CN105566112A - Continuous hydrogenation reaction method of organic intermediates and reactor thereof - Google Patents
Continuous hydrogenation reaction method of organic intermediates and reactor thereof Download PDFInfo
- Publication number
- CN105566112A CN105566112A CN201610110531.5A CN201610110531A CN105566112A CN 105566112 A CN105566112 A CN 105566112A CN 201610110531 A CN201610110531 A CN 201610110531A CN 105566112 A CN105566112 A CN 105566112A
- Authority
- CN
- China
- Prior art keywords
- organic intermediate
- reaction
- liquid
- hydrogen
- reaction vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000543 intermediate Substances 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 51
- 239000001257 hydrogen Substances 0.000 claims abstract description 46
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007791 liquid phase Substances 0.000 claims abstract description 23
- 239000011949 solid catalyst Substances 0.000 claims abstract description 9
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 90
- 239000000047 product Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 25
- 238000000926 separation method Methods 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000008247 solid mixture Substances 0.000 claims description 8
- 238000009527 percussion Methods 0.000 claims description 7
- 239000011343 solid material Substances 0.000 claims description 7
- UETHPMGVZHBAFB-OWOJBTEDSA-N 4,4'-dinitro-trans-stilbene-2,2'-disulfonic acid Chemical group OS(=O)(=O)C1=CC([N+]([O-])=O)=CC=C1\C=C\C1=CC=C([N+]([O-])=O)C=C1S(O)(=O)=O UETHPMGVZHBAFB-OWOJBTEDSA-N 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- PLAZTCDQAHEYBI-UHFFFAOYSA-N 2-nitrotoluene Chemical group CC1=CC=CC=C1[N+]([O-])=O PLAZTCDQAHEYBI-UHFFFAOYSA-N 0.000 claims description 4
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical group COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 claims description 4
- 238000005191 phase separation Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 230000002459 sustained effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000012071 phase Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005299 abrasion Methods 0.000 abstract description 2
- 238000009903 catalytic hydrogenation reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 13
- 230000035484 reaction time Effects 0.000 description 11
- 239000007921 spray Substances 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 230000001020 rhythmical effect Effects 0.000 description 2
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- RNVCVTLRINQCPJ-UHFFFAOYSA-N o-toluidine Chemical compound CC1=CC=CC=C1N RNVCVTLRINQCPJ-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/303—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by hydrogenation of unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of catalytic hydrogenation of organic intermediates and particularly discloses a continuous hydrogenation reaction method of organic intermediates and a reactor thereof. Two ejectors are coaxially and symmetrically arranged, so that hydrogen, liquid-phase organic intermediates and solid catalyst three-phase materials are mixed to form jet flow and then impact oppositely to generate impact flow, the hydrogenation reaction is enhanced, the hydrogenation reaction efficiency and the product quality can be significantly improved, the utilization rate of the hydrogen in the hydrogenation process is increased, the material circulation quantity and the energy consumption are reduced, the abrasion of the catalyst is reduced, and the production cost is lower.
Description
Technical field
The present invention relates to technical field of fine, especially relate to the technical field of catalytic hydrogenation of organic intermediate.
Background technology
Shortening 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, and more clean and effective.Current priority have developed autoclave interval liquid phase hydrogenation technology, gas-phase fluidized-bed hydrogen addition technology, sprays hydrogenation reaction technology etc., and is all industrially applied.But these technology all show certain deficiency in the actual production of organic intermediate.
Autoclave rhythmic reaction technology is only suitable for the little product of output, and for large-tonnage product, autoclave rhythmic reaction is more difficult realizes automatic control, and 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 temperature of reaction is high, and the by products such as whole process energy consumption is high, tar are many, and holistic cost is high.
Spraying hydrogen addition technology is utilize to spray 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 spraying reaction vessel utilizes flow at high speed to go mutually to entrainment other phases, makes each phase close contact, then dispersed in reaction vessel or suspension, and complete reaction.Spray reaction vessel to form primarily of injector (ejector nozzle) and reaction vessel, spray hydrogen addition technology many employings loop spray reaction vessel, namely utilize recycle pump repeatedly to be circulated by material.
In existing injection hydrogen addition technology, injector is located at single lower spray in reaction vessel, only react in injector by recycle pump recycle stock, suction hydrogen, fast due to material flow, in injector reaction time is short, this causes the circulation needing material a large amount of, can ensure to provide enough reaction times in injector, due to the iterative cycles that material is a large amount of, overall operation power consumption is very high, the wearing and tearing of catalyzer simultaneously increase, cause difficulty to the filtration of catalyzer, the production cost of Total Product is high.
Summary of the invention
The technical problem to be solved in the present invention is to provide organic intermediate continuous hydrogenation reaction method and 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 the problems of the technologies described above, the technical solution used in the present invention is: organic intermediate continuous hydrogenation reaction method, comprise continuous print and the liquid phase organic intermediate and hydrogen that contain solid catalyst particle, with the mixing of the form of jet, organic intermediate hydrogenation reaction is occurred, described jet is two strands, coaxially clash in opposite directions after jet is sprayed, form percussion flow and proceed hydrogenation reaction; Matter Transfer carries out above reaction;
Described liquid phase organic intermediate is the solution that neat liquid organic intermediate or organic intermediate are dissolved in solvent;
In reaction gained system, hydrogen floats and is separated with liquid-solid mixture, and liquid-solid mixture, again through solid-liquid separation, contains product organic intermediate hydrogenation products in gained liquid phase separation thing.
Further, described Matter Transfer mode is: part liquid-solid mixture is through solid-liquid separation, gained liquid phase separation thing flows out reactive system as product, hydrogen and remaining fluid solid mixture mix with the hydrogen newly added with containing the liquid phase organic intermediate of solid catalyst particle respectively, then with the form circulating reaction of jet.
As preferably, described liquid phase organic intermediate is dimethyl maleate, and reaction process keeps temperature of charge 120 ~ 130 DEG C.
As preferably, described liquid phase organic intermediate is 4,4 '-dinitrostilbene-2,2 '-disulphonic acid, and reaction process keeps temperature of charge 90 ~ 95 DEG C.
As preferably, described liquid phase organic intermediate is 4,4 '-dinitrostilbene-2,2 '-disulphonic acid, and reaction process keeps temperature of charge 95 ~ 100 DEG C.
As preferably, described liquid phase organic intermediate is Ortho Nitro Toluene, and reaction process keeps temperature of charge 90 ~ 95 DEG C.
Organic intermediate continuous hydrogenation reactor, it comprises reaction vessel, the top of described reaction vessel is provided with injector, for being mixed to form jet by hydrogen with containing the liquid phase organic intermediate of solid catalyst particle, described reaction vessel is also provided with hydrogen feed mouth and main material inlet, the gas inlet of described injector is communicated with the top of described reaction vessel by hydrogen recycle pipeline, the liquid inlet of described injector is by the fluid connection of the bottom of principal goods material circulation line and described reaction vessel, described injector is two, the jet orifice of two injectors is coaxially distributed in described reaction vessel in opposite directions, two strands of jets that injector is produced can produce percussion flow, described principal goods material circulation line is provided with recycle pump and interchanger, and described recycle pump is used for liquid-solid material circulation in reaction vessel provides power, and described interchanger is used for the liquid-solid material temperature control in principal goods material circulation line.
As preferably, two jet orifices are positioned at reaction vessel sustained height.
Further, described principal goods material circulation line is also provided with strainer, for carrying out solid-liquid separation to the liquid-solid material of part in principal goods material circulation line, in strainer, filtrate discharges described spraying cycle impact flow reactor.
The beneficial effect adopting technique scheme to produce is:
Organic intermediate continuous hydrogenation reactor provided by the invention and method, compared with prior art, its distinguishing feature is, on the reaction vessel in space, portion, coaxially opposed two injectors, after material flows out injector tip, clash in opposite directions.According to the principle of percussion flow, after material clashes in opposite directions, can fully promote that multi phase interface upgrades, strengthening gas-liquid-solid multiphase mass transfer, thoroughly eliminates external diffusion impact, makes reaction not by mass transport limitation.Under the effect of percussion flow principle, this makes material after outflow jet end, still continuing hydrogenation reaction by clashing into the renewal of promotion multi phase interface, in single cycle, obviously extending reaction time.These characteristics significantly can improve product quality, and improve hydrogenation process hydrogen utilization efficiency, reduce hydrogen circulation amount, thus reduce hydrogenation process energy consumption, total procedural strength is high, and space-time production capacity is large, and Total Product production cost is low.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of embodiment of organic intermediate continuous hydrogenation reactor of the present invention.
Wherein, 1, reaction vessel; 2, injector; 3, hydrogen recycle pipeline; 4, principal goods material circulation line; 5, recycle pump; 6, interchanger; 7, strainer; 11, hydrogen feed mouth; 12, main material inlet; 61, circulating water outlet; 62, circulating water intake; 71, filtrate outlet.
Embodiment
Embodiment 1
Organic intermediate continuous hydrogenation reactor, see Fig. 1, it comprises reaction vessel 1, two injectors 2 that reaction vessel 1 top coaxial-symmetrical is arranged, injector 2 is for being mixed to form jet by hydrogen with containing the liquid phase organic intermediate of solid catalyst particle, the jet orifice of two injectors 2 is coaxially distributed in reaction vessel 1 in opposite directions, and two strands of jets that injector 2 is produced can produce percussion flow; Reaction vessel 1 is also provided with hydrogen feed mouth 11 and main material inlet 12, the gas inlet of injector 2 is communicated with the top of reaction vessel 1 by hydrogen recycle pipeline 3, the liquid inlet of injector 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 recycle pump 5 and interchanger 6, recycle pump 5 provides power for material circulation liquid-solid in reaction vessel 1, and interchanger 6 is for the liquid-solid material temperature control in principal goods material circulation line 4.Interchanger 6 adopts recirculated water as heat transferring medium, and it is respectively equipped with circulating water outlet 61 and circulating water intake 62.
As preferably, two jet orifices are positioned horizontally in sustained height in reaction vessel 1.
To the further improvement of the technical program, principal goods material circulation line 4 is also provided with strainer 7, for carrying out solid-liquid separation to the liquid-solid material of part in principal goods material circulation line 4, in strainer 7, filtrate discharges spraying cycle impact flow reactor by filtrate outlet 71.
Embodiment 2
Adopt as organic intermediate continuous hydrogenation reactor in embodiment 1, the organic intermediate dimethyl maleate of catalyzer will be mixed with, quantitatively add in reaction vessel 1 continuously by main material inlet 12, hydrogen quantitatively adds in reaction vessel 1 by hydrogen feed mouth 11 continuously; Under recycle pump 5 is carried, material in reaction vessel 1, the interchanger 6 flowed through successively outside reaction vessel 1 carries out heat-obtaining, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out reactive system as product and is carried out subsequent disposal, and rest materials enters injector 2, and injector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, coaxially clash in opposite directions and proceed hydrogenation reaction; In reaction vessel 1, float after hydrogen and liquid and catalyst separating, liquid and catalyzer continue through recycle pump 5 circulating reaction.Reaction process keeps temperature of charge 120 ~ 130 DEG C, and the mean residence time of material in reaction vessel 1 is only 15min.
This reaction adopts autoclave hydrogenation, and reaction time needs 2h, and adopt common injection hydrogenation reaction residence time 1h, in the embodiment of the present invention, reaction time significantly shortens.
Embodiment of the present invention reaction product is by analysis: transformation efficiency reaches 99.9%, and unconverted starting material dimethyl maleate content about 0.1%, hydrogenation products dimethyl succinate content about 99.8%, can sell as product, without the need to follow-up treating process.
Embodiment 3
Adopt as organic intermediate continuous hydrogenation reactor in embodiment 1, the organic intermediate 2 of catalyzer will be mixed with, 5-dimethoxy-4 '-chloronitrobenzene solution, quantitatively adds in reaction vessel 1 by main material inlet 12 continuously, and hydrogen quantitatively adds in reaction vessel 1 by hydrogen feed mouth 11 continuously; Under recycle pump 5 is carried, material in reaction vessel 1, the interchanger 6 flowed through successively outside reaction vessel 1 carries out heat-obtaining, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out reactive system as product and is carried out subsequent disposal, and rest materials enters injector 2, and injector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, coaxially clash in opposite directions and proceed hydrogenation reaction; In reaction vessel 1, float after hydrogen and liquid and catalyst separating, liquid and catalyzer continue through recycle pump 5 circulating reaction.Reaction process keeps temperature of charge 90 ~ 95 DEG C, and the mean residence time of material in reaction vessel 1 is only 10min.
This reaction adopts autoclave hydrogenation, and reaction time needs 1h, adopts the common injection hydrogenation reaction residence time 40 ~ 45min, and in the embodiment of the present invention, reaction time significantly shortens.
Embodiment of the present invention reaction product is by analysis: transformation efficiency is greater than 99.9%, and unconverted starting material 2,5-dimethoxy-4 's-chloronitrobenzene content is lower than 0.1%, hydrogenation products 2,5-dimethoxy-4 '-chloroaniline content about 99.9%, can sell as product, without the need to follow-up treating process.
Embodiment 4
Adopt as organic intermediate continuous hydrogenation reactor in embodiment 1, the organic intermediate 4 of catalyzer will be mixed with, 4 '-dinitrostilbene-2,2 '-disulphonic acid, quantitatively add in reaction vessel 1 continuously by main material inlet 12, hydrogen quantitatively adds in reaction vessel 1 by hydrogen feed mouth 11 continuously; Under recycle pump 5 is carried, material in reaction vessel 1, the interchanger 6 flowed through successively outside reaction vessel 1 carries out heat-obtaining, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out reactive system as product and is carried out subsequent disposal, and rest materials enters injector 2, and injector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, coaxially clash in opposite directions and proceed hydrogenation reaction; In reaction vessel 1, float after hydrogen and liquid and catalyst separating, liquid and catalyzer continue through recycle pump 5 circulating reaction.Reaction process keeps temperature of charge 95 ~ 100 DEG C, and the mean residence time of material in reaction vessel 1 is only 55 ~ 60min.
This reaction adopts autoclave hydrogenation, and reaction time is about 3h, adopts the common injection hydrogenation reaction residence time to be about 1.5h, and in the embodiment of the present invention, reaction time significantly shortens.
Embodiment of the present invention product is by analysis: transformation efficiency is greater than 99.9%, unconverted starting material 4,4 '-dinitrostilbene-2,2 '-disulfonic acid content is lower than 0.1%, hydrogenation products 4,4 '-dinitrostilbene-2,2 '-disulfonic acid (DSD acid) content about 99%, can sell as product, without the need to follow-up treating process.
Embodiment 5
Adopt as organic intermediate continuous hydrogenation reactor in embodiment 1, the organic intermediate Ortho Nitro Toluene of catalyzer will be mixed with, quantitatively add in reaction vessel 1 continuously by main material inlet 12, hydrogen quantitatively adds in reaction vessel 1 by hydrogen feed mouth 11 continuously; Under recycle pump 5 is carried, material in reaction vessel 1, the interchanger 6 flowed through successively outside reaction vessel 1 carries out heat-obtaining, flow through filter 7 and carry out part solid-liquid separation, filtrate is flowed out reactive system as product and is carried out subsequent disposal, and rest materials enters injector 2, and injector 2 aspirates circulating hydrogen mixing and reacts, after material outflow jet 2 end, coaxially clash in opposite directions and proceed hydrogenation reaction; In reaction vessel 1, float after hydrogen and liquid and catalyst separating, liquid and catalyzer continue through recycle pump 5 circulating reaction.Reaction process keeps temperature of charge 90 ~ 95 DEG C, and the mean residence time of material in reaction vessel 1 is only 25min.
This reaction adopts autoclave hydrogenation, and reaction time is about 1.5h, adopts the common injection hydrogenation reaction residence time to be about 1h, and in the embodiment of the present invention, reaction time significantly shortens.
Embodiment of the present invention product is by analysis: transformation efficiency is greater than 99.9%, and unconverted starting material Ortho Nitro Toluene is lower than 0.1%, and hydrogenation products Ortho Toluidine content about 99.7%, can sell as product, without the need to follow-up rectifying purge process.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, and under the premise of not departing from the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (9)
1. organic intermediate continuous hydrogenation reaction method, comprise continuous print and the liquid phase organic intermediate and hydrogen that contain solid catalyst particle, with the mixing of the form of jet, organic intermediate hydrogenation reaction is occurred, it is characterized in that, described jet is two strands, coaxially clash in opposite directions after jet is sprayed, form percussion flow and proceed hydrogenation reaction; Matter Transfer carries out above reaction;
Described liquid phase organic intermediate is the solution that neat liquid organic intermediate or organic intermediate are dissolved in solvent;
In reaction gained system, hydrogen floats and is separated with liquid-solid mixture, and liquid-solid mixture, again through solid-liquid separation, contains product organic intermediate hydrogenation products in gained liquid phase separation thing.
2. organic intermediate continuous hydrogenation reaction method according to claim 1, it is characterized in that, described Matter Transfer mode is: part liquid-solid mixture is through solid-liquid separation, gained liquid phase separation thing flows out reactive system as product, hydrogen and remaining fluid solid mixture mix with the hydrogen newly added with containing the liquid phase organic intermediate of solid catalyst particle respectively, then with the form circulating reaction of jet.
3. organic intermediate continuous hydrogenation reaction method according to claim 1, is characterized in that, described liquid phase organic intermediate is dimethyl maleate, and reaction process keeps temperature of charge 120 ~ 130 DEG C.
4. organic intermediate continuous hydrogenation reaction method according to claim 1, is characterized in that, described liquid phase organic intermediate is 2,5-dimethoxy-4 '-chloronitrobenzene solution, and reaction process keeps temperature of charge 90 ~ 95 DEG C.
5. organic intermediate continuous hydrogenation reaction method according to claim 1, is characterized in that, described liquid phase organic intermediate is 4,4 '-dinitrostilbene-2,2 '-disulphonic acid, and reaction process keeps temperature of charge 95 ~ 100 DEG C.
6. organic intermediate continuous hydrogenation reaction method according to claim 1, is characterized in that, described liquid phase organic intermediate is Ortho Nitro Toluene, and reaction process keeps temperature of charge 90 ~ 95 DEG C.
7. organic intermediate continuous hydrogenation reactor, comprise reaction vessel (1), the top of described reaction vessel (1) is provided with injector (2), for being mixed to form jet by hydrogen with containing the liquid phase organic intermediate of solid catalyst particle, described reaction vessel (1) is also provided with hydrogen feed mouth (11) and main material inlet (12), it is characterized in that: the gas inlet of described injector (2) is communicated with the top of described reaction vessel (1) by hydrogen recycle pipeline (3), the liquid inlet of described injector (2) is by the fluid connection of principal goods material circulation line (4) with the bottom of described reaction vessel (1), described injector (2) is two, the jet orifice of two injectors (2) is coaxially distributed in described reaction vessel (1) in opposite directions, two strands of jets that injector (2) is produced can produce percussion flow, described principal goods material circulation line (4) is provided with recycle pump (5) and interchanger (6), described recycle pump (5) provides power for material circulation liquid-solid in reaction vessel (1), and described interchanger (6) is for the liquid-solid material temperature control in principal goods material circulation line (4).
8. organic intermediate continuous hydrogenation reactor according to claim 7, is characterized in that, two jet orifices are positioned at reaction vessel (1) sustained height.
9. organic intermediate continuous hydrogenation reactor according to claim 7, it is characterized in that, described principal goods material circulation line (4) is also provided with strainer (7), for carrying out solid-liquid separation to the liquid-solid material of part in principal goods material circulation line (4), in strainer (7), filtrate discharges described spraying cycle impact flow reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110531.5A CN105566112A (en) | 2016-02-29 | 2016-02-29 | Continuous hydrogenation reaction method of organic intermediates and reactor thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110531.5A CN105566112A (en) | 2016-02-29 | 2016-02-29 | Continuous hydrogenation reaction method of organic intermediates and reactor thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105566112A true CN105566112A (en) | 2016-05-11 |
Family
ID=55876822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610110531.5A Pending CN105566112A (en) | 2016-02-29 | 2016-02-29 | Continuous hydrogenation reaction method of organic intermediates and reactor thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105566112A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069491A (en) * | 2016-11-18 | 2018-05-25 | 北京化工大学 | For the electrocatalytic oxidation method and reaction unit of used water difficult to degradate |
| CN108579491A (en) * | 2018-03-15 | 2018-09-28 | 青岛科技大学 | A kind of percussion flow spraying mixer |
| CN110152588A (en) * | 2019-04-19 | 2019-08-23 | 张其凯 | Liquid non-submersion formula impinging stream reaction device and reaction method |
| CN110756120A (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 and reaction process |
| CN113651664A (en) * | 2020-05-12 | 2021-11-16 | 中国石油化工股份有限公司 | Method for conversion of benzyl alcohol |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287365A (en) * | 1977-03-25 | 1981-09-01 | Bayer Aktiengesellschaft | Reduction of aromatic nitro compounds with Raney nickel catalyst |
| CN102070448A (en) * | 2011-02-22 | 2011-05-25 | 湖南长岭石化科技开发有限公司 | Method for preparing dimethyl succinate |
| CN203329731U (en) * | 2013-02-06 | 2013-12-11 | 武汉工程大学 | Vertical impinging stream reactor |
| CN104098474A (en) * | 2014-07-28 | 2014-10-15 | 淮安嘉诚高新化工股份有限公司 | Device and method for producing methyl aniline through performing continuous liquid-phase catalytic hydrogenation reduction on nitrotoluene |
| CN205556513U (en) * | 2016-02-29 | 2016-09-07 | 彩客科技（北京）有限公司 | Continuous hydrogenation ware of organic intermediate |
-
2016
- 2016-02-29 CN CN201610110531.5A patent/CN105566112A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287365A (en) * | 1977-03-25 | 1981-09-01 | Bayer Aktiengesellschaft | Reduction of aromatic nitro compounds with Raney nickel catalyst |
| CN102070448A (en) * | 2011-02-22 | 2011-05-25 | 湖南长岭石化科技开发有限公司 | Method for preparing dimethyl succinate |
| CN203329731U (en) * | 2013-02-06 | 2013-12-11 | 武汉工程大学 | Vertical impinging stream reactor |
| CN104098474A (en) * | 2014-07-28 | 2014-10-15 | 淮安嘉诚高新化工股份有限公司 | Device and method for producing methyl aniline through performing continuous liquid-phase catalytic hydrogenation reduction on nitrotoluene |
| CN205556513U (en) * | 2016-02-29 | 2016-09-07 | 彩客科技（北京）有限公司 | Continuous hydrogenation ware of organic intermediate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069491A (en) * | 2016-11-18 | 2018-05-25 | 北京化工大学 | For the electrocatalytic oxidation method and reaction unit of used water difficult to degradate |
| CN108069491B (en) * | 2016-11-18 | 2021-06-25 | 北京化工大学 | Electrocatalytic oxidation method and reaction device for refractory wastewater |
| CN108579491A (en) * | 2018-03-15 | 2018-09-28 | 青岛科技大学 | A kind of percussion flow spraying mixer |
| CN110756120A (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 and reaction process |
| CN110152588A (en) * | 2019-04-19 | 2019-08-23 | 张其凯 | Liquid non-submersion formula impinging stream reaction device and reaction method |
| CN110152588B (en) * | 2019-04-19 | 2021-07-13 | 张其凯 | Liquid non-submerged impinging stream reaction device and reaction method |
| CN113651664A (en) * | 2020-05-12 | 2021-11-16 | 中国石油化工股份有限公司 | Method for conversion of benzyl alcohol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105566112A (en) | Continuous hydrogenation reaction method of organic intermediates and reactor thereof | |
| CN101735047B (en) | A kind of technique of continuous production sec-butyl acetate | |
| CN103936559B (en) | The method of continuous prodution Resorcinol | |
| CN102241558B (en) | Reaction device and process for preparing cyclohexene by selectively hydrogenating benzene | |
| CN102875469B (en) | Method for preparing caprolactam through adopting radial moving bed reactor | |
| CN101696024B (en) | Stirring-free method and device for producing sodium nitrate through continuous conversion | |
| CN105237409A (en) | Method used for reductive amination using jet reactor | |
| CN101804317A (en) | Multiphase catalysis tower type collision current reactor | |
| CN107056670B (en) | A kind of preparation method of two tertiary base peroxide | |
| CN103708426A (en) | Device for producing hydrogen peroxide by adopting anthraquinone process | |
| CN112499592A (en) | System and process for preparing hydrogen peroxide based on anthraquinone method | |
| CN106622045A (en) | Device and method for improving reaction efficiency of bubble tower by using micro-nano bubbles | |
| CN205556513U (en) | Continuous hydrogenation ware of organic intermediate | |
| CN102285861A (en) | Reaction device for preparing cyclohexene by heterogeneous catalysis of selective hydrogenation of benzene with liquid phase method | |
| CN110183370B (en) | Industrial production method of N-ethyl pyrrolidone | |
| CN203699908U (en) | Anthraquinone process hydrogen peroxide production device | |
| CN119346054A (en) | A method and device for preparing CLT acid by pipeline continuous catalytic hydrogenation reduction | |
| CN104549087A (en) | Sectional feeding type alkylation reactor and alkylation reaction method | |
| CN212595615U (en) | Reaction unit and system for synthesizing acetic acid by methanol carbonyl | |
| CN202237798U (en) | Separation device for catalyst in benzene partial hydrogenation reaction in production process of cyclohexanone | |
| CN109735364A (en) | A kind of residual hydrogenation equipment and technique | |
| CN106146441A (en) | A kind of preparation technology of furfural | |
| CN204939338U (en) | A kind of reactive system of coking crude benzene hydrogenation technique | |
| CN208824453U (en) | The isothermal fixed bed tandem reactor of propylene oxide is prepared for HPPO method | |
| CN204981700U (en) | Equipment system of production 2 - ethyl anthraquinone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160511 |
|
| RJ01 | Rejection of invention patent application after publication |