CN205556513U - Continuous hydrogenation ware of organic intermediate - Google Patents
Continuous hydrogenation ware of organic intermediate Download PDFInfo
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- CN205556513U CN205556513U CN201620150081.8U CN201620150081U CN205556513U CN 205556513 U CN205556513 U CN 205556513U CN 201620150081 U CN201620150081 U CN 201620150081U CN 205556513 U CN205556513 U CN 205556513U
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Abstract
The utility model relates to a catalytic hydrogenation technical field of organic intermediate, continuous hydrogenation ware of organic intermediate is specifically disclosed, set up two sprayers through coaxial symmetry, make hydrogen, liquid phase organic intermediate and solid catalyst three -phase material mix behind the formation efflux, impact in opposite directions, the percussion flow produces, reinforce hydrogenation, can show and put forward high pressure heater hydrogen reaction efficiency and product quality, put forward high pressure heater hydrogen in -process hydrogen utilization ratio, reduce material circulation volume and energy consumption, the catalyst wearing and tearing reduce, low production cost.
Description
Technical field
This utility model relates to technical field of fine, especially relates to the technical field of catalytic hydrogenation of organic intermediate.
Background technology
Catalytic hydrogenation is the important technology of organic intermediate synthesis, and it instead of iron powder reducing technology in the past, for the organic intermediate reduction reaction containing unsaturated group, more clean and effective.The most successively have developed autoclave interval liquid phase hydrogenation technology, gas-phase fluidized-bed hydrogen addition technology, injection hydrogenation reaction technology etc., and the most industrially applied.But these technology all show certain deficiency in the actual production of organic intermediate.
Autoclave intermittent reaction technology is appropriate only for the product that yield is little, and for large-tonnage product, the automatic control relatively difficult to achieve of autoclave intermittent reaction, the quality of product is difficult to stable.Gas-phase fluidized-bed hydrogenation reaction technology can be used for large-tonnage product, but needs before hydrogenation reaction first to be gasified by intermediate reaction thing, and reaction temperature is high, and the by-product such as whole process energy consumption height, tar is many, holistic cost height.
Injection hydrogen addition technology is to utilize injection reaction vessel, and by solid catalyst particle, liquid organic intermediate raw material and hydrogen hybrid reaction, hydrogenation process mostly is mass transport limitation.The principle of injection reaction vessel is to utilize flow at high speed to go volume to inhale other phases mutually, makes each phase close contact, then dispersed in reaction vessel or suspension, and completes reaction.Injection reaction vessel is mainly made up of ejector (jet nozzle) and reaction vessel, sprays hydrogen addition technology many employings loop spray reaction vessel, i.e. utilizes circulating pump repeatedly to be circulated by material.
In existing injection hydrogen addition technology, ejector is located at single lower spray in reaction vessel, only react in ejector by circulating pump recycle stock, suction hydrogen, reaction time fast due to material flow, in ejector is short, this causes needing the substantial amounts of circulation of material, can ensure to provide enough reaction times in ejector, due to the substantial amounts of iterative cycles of material, overall operation power consumption is the highest, the abrasion of catalyst simultaneously increases, difficulty is caused, the production cost height that product is overall to the filtration of catalyst.
Utility model content
The technical problems to be solved in the utility model is to provide organic intermediate continuously hydrogen adding reactor, hydrogenation reaction efficiency and product quality can be significantly improved, improve hydrogen utilization ratio in hydrogenation process, reduce solid circulating rate and energy consumption, catalyst abrasion reduces, and production cost is lower.
For solving above-mentioned technical problem, technical solution adopted in the utility model is: organic intermediate continuously hydrogen adding reactor, it includes reaction vessel, the top of described reaction vessel is provided with ejector, for hydrogen and the liquid phase organic intermediate containing solid catalyst particle are mixed to form jet, hydrogen charging aperture and main material inlet it is additionally provided with on described reaction vessel, the gas access of described ejector is connected with the top of described reaction vessel by hydrogen circulation line, the liquid inlet of described ejector is by the fluid connection of principal goods material circulation line with the bottom of described reaction vessel, described ejector is two, the jet of two ejectors is distributed in described reaction vessel the most in opposite directions, two strands of jets that ejector is produced can produce percussion flow；Described principal goods material circulation line is provided with circulating pump and heat exchanger, and the liquid-solid material circulation in reaction vessel of described circulating pump provides power, the described heat exchanger liquid-solid material temperature control in principal goods material circulation line.
As preferably, two jets are positioned at reaction vessel sustained height.
Further, described principal goods material circulation line being additionally provided with filter, for the liquid-solid material of part in principal goods material circulation line is carried out solid-liquid separation, in filter, filtrate discharges organic intermediate continuously hydrogen adding reactor.
Use and have the beneficial effects that produced by technique scheme:
The organic intermediate continuously hydrogen adding reactor that this utility model provides, compared with prior art, its distinguishing feature is, on the reaction vessel in space, portion, the most opposed two ejectors, when after material outflow jet end, clash in opposite directions.According to the principle of percussion flow, after material clashes in opposite directions, multi phase interface can be sufficiently promoted and update, strengthen gas-liquid-solid multiphase mass transfer, thoroughly eliminate external diffusion impact, make reaction not by mass transport limitation.Under percussion flow principle effect, this makes material after outflow jet end, remains to continue hydrogenation reaction by clashing into promotion multi phase interface renewal, has been obviously prolonged reaction time in single cycle.These characteristics can significantly improve product quality, improves hydrogenation process hydrogen utilization efficiency, reduces hydrogen circulation amount, thus reduces hydrogenation process energy consumption, and total procedural strength is high, and space-time production capacity is big, product integral production low cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of embodiment of this utility model organic intermediate continuously hydrogen adding reactor；
Wherein, 1, reaction vessel；2, ejector；3, hydrogen circulation line；4, principal goods material circulation line；5, circulating pump；6, heat exchanger；7, filter；11, hydrogen charging aperture；12, main material inlet；61, circulating water outlet；62, circulating water intake；71, filtrate (liquid.
Detailed description of the invention
Embodiment 1
Organic intermediate continuously hydrogen adding reactor, see Fig. 1, it includes reaction vessel 1, two ejectors 2 that reaction vessel 1 top coaxial-symmetrical is arranged, ejector 2 is for being mixed to form jet by hydrogen and the liquid phase organic intermediate containing solid catalyst particle, the jet of two ejectors 2 is distributed in reaction vessel 1 the most in opposite directions so that two strands of jets that ejector 2 produces can produce percussion flow；Hydrogen charging aperture 11 and main material inlet 12 it is additionally provided with on reaction vessel 1, the gas access of ejector 2 is connected with the top of reaction vessel 1 by hydrogen circulation line 3, the liquid inlet of ejector 2 is by the fluid connection of principal goods material circulation line 4 with the bottom of reaction vessel 1, principal goods material circulation line 4 is provided with circulating pump 5 and heat exchanger 6, circulating pump 5 liquid-solid material circulation in reaction vessel 1 provides power, the heat exchanger 6 liquid-solid material temperature control in principal goods material circulation line 4.Heat exchanger 6 uses recirculated water as heat transferring medium, and it is respectively equipped with circulating water outlet 61 and circulating water intake 62.
Organic intermediate continuously hydrogen adding reaction method, liquid phase organic intermediate containing solid catalyst particle and hydrogen are mixed generation organic intermediate hydrogenation reaction at ejector 2 with the form of jet by continuous print, coaxially clash in opposite directions after the jet ejection of two ejectors 2, form percussion flow and proceed hydrogenation reaction；Reaction gained system in, hydrogen float separate with liquid-solid mixture, liquid-solid mixture is deposited on bottom reaction vessel 1, then through circulating pump 5 and heat exchanger 6 arrive ejector 2 realize Matter Transfer reaction.After circulation some cycles, separate and collect hydrogenation products.
Further, preferred Matter Transfer mode is: after Matter Transfer reaction some cycles, part liquid-solid mixture is through solid-liquid separation, gained liquid phase separation thing flows out response system as product, hydrogen and remaining fluid solid mixture mix with the hydrogen being newly added and the liquid phase organic intermediate containing solid catalyst particle respectively, then the form circular response with jet.
As preferably, two jets are positioned horizontally in sustained height in reaction vessel 1.
Further improvement to the technical program, principal goods material circulation line 4 is additionally provided with filter 7, and for the liquid-solid material of part in principal goods material circulation line 4 is carried out solid-liquid separation, in filter 7, filtrate discharges organic intermediate continuously hydrogen adding reactor by filtrate (liquid 71.
Embodiment 2
Use such as organic intermediate continuously hydrogen adding reactor in embodiment 1, it is blended with the organic intermediate dimethyl maleate of catalyst, quantitatively being continuously added in reaction vessel 1 by main material inlet 12, hydrogen is quantitatively continuously added in reaction vessel 1 by hydrogen charging aperture 11；Under circulating pump 5 carries, material in reaction vessel 1, the heat exchanger 6 flowed through successively outside reaction vessel 1 carries out taking heat, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out response system as product and is carried out subsequent treatment, and rest materials enters ejector 2, and ejector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, clash into the most in opposite directions and proceed hydrogenation reaction；In reaction vessel 1, hydrogen floats after separating with liquid and catalyst, and liquid and catalyst continue on through circulating pump 5 circular response.Course of reaction keeps temperature of charge 120～130 DEG C, and material mean residence time in reaction vessel 1 is only 15min.
This reaction uses autoclave hydrogenation, and reaction time needs 2h, uses common injection hydrogenation reaction time of staying 1h, and in this utility model embodiment, reaction time is greatly shortened.
This utility model embodiment product is through analyzing: conversion ratio reaches 99.9%, unconverted raw material dimethyl maleate content about 0.1%, and hydrogenation products dimethyl succinate content about 99.8% can sell as product, it is not necessary to follow-up subtractive process.
Embodiment 3
Use such as organic intermediate continuously hydrogen adding reactor in embodiment 1, it is blended with the organic intermediate 2 of catalyst, 5-dimethoxy-4 '-chloronitrobenzene solution, is quantitatively continuously added in reaction vessel 1 by main material inlet 12, and hydrogen is quantitatively continuously added in reaction vessel 1 by hydrogen charging aperture 11；Under circulating pump 5 carries, material in reaction vessel 1, the heat exchanger 6 flowed through successively outside reaction vessel 1 carries out taking heat, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out response system as product and is carried out subsequent treatment, and rest materials enters ejector 2, and ejector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, clash into the most in opposite directions and proceed hydrogenation reaction；In reaction vessel 1, hydrogen floats after separating with liquid and catalyst, and liquid and catalyst continue on through circulating pump 5 circular response.Course of reaction keeps temperature of charge 90～95 DEG C, and material mean residence time in reaction vessel 1 is only 10min.
This reaction uses autoclave hydrogenation, and reaction time needs 1h, uses the common injection hydrogenation reaction time of staying 40～45min, and in this utility model embodiment, reaction time is greatly shortened.
This utility model embodiment product through analyze: conversion ratio be more than 99.9%, unconverted raw material 2,5-dimethoxy-4 '-chloronitrobenzene content be less than 0.1%, hydrogenation products 2,5-dimethoxy-4 '-chloroaniline content about 99.9%, can sell as product, it is not necessary to follow-up subtractive process.
Embodiment 4
Use such as organic intermediate continuously hydrogen adding reactor in embodiment 1, it is blended with the organic intermediate 4 of catalyst, 4 '-dinitrostilbene-2,2 '-disulphonic acid, quantitatively being continuously added in reaction vessel 1 by main material inlet 12, hydrogen is quantitatively continuously added in reaction vessel 1 by hydrogen charging aperture 11；Under circulating pump 5 carries, material in reaction vessel 1, the heat exchanger 6 flowed through successively outside reaction vessel 1 carries out taking heat, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out response system as product and is carried out subsequent treatment, and rest materials enters ejector 2, and ejector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, clash into the most in opposite directions and proceed hydrogenation reaction；In reaction vessel 1, hydrogen floats after separating with liquid and catalyst, and liquid and catalyst continue on through circulating pump 5 circular response.Course of reaction keeps temperature of charge 95～100 DEG C, and material mean residence time in reaction vessel 1 is only 55～60min.
This reaction uses autoclave hydrogenation, and reaction time about 3h, the employing common injection hydrogenation reaction time of staying about 1.5h, in this utility model embodiment, reaction time significantly shortens.
This utility model embodiment product is through analyzing: conversion ratio is more than 99.9%, unconverted raw material 4,4 '-dinitrostilbene-2,2 '-disulfonic acid content is less than 0.1%, hydrogenation products 4,4 '-dinitrostilbene-2,2 '-disulfonic acid (DSD acid) content about 99%, can sell as product, it is not necessary to follow-up subtractive process.
Embodiment 5
Use such as organic intermediate continuously hydrogen adding reactor in embodiment 1, it is blended with the organic intermediate ortho-methylnitrobenzene of catalyst, quantitatively being continuously added in reaction vessel 1 by main material inlet 12, hydrogen is quantitatively continuously added in reaction vessel 1 by hydrogen charging aperture 11；Under circulating pump 5 carries, material in reaction vessel 1, the heat exchanger 6 flowed through successively outside reaction vessel 1 carries out taking heat, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out response system as product and is carried out subsequent treatment, and rest materials enters ejector 2, and ejector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, clash into the most in opposite directions and proceed hydrogenation reaction；In reaction vessel 1, hydrogen floats after separating with liquid and catalyst, and liquid and catalyst continue on through circulating pump 5 circular response.Course of reaction keeps temperature of charge 90～95 DEG C, and material mean residence time in reaction vessel 1 is only 25min.
This reaction uses autoclave hydrogenation, and reaction time about 1.5h, the employing common injection hydrogenation reaction time of staying about 1h, in this utility model embodiment, reaction time significantly shortens.
This utility model embodiment product through analyze: conversion ratio be more than 99.9%, unconverted raw material ortho-methylnitrobenzene be less than 0.1%, hydrogenation products ortho-aminotoluene content about 99.7%, can sell as product, it is not necessary to follow-up rectification purge process.
To sum up, this utility model hydrogenation reactor can significantly improve hydrogenation reaction efficiency and product quality, improves hydrogen utilization ratio in hydrogenation process, reduces solid circulating rate and energy consumption, reduces organic intermediate hydrogenation reaction production cost.
The above is only preferred implementation of the present utility model; it should be pointed out that, for those skilled in the art, without departing under premise of the present utility model; can also make some improvements and modifications, these improvements and modifications also should be regarded as in protection domain of the present utility model.
Claims (3)
- null1. organic intermediate continuously hydrogen adding reactor，Including reaction vessel (1)，The top of described reaction vessel (1) is provided with ejector (2)，For hydrogen and the liquid phase organic intermediate containing solid catalyst particle are mixed to form jet，Hydrogen charging aperture (11) and main material inlet (12) it is additionally provided with on described reaction vessel (1)，It is characterized in that: the gas access of described ejector (2) is connected with the top of described reaction vessel (1) by hydrogen circulation line (3)，The liquid inlet of described ejector (2) is by the fluid connection of principal goods material circulation line (4) with the bottom of described reaction vessel (1)，Described ejector (2) is two，The jet of two ejectors (2) is distributed in described reaction vessel (1) the most in opposite directions，Two strands of jets that ejector (2) is produced can produce percussion flow；Described principal goods material circulation line (4) is provided with circulating pump (5) and heat exchanger (6), and described circulating pump (5) liquid-solid material circulation in reaction vessel (1) provides power, the described heat exchanger (6) liquid-solid material temperature control in principal goods material circulation line (4).
- Organic intermediate continuously hydrogen adding reactor the most according to claim 1, it is characterised in that two jets are positioned at reaction vessel (1) sustained height.
- Organic intermediate continuously hydrogen adding reactor the most according to claim 1, it is characterized in that, it is additionally provided with filter (7) on described principal goods material circulation line (4), for the liquid-solid material of part in principal goods material circulation line (4) is carried out solid-liquid separation, in filter (7), filtrate discharges organic intermediate continuously hydrogen adding reactor.
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| CN201620150081.8U CN205556513U (en) | 2016-02-29 | 2016-02-29 | Continuous hydrogenation ware of organic intermediate |
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| CN201620150081.8U CN205556513U (en) | 2016-02-29 | 2016-02-29 | Continuous hydrogenation ware of organic intermediate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566112A (en) * | 2016-02-29 | 2016-05-11 | 彩客科技（北京）有限公司 | Continuous hydrogenation reaction method of organic intermediates and reactor thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566112A (en) * | 2016-02-29 | 2016-05-11 | 彩客科技（北京）有限公司 | Continuous hydrogenation reaction method of organic intermediates and reactor thereof |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190924 Address after: Cangzhou City, Hebei province 061600 DAZHANGZHUANG south of Dongguang County Patentee after: Choi Yue chemical (Cangzhou) Limited Address before: 101111, Daxing District economic and Technological Development Zone, Beijing No. three road, No. 109, No. 10 hospital building Patentee before: Caike Technology (Beijing) Co., Ltd. |
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| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 061600 Chengnan Da Zhang Zhuang, Dongguang County, Cangzhou City, Hebei Province Patentee after: Hebei caike New Material Technology Co.,Ltd. Address before: 061600 Chengnan Da Zhang Zhuang, Dongguang County, Cangzhou City, Hebei Province Patentee before: TSAKER CHEMICAL (ZHANGZHOU) CO.,LTD. |
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| CP01 | Change in the name or title of a patent holder |