CN207973695U - A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine - Google Patents

A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine Download PDF

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Publication number
CN207973695U
CN207973695U CN201820143327.8U CN201820143327U CN207973695U CN 207973695 U CN207973695 U CN 207973695U CN 201820143327 U CN201820143327 U CN 201820143327U CN 207973695 U CN207973695 U CN 207973695U
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catalyst
phenylenediamine
liquid
tank body
reduction method
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CN201820143327.8U
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倪晓峰
张玉宝
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SHANGHAI HONGYUAN XINCHUANG MATERIAL TECHNOLOGY CO., LTD.
Zhejiang Hongsheng Chemical Research Limited
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ZHEJIANG HONGSHENG CHEMICAL RESEARCH Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The utility model is related to chemical fields, disclose the preparation system that a kind of liquid-phase catalyst hydrogenating reduction method prepares p-phenylenediamine, tank, hydrogenation reaction kettle, catalyst filtration device, rectifying column, recycling can are added including nitroaniline, hydrogen inlet pipe is provided on the hydrogenation reaction kettle, catalyst adds pipe, it is characterised in that:The catalyst filtration device includes tank body, is arranged in the middle part of tank body and for the filter core of filtration catalytic agent;The inlet tube being connect with the hydrogenation reaction kettle is provided at the top of the tank body, the bottom of the tank body is provided with the outlet tube being connect with the rectifying column.The utility model has the following advantages and effect:This programme utilizes new mechanical structure, the nitro of nitroaniline is under the action of catalyst amino by hydrogen reducing, to prepare p-phenylenediamine, the phenylenediamine solution for being mixed with catalyst at this time enters the filter core of catalyst filtration device and is filtered, catalyst stays in filter core, to improve the rate of recovery to catalyst.

Description

A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine
Technical field
The utility model is related to chemical field, more particularly to a kind of liquid-phase catalyst hydrogenating reduction method prepares p-phenylenediamine Preparation system.
Background technology
P-phenylenediamine is a kind of important organic intermediate, is widely used in the industries such as dyestuff, rubber, national defence.In dyestuff Industry can make azo dyes, fur dyeing agent;Rubber antioxidant etc. can be made in rubber industry.The life of traditional p-phenylenediamine Production. art is the crude product that paranitroanilinum generates p-phenylenediamine through akali sulphide or iron powder reducing, is most purified afterwards through recrystallization and height is made Purity p-phenylenediamine.When traditional production technology uses iron powder as catalyst, product yield is low, and will produce with largely having The iron cement of machine poisonous substance pollutes environment.It uses at present and more prepares p-phenylenediamine for liquid-phase catalyst hydrogenating reduction method.
Currently, Authorization Notice No. is CN202099218U, authorized announcement date is that the Chinese patent on January 4th, 2012 discloses A kind of device of producing p-phenylenediamine by using liquid phase continuous hydrogenation method, the device include paranitroanilinum storage tank, methanol storage tank, level-one Hydrogenation reaction kettle, secondary hydrogenation reaction kettle, out-feed liquid control tank, catalyst sedimentation slot and smart gold-plating tower, level-one hydrogenation reaction kettle string Union II grade hydrogenation reaction kettle connects paranitroanilinum storage tank and first by pipeline through metering pump respectively on level-one hydrogenation reaction kettle Alcohol storage tank, hydrogen inlet is set on I and II hydrogenation reaction kettle, and the discharge port of secondary hydrogenation reaction kettle is connected to discharging hydraulic control through pipeline Tank processed, out-feed liquid control tank connect two catalyst sedimentation slots by pipeline, and the discharge port of catalyst sedimentation slot is connected to through pipeline Smart gold-plating tower.In process involved by the device of this producing p-phenylenediamine by using liquid phase continuous hydrogenation method, the nitro of nitroaniline It is under the action of catalyst amino by hydrogen reducing, to prepare p-phenylenediamine.
In the device of the producing p-phenylenediamine by using liquid phase continuous hydrogenation method, two are connected with by pipeline on out-feed liquid control tank A catalyst sedimentation slot, catalyst is deposited under the effect of gravity in the lower part cone of catalyst sedimentation slot, and passes through catalyst Recovery port is recycled.But the solution for preparing is when entering in catalyst sedimentation slot after reacting, the flowing velocity of liquid compared with Soon, the case where easy to carry catalyst is discharged from subsider discharge port at this time, reduces the rate of recovery of catalyst.
Utility model content
The purpose of this utility model is to provide the preparation system that a kind of liquid-phase catalyst hydrogenating reduction method prepares p-phenylenediamine, Have the effect of improving to solid catalyst recovery yield.
The above-mentioned technical purpose of the utility model technical scheme is that:A kind of liquid-phase catalyst adds Hydrogen reduction method prepares the preparation system of p-phenylenediamine, including nitroaniline add tank, added with nitroaniline it is being connected on tank plus Hydrogen reaction kettle, the catalyst filtration device being connect with hydrogenation reaction kettle, the rectifying column being connect with the catalyst filtration device, with The recycling can of rectifying column connection is provided with hydrogen inlet pipe on the hydrogenation reaction kettle, catalyst adds pipe, the catalyst Filter device includes tank body, is arranged in the middle part of tank body and for the filter core of filtration catalytic agent;Be provided at the top of the tank body with The inlet tube of the hydrogenation reaction kettle connection, the bottom of the tank body is provided with the outlet tube being connect with the rectifying column.
By using said program, the nitro of nitroaniline is under the action of catalyst amino by hydrogen reducing, to make Standby p-phenylenediamine, the phenylenediamine solution for being mixed with catalyst at this time enter the filter core of catalyst filtration device and are filtered, urge Agent stays in filter core, to improve to the rate of recovery of catalyst, then filtered phenylenediamine solution enter rectifying column into Row rectifying.
The utility model is further arranged to:The bore of the filter core gradually increases along vertically downward direction.
By using said program, when remaining in filter core because of catalyst, certain blocking can be generated on filter core to be influenced, from And make flowing velocity of the phenylenediamine solution through filtration core when slack-off, at this time so that the bore of filter core is along vertically downward direction Gradually increase, to increase the vessel space of filter core, reduces the influence generated when catalyst blockage filter core.
The utility model is further arranged to:The tank body includes the feed end with the inlet tube, with described The discharge end of outlet tube, the connecting tube being detachably arranged between feed end and the discharge end, the filter core are arranged described In connecting tube and in the connecting tube.
By using said program, because connecting tube is detachably connected between feed end and discharge end, and filter core setting exists In connecting tube, at this time by the way that connecting tube is dismantled between feed end and discharge end after, it is convenient in the filter core in connecting tube Catalyst is recycled.
The utility model is further arranged to:Mounting ring, the top of the filter core are provided on the inner wall of the connecting tube Portion is provided with the locating ring being shelved in the mounting ring.
By using said program, filter core is shelved on by locating ring in the mounting ring on connection inside pipe wall, so that Filter core is detachably connected in connecting tube, after dismantling lower connector, filter core is dismantled by continuing, to realize in filter core Catalyst is recycled.
The utility model is further arranged to:The both ends of the connecting tube are respectively arranged with first flange, the charging End is respectively arranged with the second flange to match with the first flange close to one end of the connecting tube with the discharge end, described It is fixedly connected by bolt and nut between first flange and the second flange.
By using said program, between connecting tube and feed end, pass through first flange, between connecting tube and discharge end Two flanges, bolt and nut are fixedly connected, to by after the Bolt dismantling in first flange and second flange, from feed end and go out Connecting tube is removed between expects pipe.
The utility model is further arranged to:The intersection of the first flange and the second flange is provided with sealing Circle.
By using said program, the sealing ring between first flange and second flange can increase first flange and second The leakproofness of flange, reducing phenylenediamine solution, there is a situation where infiltrations or leakage to occur.
The utility model is further arranged to:The connecting tube is made of transparent organic glass.
By using said program, connecting tube is made of transparent organic glass, can be observed connect by connecting tube at this time Filter core in pipe selects the suitable time to dismantle connecting tube, and to filter core the recovering state of catalyst to facilitate In catalyst recycled.
The utility model is further arranged to:There are two the tank body settings, between the inlet tube of two tank bodies It is provided with the feed liquor house steward for connecting the hydrogenation reaction kettle, is provided between the outlet tube of two tank bodies for connecting The go out liquid house steward of the rectifying column is provided with liquid flowing valve on the inlet tube, liquid valve door is provided on the outlet tube.
By using said program, there are two tank body settings, and the catalyst in the filter core in a tank body needs at this time When recycling, can by the tank body liquid flowing valve and liquid valve door close so that filter core in another tank body is realized to benzene two Amine aqueous solution is filtered.
In conclusion the utility model has the advantages that:
1, the nitro of nitroaniline is under the action of catalyst amino by hydrogen reducing, to prepare p-phenylenediamine, at this time The phenylenediamine solution for being mixed with catalyst enters the filter core of catalyst filtration device and is filtered, and catalyst stays in filter core, To improve the rate of recovery to catalyst;
2, tank body includes feed end, connecting tube and discharge end, and connecting tube is detachably connected between feed end and discharge end, Filter core is detachably connected in connecting tube, is recycled to the catalyst in filter core to convenient;
It 3,, can will be on the tank body when catalyst in filter core in a tank body needs recycling there are two tank body settings Liquid flowing valve and liquid valve door close so that filter core in another tank body realizes that p-phenylenediamine solution is filtered.
Description of the drawings
Fig. 1 is the structural schematic diagram of the utility model;
Fig. 2 is the structural schematic diagram that the utility model is located at catalyst filtration device.
Reference numeral:1, nitroaniline adds tank;2, hydrogenation reaction kettle;21, hydrogen inlet pipe;22, catalyst adds pipe;3、 Catalyst filtration device;31, tank body;311, feed end;3111, inlet tube;3112, liquid flowing valve;312, connecting tube;3121、 Mounting ring;313, discharge end;3131, outlet tube;3132, liquid valve door;32, filter core;321, locating ring;33, first flange; 34, second flange;35, bolt and nut;36, sealing ring;37, feed liquor house steward;38, go out liquid house steward;4, rectifying column;5, recycling can.
Specific implementation mode
The utility model is described in further detail below in conjunction with attached drawing.
Embodiment 1:A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine, as shown in Figure 1, including Nitroaniline adds tank 1, adds the hydrogenation reaction kettle 2 connected on tank 1, the catalysis being connect with hydrogenation reaction kettle 2 with nitroaniline Agent filter device 3, the rectifying column 4 being connect with catalyst filtration device 3, the recycling can 5 being connect with rectifying column 4;And adding hydrogen anti- It answers and has been wholely set hydrogen inlet pipe 21 on kettle 2 and catalyst adds pipe 22.
As shown in Fig. 2, catalyst filtration device 3(See Fig. 1)Including two tank bodies, 31, two filter cores 32.
As shown in Fig. 2, tank body 31 includes feed end 311, connecting tube 312 and discharge end 313.One on feed end 311 Body is provided with inlet tube 3111, and liquid flowing valve 3112 is equipped on inlet tube 3111;It has been wholely set out on discharge end 313 Liquid pipe 3131 is equipped with liquid valve door 3132 on outlet tube 3131;Connecting tube 312 is made of transparent organic glass, even The both ends of take over 312 have been respectively fixedly connected with first flange 33, and in feed end 311 and discharge end 313 close to connecting tube 312 Part is respectively fixedly connected with the second flange 34 to match with first flange 33, mutually close first flange 33 and second flange 34 It is fixedly connected by bolt and nut 35, and intrinsic sealing ring between inconsistent first flange 33 and second flange 34 36.It is connected between inlet tube 3111 on the feed end 311 of two tank bodies 31 and hydrogenation reaction kettle 2(See Fig. 1)It communicates Feed liquor house steward 37 is connected with and rectifying column 4 between the outlet tube 3131 on the discharge end 313 of two tank bodies 31(See Fig. 1)Phase Logical go out liquid house steward 38.
As shown in Fig. 2, being wholely set mounting ring 3121 on the inner wall of connecting tube 312, two filter cores 32 are installed respectively In two connecting tubes 312, the locating ring 321 being useful for being shelved in mounting ring 3121 is wholely set at the top of filter core 32; The bore of filter core 32 is gradually increased along vertically downward direction simultaneously.
Implementation process:When the nitroaniline during nitroaniline adds tank 1 enters in hydrogenation reaction kettle 2, nitroaniline Nitro under the action of catalyst by hydrogen reducing be amino be mixed with catalyst at this time to prepare p-phenylenediamine solution Phenylenediamine solution is entered in filter core 32 and is filtered so that catalyst stays in filter core 32, is returned to catalyst to improve Yield, filtered phenylenediamine solution are continued through after rectifying column 4 distilled, are collected in recycling can 5.
This specific embodiment is only the explanation to the utility model, is not limitations of the present invention, ability Field technique personnel can as needed make the present embodiment the modification of not creative contribution after reading this specification, but As long as all being protected by Patent Law in the right of the utility model.

Claims (8)

1. a kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine, including nitroaniline adds tank(1)And Nitroaniline adds tank(1)The hydrogenation reaction kettle of upper connection(2)With hydrogenation reaction kettle(2)The catalyst filtration device of connection (3)And the catalyst filtration device(3)The rectifying column of connection(4)And the rectifying column(4)The recycling can of connection(5), institute State hydrogenation reaction kettle(2)On be provided with hydrogen inlet pipe(21), catalyst add pipe(22), it is characterised in that:The catalyst mistake Filter device(3)Including tank body(31), be arranged in tank body(31)Middle part and the filter core for being used for filtration catalytic agent(32);The tank body (31)Top be provided with and the hydrogenation reaction kettle(2)The inlet tube of connection(3111), the tank body(31)Bottom setting Have and the rectifying column(4)The outlet tube of connection(3131).
2. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 1 prepares the preparation system of p-phenylenediamine, special Sign is:The filter core(32)Bore gradually increase along vertically downward direction.
3. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 1 prepares the preparation system of p-phenylenediamine, special Sign is:The tank body(31)Including with the inlet tube(3111)Feed end(311), have the outlet tube(3131) Discharge end(313), be detachably arranged at feed end(311)With the discharge end(313)Between connecting tube(312), described Filter core(32)It is arranged in the connecting tube(312)Above and it is located at the connecting tube(312)It is interior.
4. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 3 prepares the preparation system of p-phenylenediamine, special Sign is:The connecting tube(312)Inner wall on be provided with mounting ring(3121), the filter core(32)Top be provided with and shelve In the mounting ring(3121)On locating ring(321).
5. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 3 prepares the preparation system of p-phenylenediamine, special Sign is:The connecting tube(312)Both ends be respectively arranged with first flange(33), the feed end(311)With the discharging End(313)Close to the connecting tube(312)One end be respectively arranged with and the first flange(33)The second flange of matching (34), the first flange(33)With the second flange(34)Between pass through bolt and nut(35)It is fixedly connected.
6. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 5 prepares the preparation system of p-phenylenediamine, special Sign is:The first flange(33)With the second flange(34)Intersection be provided with sealing ring(36).
7. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 3 prepares the preparation system of p-phenylenediamine, special Sign is:The connecting tube(312)It is made of transparent organic glass.
8. a kind of liquid-phase catalyst hydrogenating reduction method according to claim 2 prepares the preparation system of p-phenylenediamine, special Sign is:The tank body(31)There are two settings, two tank bodies(31)Inlet tube(3111)Between be provided with for connecting Connect the hydrogenation reaction kettle(2)Feed liquor house steward(37), two tank bodies(31)Outlet tube(3131)Between be arranged it is useful In the connection rectifying column(4)Go out liquid house steward(38), the inlet tube(3111)On be provided with liquid flowing valve(3112), described Outlet tube(3131)On be provided with liquid valve door(3132).
CN201820143327.8U 2018-01-27 2018-01-27 A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine Active CN207973695U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110437075A (en) * 2019-08-16 2019-11-12 上海鸿源鑫创材料科技有限公司 A kind of phenylenediamine preparation preparation method of dinitrobenzene continuous catalytic hydrogenation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110437075A (en) * 2019-08-16 2019-11-12 上海鸿源鑫创材料科技有限公司 A kind of phenylenediamine preparation preparation method of dinitrobenzene continuous catalytic hydrogenation
CN110437075B (en) * 2019-08-16 2022-03-11 上海鸿源鑫创材料科技有限公司 Preparation method of dinitrobenzene for preparing phenylenediamine through continuous catalytic hydrogenation

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Effective date of registration: 20190605

Address after: Room 322 and 323, 1345 and 1363 Hutai Road, Shanghai, 200436

Co-patentee after: Zhejiang Hongsheng Chemical Research Limited

Patentee after: SHANGHAI HONGYUAN XINCHUANG MATERIAL TECHNOLOGY CO., LTD.

Address before: 312369 Weisan Road, Shangyu Economic and Technological Development Zone, Hangzhou Bay, Shaoxing City, Zhejiang Province

Patentee before: Zhejiang Hongsheng Chemical Research Limited