CN208865594U - A kind of continuously hydrogen adding reaction unit with Hydrogen distribution device - Google Patents

A kind of continuously hydrogen adding reaction unit with Hydrogen distribution device Download PDF

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CN208865594U
CN208865594U CN201821206335.9U CN201821206335U CN208865594U CN 208865594 U CN208865594 U CN 208865594U CN 201821206335 U CN201821206335 U CN 201821206335U CN 208865594 U CN208865594 U CN 208865594U
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hydrogen
catalyst
autoclave
distribution device
membrane tube
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杨俞
葛文越
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Shanghai Kaixin Isolation Technology Co Ltd
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Shanghai Kaixin Isolation Technology Co Ltd
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Abstract

The utility model relates to a kind of continuously hydrogen adding reaction units with Hydrogen distribution device, described device includes autoclave, heat exchanger and membrane module, the autoclave is equipped with Hydrogen distribution device, and Hydrogen distribution device hydrogen enter autoclave with nanoscale bubble regime to come into full contact with raw material and catalyst.In reaction process, substrate, hydrogen and fine catalyst react in a high pressure reaction kettle, feed liquid after reaction is delivered to membrane module by heat exchanger, membrane module by feed liquid product and catalyst carry out high-precision filtration separation, the catalyst after separation, which is back in reaction kettle, to be continued to use.Compared with prior art, the utility model uses Hydrogen distribution device to be dispersed in hydrogen in autoclave with nano grade air bubbles, greatly improves reaction efficiency.

Description

A kind of continuously hydrogen adding reaction unit with Hydrogen distribution device
Technical field
The utility model relates to chemical reaction devices, react more particularly, to a kind of continuously hydrogen adding with Hydrogen distribution device Device.
Background technique
Hydrogenation reaction is broadly divided into intermittent and continous way at present, continous way be mainly more kettles series winding continuously hydrogen adding devices and Continuously hydrogen adding device is recycled in one-pot.The continuously hydrogen adding device of two ways realizes being carried out continuously for hydrogenation reaction, but produces It is generally entrained with catalyst fines in product, needs further separating-purifying, and separation process is cumbersome, is not easy to realize continuous metaplasia It produces.
It therefore is a urgent need to solve the problem by the continuous separation of product and catalyst in hydrogenation process.This dress The high voltage bearing membrane separation technique of middle use is set, existing two separate unit-reaction members and separative unit are organically combined, made It obtains hydrogenation catalyst reaction and gets rid of subsequent many and diverse separation system while continuous production.Directly in the reaction system continuous point From product and catalyst, the continuous and steady operation of hydrogenation reaction ensure that.The continuous production of hydrogenation reaction is realized in success.
Utility model content
The purpose of this utility model is exactly to provide a kind of with hydrogen to overcome the problems of the above-mentioned prior art The continuously hydrogen adding reaction unit of distributor.
The purpose of this utility model can be achieved through the following technical solutions:
A kind of continuously hydrogen adding reaction unit, described device include autoclave, heat exchanger and membrane module, and the high pressure is anti- Kettle is answered to be equipped with hydrogen inlet, feed/catalyst import, catalyst refluxing opening and outlet, the outlet of the autoclave and institute Heat exchanger connection is stated, the outlet of the heat exchanger is connect with the membrane module import, and there are two discharge ports for the membrane module, respectively For positioned at the outlet for product of film two sides and catalyst discharge port, the catalyst time of the catalyst discharge port and autoclave Head piece connection, it is described for catalytic agent reuse in autoclave, to be equipped with Hydrogen distribution device in the autoclave Hydrogen distribution device is connect with hydrogen inlet.
In a specific embodiment of the utility model, the Hydrogen distribution device is by hydrogen inlet, hydrogen gas collection Room and membrane tube composition, the hydrogen inlet import are connected to hydrogen inlet on autoclave, the hydrogen inlet outlet It is connect with the hydrogen collecting chamber, the membrane tube includes radial distribution membrane tube and circumferentially distributed membrane tube, the radial distribution membrane tube It is evenly distributed on hydrogen collecting chamber's surrounding, the circumferentially distributed membrane tube is connected to the outside of radial distribution membrane tube, the hydrogen Gas air inlet, hydrogen collecting chamber, radial distribution membrane tube and circumferentially distributed membrane tube inside be interconnected.Hydrogen distribution device makes hydrogen Gas enters autoclave with nanoscale bubble regime and comes into full contact with raw material and catalyst.
In a specific embodiment of the utility model, the radial distribution membrane tube includes with circumferentially distributed membrane tube Internal supporting layer and external film layer, the supporting layer have the channel for passing through hydrogen, and the film layer, which is equipped with, makes hydrogen By fenestra.
In a specific embodiment of the utility model, the outer diameter of the radial distribution membrane tube and circumferentially distributed membrane tube For 2-40mm, the aperture of fenestra is 2-1000nm, the pressure-resistant range 1-50bar of the film layer, the film layer material in the film layer Matter is aluminum oxide, zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or silicon carbide.
In a specific embodiment of the utility model, air inlet, collection chamber material be 304 stainless steels, 316L not The various metal or alloy materials such as rust steel, two phase stainless steel, Hastelloy, titanium, surface can serve as a contrast ceramics, silicon carbide or other high scores Sub- resistant material.
In a specific embodiment of the utility model, the hydrogen inlet of the autoclave connects hydrogen gas Pipe is equipped with hydrogen inlet valve on hydrogen gas pipe;The feed/catalyst import of the autoclave connects raw material/catalysis Agent feed pipe is equipped with feed/catalyst inlet valve on feed/catalyst feed pipe.
In a specific embodiment of the utility model, between the outlet of the autoclave and the heat exchanger Connecting line on be provided with high-pressure pump, be arranged on the connecting line between the outlet and the membrane module import of the heat exchanger There is high-pressure circulation pump.
In a specific embodiment of the utility model, high-pressure pump is mainly that autoclave provides enough pressures Power guarantees being normally carried out for reaction.The lift of high-pressure pump be 20-1000 meter, material be Hastelloy, titanium, two phase stainless steel, 316L stainless steel, stainless steel (or carbon steel) lining plastic, stainless steel (or carbon steel) or other resistant materials.
In a specific embodiment of the utility model, the outlet for product of the membrane module connects product discharge Valve;The catalyst discharge port is connected to autoclave by return line, and return valve is provided on return line, Catalyst exit line is drawn on the return line, catalyst dump valve is provided on catalyst exit line.
In a specific embodiment of the utility model, the autoclave surface serves as a contrast resistant material.
In a specific embodiment of the utility model, the autoclave has insulating.
In a specific embodiment of the utility model, the form of the heat exchanger is shell and tube or jacket type, peace Dress mode is vertical or horizontal.Because hydrogenation reaction is mainly exothermic reaction, to guarantee that reaction process obtains target product, heat exchanger Guarantee suitable temperature environment for recycle system of reaction.
In a specific embodiment of the utility model, the membrane module includes filter membrane and putamina, the filtering The sealing means of film and putamina are welding or sealing ring sealing.
In a specific embodiment of the utility model, the filter membrane of the membrane module is inorganic, the mistake The aperture of filter membrane is 2-1000nm, and the inorganic is metal oxide, and the metal oxide includes aluminum oxide, two Zirconium oxide, titanium dioxide, stainless steel, alloy, nickel alloy or silicon carbide.
In a specific embodiment of the utility model, sealing ring material is fluorine element rubber, hydrogenation nitrile rubber, third Olefin(e) acid rouge rubber, neoprene, three are without EP rubbers, fluorine silicone rubber or nitrile rubber.
In a specific embodiment of the utility model, the autoclave, heat exchanger, putamina and valve material Matter is 304 stainless steels or 316L stainless steel or two phase stainless steel or Hastelloy or titanium.
All pipelines of the whole system of the utility model use two phase stainless steel, Hastelloy, titanium or other corrosion-resistant Material.
Meter contact feed liquid part needed on pipeline is all made of resistant material, including two phase stainless steel, Hastelloy, Titanium, stainless steel (or carbon steel) lining plastic, stainless steel (or carbon steel) serve as a contrast other macromolecule resistant materials.
The utility model continuously hydrogen adding reaction unit, hydrogen, raw material and catalyst continuous feed, in a high pressure reaction kettle instead Ying Hou, reacting rear material continuously enter membrane module after exchanging heat into heat exchanger excessively and are filtered, and product passes through membrane filtration outlet tube road Product discharge valve continuous discharge, catalyst, which returns in autoclave, continues to participate in reaction, when catalyst reflux cause for several times Catalyst is discharged close to when failure in catalyst from catalyst exit line.The present apparatus can be realized successive reaction, continuous discharge.
Compared with prior art, the utility model has unique Hydrogen distribution device, and Hydrogen distribution device makes hydrogen to receive The bubble regime of meter level enters autoclave and comes into full contact with raw material and catalyst, and hydrogen, raw material, catalyst three is promoted to connect Touching, greatly improves three phase catalytic reaction efficiency;High-precision filtration is realized using membrane module, efficiently separates product and solid catalyst Powder, efficiently separating for catalyst provide conveniently for catalyst regeneration;The utility model is by reaction process and separating and filtering process It organically combines, continuous feed continuous discharge realizes the continuity of hydrogenation reaction;The equipment of the utility model can be fully automated Control reduces human cost.
Detailed description of the invention
Fig. 1: continuously hydrogen adding reaction unit structural schematic diagram;
Fig. 2: Hydrogen distribution device schematic view of the front view;
Fig. 3: Hydrogen distribution device overlooking structure diagram;
Fig. 4: the structural schematic diagram of membrane tube.
Figure label: 101 autoclaves, 102 hydrogen inlet valves, 103 feed/catalyst inlet valves, 104 high-pressure pumps, 105 heat exchangers, 106 high-pressure circulation pumps, 107 membrane modules, 108 product discharge valves, 109 catalyst dump valves, 110 reflux are adjusted Valve, 111 Hydrogen distribution devices, 111.1 circumferentially distributed membrane tubes, 111.2 radial distribution membrane tubes, 111.3 hydrogen inlets, 111.4 hydrogen Gas collection chamber, 111.5 film layers, 111.6 supporting layers.
Specific embodiment
The utility model is described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
A kind of continuously hydrogen adding reaction unit, as shown in Figure 1, device includes autoclave 101, heat exchanger 105 and film group Part 107, autoclave 101 are equipped with hydrogen inlet, feed/catalyst import, catalyst refluxing opening and outlet, autoclave 101 outlet is connect with heat exchanger 105, and the outlet of heat exchanger 105 is connect with 107 import of membrane module, and there are two go out for membrane module 107 Material mouth is respectively located at the outlet for product and catalyst discharge port of film two sides, catalyst discharge port and autoclave 101 Catalyst refluxing opening connection, for catalytic agent reuse in autoclave 101, to be equipped with hydrogen in autoclave 101 Distributor 111, Hydrogen distribution device 111 are connect with hydrogen inlet.
With reference to Fig. 1, in the present embodiment, the hydrogen inlet of autoclave connects hydrogen gas pipe, on hydrogen gas pipe Equipped with hydrogen inlet valve 102;The feed/catalyst import of autoclave connects feed/catalyst feed pipe, in raw material/urge Agent feed pipe is equipped with feed/catalyst inlet valve 103.
Such as Fig. 2 and Fig. 3, Hydrogen distribution device is made of hydrogen inlet 111.3, hydrogen collecting chamber 111.4 and membrane tube, hydrogen 111.3 import of air inlet is connected to hydrogen inlet on autoclave, the outlet of hydrogen inlet 111.3 and hydrogen collecting chamber 111.4 connections, membrane tube includes radial distribution membrane tube 111.2 and circumferentially distributed membrane tube 111.1, and 111.4 surrounding of hydrogen collecting chamber is equal For eight root diameters of even distribution to distribution membrane tube 111.2, the outside of radial distribution membrane tube 111.2 is connected with circumferentially distributed membrane tube 111.1, hydrogen Gas air inlet 111.3, hydrogen collecting chamber 111.4, the inside of radial distribution membrane tube 111.2 and circumferentially distributed membrane tube 111.1 are mutual Connection.
Hydrogen inlet, hydrogen collecting chamber's material be 304 stainless steels, 316L stainless steel, two phase stainless steel, Hastelloy, The various metal or alloy materials such as titanium, surface can serve as a contrast ceramics, silicon carbide or other macromolecule resistant materials.
Radial distribution membrane tube, circumferentially distributed membrane tube diameter 2-40mm, membrane tube material are aluminum oxide, zirconium dioxide, two Titanium oxide, stainless steel, alloy, nickel alloy, silicon carbide.
Such as Fig. 4, radial distribution membrane tube and circumferentially distributed membrane tube include internal supporting layer 111.6 and external film layer 111.5, supporting layer 111.6 has the channel for passing through hydrogen, and film layer 111.5 is equipped with the fenestra for passing through hydrogen.In film layer The aperture of fenestra is 2-1000nm, film pressure resistance range 1-50bar.
With reference to Fig. 1, in the present embodiment, high pressure is provided on the connecting line between the outlet and heat exchanger of autoclave 104 are pumped, is provided with high-pressure circulation pump 106 on the connecting line between the outlet and membrane module import of heat exchanger.
In the present embodiment, high-pressure pump is mainly that autoclave provides enough pressure, guarantees being normally carried out for reaction.It is high The lift of press pump is 20-1000 meters, and material is Hastelloy, titanium, two phase stainless steel, 316L stainless steel, stainless steel (or carbon steel) Lining plastic, stainless steel (or carbon steel) or other resistant materials.
With reference to Fig. 1, in the present embodiment, the outlet for product of membrane module 107 connects product discharge valve 108;Catalyst discharging Mouth is connected to autoclave 101 by return line, return valve 110 is provided on return line, in return line Upper extraction catalyst exit line, is provided with catalyst dump valve 109 on catalyst exit line.
In the present embodiment, autoclave surface serves as a contrast resistant material.
In the present embodiment, autoclave has insulating.
In the present embodiment, the form of heat exchanger 105 is shell and tube or jacket type, and mounting means is vertical or horizontal.Because adding Hydrogen reaction is mainly exothermic reaction, and to guarantee that reaction process obtains target product, heat exchanger 105 is that recycle system of reaction guarantees suitable Suitable temperature environment.
In the present embodiment, membrane module 107 includes filter membrane and putamina, and the sealing means of filter membrane and putamina are welding or close Seal sealing.
In the present embodiment, the filter membrane of membrane module 107 is inorganic, and the aperture of filter membrane is 2-1000nm, inorganic material Matter is metal oxide, and metal oxide includes aluminum oxide, zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy Or silicon carbide.
In the present embodiment, sealing ring material is fluorine element rubber, hydrogenation nitrile rubber, acrylate rubber, neoprene, three Without EP rubbers, fluorine silicone rubber or nitrile rubber.
In the present embodiment, autoclave 101, heat exchanger 105, putamina and all kinds of valves material be 304 stainless steels or 316L stainless steel or two phase stainless steel or Hastelloy or titanium.
All pipelines of whole system use two phase stainless steel, Hastelloy, titanium or other corrosion-resistant materials in the present embodiment Material.
Meter contact feed liquid part needed on pipeline is all made of resistant material, including two phase stainless steel, Hastelloy, Titanium, stainless steel (or carbon steel) lining plastic, stainless steel (or carbon steel) serve as a contrast other macromolecule resistant materials.
Embodiment 2
A kind of technique of continuously hydrogen adding reaction unit, processing step are as follows:
(1) the feed/catalyst inlet valve 103 that raw material and catalyst pass through feed/catalyst transfer pipeline enters high pressure Reaction kettle 101;
(2) hydrogen enters Hydrogen distribution device 111 by the hydrogen inlet valve 102 on hydrogen delivery tube road, in Hydrogen distribution device In 111, hydrogen collecting chamber 111.4 is entered by hydrogen inlet 111.3, then radial distribution is dispersed by collection chamber 111.4 Membrane tube 111.2 and circumferentially distributed membrane tube 111.1, hydrogen is in membrane tube successively by film layer 111.5 and support under high pressure effect Layer 111.6, enters autoclave 101 with bubble regime and comes into full contact with raw material and catalyst, react and generate product, institute There is material by heat exchanger 105;
(3) enter membrane module 107 by high-pressure circulation pump 106 by the material of heat exchanger, filtered by membrane module, product It is discharged by the product discharge valve 108 of membrane filtration outlet tube road, catalyst returns to autoclave by return valve 110 Reaction is continued to participate in 101.
Wherein in step (1), solid powder th-1 catalyst is added in raw material enters reaction kettle together, step (2) mesohigh pump 104 for system provide enough pressure conditions to realize the continuous circulation of reaction, at the same mixed material in certain pressure and Hydrogen reacts under the action of catalyst with raw material under the conditions of temperature, and product is generated in autoclave.The purpose of heat exchanger exists Cool down in material, first is that preventing the excessively high side reaction product of temperature from increasing, second is that guaranteeing that temperature is stablized, prevents temperature fluctuation excessive Damage membrane module.
It is gradually inactivated by certain time post catalyst reaction, periodically from catalyst dump valve 109 by the catalyst of inactivation Discharge regeneration, and add new catalyst from raw material pipeline and reaction system is entered by feed/catalyst inlet valve 103.
The utility model uses unique Hydrogen distribution device, helps hydrogen high efficiency dispersion, promotes hydrogen, raw material, catalyst Three are in contact, and greatly improve three phase catalytic reaction efficiency.
It can understand the above description of the embodiments is intended to facilitate those skilled in the art and use practical It is novel.Person skilled in the art obviously easily can make various modifications to these embodiments, and illustrating herein General Principle be applied in other embodiments without having to go through creative labor.Therefore, the utility model is not limited to above-mentioned Embodiment, those skilled in the art's announcement according to the present utility model, do not depart from improvement that the utility model scope is made and Modification should be all within the protection scope of the utility model.

Claims (9)

1. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device, which is characterized in that described device include autoclave, Heat exchanger and membrane module, the autoclave are equipped with hydrogen inlet, feed/catalyst import, catalyst refluxing opening and outlet, The outlet of the autoclave is connect with the heat exchanger, and the outlet of the heat exchanger is connect with the membrane module import, institute Stating membrane module, there are two discharge ports, are respectively located at the outlet for product and catalyst discharge port of film two sides, and the catalyst goes out The connection of the catalyst refluxing opening of material mouth and autoclave, is used for by catalytic agent reuse in autoclave, in the high pressure Hydrogen distribution device is equipped in reaction kettle, the Hydrogen distribution device is connect with hydrogen inlet.
2. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described Hydrogen distribution device is made of hydrogen inlet, hydrogen collecting chamber and membrane tube, in the hydrogen inlet import and autoclave Hydrogen inlet connection, the hydrogen inlet outlet are connect with the hydrogen collecting chamber, and the membrane tube includes radial distribution membrane tube With circumferentially distributed membrane tube, the radial distribution membrane tube is evenly distributed on hydrogen collecting chamber's surrounding, the circumferentially distributed membrane tube It is connected to the outside of radial distribution membrane tube, the hydrogen inlet, hydrogen collecting chamber, radial distribution membrane tube and circumferentially distributed membrane tube Inside be interconnected.
3. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 2, which is characterized in that described Radial distribution membrane tube and circumferentially distributed membrane tube include internal supporting layer and external film layer, and the supporting layer has and makes hydrogen By channel, the film layer be equipped with pass through hydrogen fenestra.
4. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 3, which is characterized in that described The outer diameter of radial distribution membrane tube and circumferentially distributed membrane tube is 2-40mm, and the aperture of fenestra is 2-1000nm in the film layer, described The pressure-resistant range 1-50bar of film layer.
5. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described The hydrogen inlet of autoclave connects hydrogen gas pipe, and hydrogen inlet valve is equipped on hydrogen gas pipe;The reaction under high pressure The feed/catalyst import of kettle connects feed/catalyst feed pipe, and feed/catalyst is equipped on feed/catalyst feed pipe Inlet valve.
6. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described High-pressure pump, the outlet of the heat exchanger and institute are provided on connecting line between the outlet of autoclave and the heat exchanger It states and is provided with high-pressure circulation pump on the connecting line between membrane module import.
7. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described The outlet for product of membrane module connects product discharge valve;The catalyst discharge port is connected to reaction under high pressure by return line Kettle is provided with return valve on return line, draws catalyst exit line on the return line, is discharged in catalyst Catalyst dump valve is provided on pipe.
8. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described Autoclave surface serves as a contrast resistant material.
9. a kind of continuously hydrogen adding reaction unit with Hydrogen distribution device according to claim 1, which is characterized in that described Autoclave has insulating.
CN201821206335.9U 2018-07-27 2018-07-27 A kind of continuously hydrogen adding reaction unit with Hydrogen distribution device Active CN208865594U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110756119A (en) * 2018-07-27 2020-02-07 上海凯鑫分离技术股份有限公司 Continuous hydrogenation reaction device with hydrogen distributor and process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110756119A (en) * 2018-07-27 2020-02-07 上海凯鑫分离技术股份有限公司 Continuous hydrogenation reaction device with hydrogen distributor and process

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