclopentane is 100%, and the purity of the obtained methyl cyclopentane is 95-95.3%.

Claims (5)

1. The device for preparing methylcyclopentane from cyclohexene is characterized in that: comprises at least one cyclohexene reactor (1), at least one rectifying tower (2) and at least one hydrogenation reactor (3),
the device is characterized in that a stirrer (4) is arranged in the cyclohexene reactor (1), a feed inlet of the cyclohexene reactor (1) is used for being connected with a cyclohexene source, a discharge outlet of the cyclohexene reactor (1) is connected with the rectifying tower (2) through a discharge pipe (5), a first valve (a) is arranged on the discharge pipe (5),
the top discharge port of the rectifying tower (2) is connected with the reflux port of the rectifying tower (2) through a condenser (6) and a reflux pipe (7), the reflux pipe (7) is provided with a reflux pump (8), the reflux pipe (7) is provided with a second valve (b) and is positioned at the downstream of the reflux pump (8),
the liquid phase feed inlet of hydrogenation ware (3) links to each other with back flow (7) through inlet pipe (9), is located between backwash pump (8) and second valve (b), sets up third valve (c) on inlet pipe (9), the gaseous phase feed inlet of hydrogenation ware (3) is located the top of hydrogenation ware (3) for link to each other with the hydrogen source, the bin outlet of hydrogenation ware (3) is located the bottom of hydrogenation ware (3).
2. The apparatus for preparing methylcyclopentane from cyclohexene according to claim 1, wherein: the rectifying towers (2) are connected in parallel and/or in series.
3. The apparatus for preparing methylcyclopentane from cyclohexene according to claim 1, wherein: the material outlet at the bottom of the rectifying tower (2) is connected with the feed inlet of the cyclohexene reactor (1) through a circulating pipeline (10), and the circulating pipeline (10) is provided with a circulating pump (11).
4. The apparatus for preparing methylcyclopentane from cyclohexene according to claim 3, wherein: and a fourth valve (d) is arranged on the circulating pipeline (10) and is positioned at the downstream of the circulating pump (11).
5. The apparatus for preparing methylcyclopentane from cyclohexene according to claim 1, wherein: the return pipe (7) is provided with a return tank (12) which is positioned at the upstream of the return pump (8).
CN202121136676.5U 2021-05-21 2021-05-21 Device of cyclohexene preparation methyl cyclopentane Active CN215162250U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113248341A (en) * 2021-05-21 2021-08-13 重庆华峰化工有限公司 Device and process for preparing methylcyclopentane from cyclohexene

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113248341A (en) * 2021-05-21 2021-08-13 重庆华峰化工有限公司 Device and process for preparing methylcyclopentane from cyclohexene
CN113248341B (en) * 2021-05-21 2023-11-24 重庆华峰化工有限公司 Device and process for preparing methylcyclopentane from cyclohexene

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