CN102816092B - The device of benzene disulfonic acid between a kind of serialization preparation - Google Patents
The device of benzene disulfonic acid between a kind of serialization preparation Download PDFInfo
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- CN102816092B CN102816092B CN201210317395.9A CN201210317395A CN102816092B CN 102816092 B CN102816092 B CN 102816092B CN 201210317395 A CN201210317395 A CN 201210317395A CN 102816092 B CN102816092 B CN 102816092B
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- sulfonation
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- benzene
- reaction
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- MIAUJDCQDVWHEV-UHFFFAOYSA-N benzene-1,2-disulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1S(O)(=O)=O MIAUJDCQDVWHEV-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 83
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 71
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 39
- 230000008676 import Effects 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 12
- 230000003068 static effect Effects 0.000 claims description 10
- 239000011343 solid material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 30
- 238000000034 method Methods 0.000 abstract description 10
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010960 commercial process Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000029087 digestion Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000006713 insertion reaction Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
This patent discloses the method for benzene disulfonic acid between a kind of serialization preparation.Adopt the sulfonation reactor of designed, designed and tower or tank reactor, connect with the form of connecting, by the industrial production that volume pump controls certain flow, concentration, temperature realize serialization.Enter in the sulfonation reactor of jacketed heating, tower or tank reactor after reaction mass metering, carry out sulfonation reaction under certain temperature, reaction mass enters next conversion unit by carrying side pipe.This patent has simple to operate, and simply, the advantages such as thermo-efficiency is high, clean environment firendly, are suitable for being applied to Resorcinol commercial process for temperature, flow control.
Description
Technical field
This patent relates to the device of benzene disulfonic acid between a kind of serialization preparation.
Background technology
Between benzene disulfonic acid be the important intermediate preparing Resorcinol, and Resorcinol is a kind of important fine chemistry industry organic raw material, is widely used in the fields such as rubber, plastics, medicine, agricultural chemicals, dye well electronic chemical product.
At present, between production traditional in the world, the method for benzene disulfonic acid is sulfonation method, and the most enterprises comprising the states such as China, the U.S., India, Russia all adopts this method.This method with benzene and oleum for raw material, under the effect of catalyzer between sulfonation reaction is produced benzene disulfonic acid (CN101613257A).The sulfonation reaction of aforesaid method is divided into a sulfonation and two stages of two sulfonation react respectively, uses excessive oleum for sulphonating agent.React unreacted sulfuric acid in rear material, a large amount of alkali need have been consumed and neutralize, produce a large amount of solid waste inorganic salt simultaneously.The raw material consumption such as oleum, alkali is very large, and production cost is higher; The a large amount of heat release of neutralization reaction, need provide cooling, and energy consumption waste is serious; Solid waste amount is large, and complex treatment process, environment is unfriendly.Use gaseous state, liquid sulphur trioxide to carry out a sulfonation and two sulfonation, two step of reaction in patent 200910063730.5, cause that operation is longer cannot realize continuous prodution, the single complete equipment utilization ratio adopted is low, and investment is large.The present invention adopts benzene disulfonic acid between liquid sulphur trioxide one-step synthesis, original production reaction two step is synthesized a step, enhances productivity greatly.
Summary of the invention
Technical problem to be solved by this invention is to provide the device of benzene disulfonic acid between a kind of serialization preparation.This patent provides a kind of using liquid sulphur trioxide as sulphonating agent, utilizes high mixed effect one step of sulfonation reactor to complete the method for sulfonation reaction.
Concrete technical scheme is as follows:
Between the serialization preparation that this this patent adopts, benzene disulfonic acid is liquid sulphur trioxide and liquid phenenyl take reaction product as carrier, in sulfonation reactor 3, carry out benzene disulfonic acid between hybrid reaction preparation.All kinds panel element is impacted when liquid sulphur trioxide and liquid phenenyl flow in the mixing tank of sulfonation reactor, increase the velocity slope of fluid telescopic movement or form turbulent flow, " segmentation-position is moved-again converged " during laminar flow, also can produce violent eddy current in section direction, there is very strong shear action in fluid, make fluid split mixing further, reach liquid sulphur trioxide and liquid phenenyl, in middle dispersion, fast, a sulfonation, two sulfonation occur, benzene disulfonic acid between direct reaction generates.
The device of benzene disulfonic acid between the serialization preparation adopted in the method for this reaction, sulfonation reactor 3 and at least plural reactors in series, described sulfonation reactor 3 arranges sulfonation material import A, benzene feedstock import B, raw material sulphur trioxide import C, material outlet D, material outlet D is connected with A reactor 4, sulfonation material import A is connected with second reactor 5, A reactor 4 and second reactor 5 are by side pipe 14, and 15 connect.
Wherein, described reactor 4,5,6 is tank reactor or tower reactor.
Wherein, described reactor 4,5,6 can have stirring or force the auxiliary mixing such as outer circulation.
Wherein, the sulfonation reactor of described series connection 3 and reactor 4,5, between 6, reactor 4,5, connected by side pipe between 6, and under the liquid level of side pipe 14,15 insertion reaction device.
Wherein, between the sulfonation reactor of described series connection and reactor, between reactor, material is carried by fresh feed pump, recycle pump.
Wherein, the feeder for solid materials position of described reactor is arranged on the top of reactor.
Wherein, described sulfonation reactor 3 responds carrier import A, liquid phenenyl import B, liquid sulphur trioxide import C, material outlet D.
Wherein, in described sulfonation reactor 3, the mixed cell of reaction carriers, liquid phenenyl and liquid sulphur trioxide is made up of two sections or more static mixers.
Wherein, the static mixer of sulfonation reactor 3 is SK, SL, SV or SX type.
Wherein, described sulfonation reactor, reactor outer setting have heating, refrigerating unit.
Beneficial effect:
(1) device that the present invention adopts makes to carry out liquid-liquid diphase Forced Mixing in sulfonation reactor, a sulfonation and two sulfonation reactions is realized simultaneously, and operation is simple, can be continuously produced, plant factor is high, less investment.
(2) raw material usage quantity can realize accurate control, avoids wastage of material and postprocessing working procedures, the problem such as solve that production cost is high, the serious and environment of energy consumption waste is unfriendly.
(3) tower, tank reactor top simultaneously, described in this patent are provided with side pipe.
(4) reaction product is accumulated to certain depth, and reaction mass flows through side pipe overflow, adds the residence time of reaction mass, digestion time, thus improves the quality of products and yield.
Accompanying drawing explanation
Fig. 1 is the tower continuous reaction apparatus figure of this patent.
Wherein: 1-benzene test tank; 2-sulphur trioxide test tank; 3-sulfonation reactor; 4-A reactor; 5-second reactor; 6-three reactor; 7-benzene volume pump; 8-sulphur trioxide metering pump; 9-Matter Transfer pump; 11-feeder for solid materials; 13,14,15-reactor discharging side pipe; 12,16 Material pipelines.
Embodiment
Can further illustrate the present invention by the following example, embodiment is unrestricted of the present invention in order to illustrate.Any those of ordinary skill of this area can both be understood these embodiments and not limit the present invention in any way, and can make suitable amendment and parameter transformation and without prejudice to essence of the present invention with depart from scope of the present invention to it.
Benzene and liquid sulphur trioxide are squeezed into according to a certain percentage in sulfonation reactor and autoclave or tower reactor by volume pump and are reacted.Reaction raw materials carries out sulfonation reaction in sulfonation material, and reaction conditions is gentle, and the heat that reaction generates is shifted out by chuck.
Embodiment 1.
A reaction unit in Resorcinol sulfonation workshop section, sulfonation reactor 3 and two or more tower reactor 4,5,6 are connected, the reactor 4,5,6 of series connection is by side pipe 13,14,15 connect, and reaction raw materials is squeezed in sulfonation reactor, tower reactor by volume pump 7,8.Reaction production material squeezes into sulfonation reactor by pump 8 from the bottom of tower reactor 5.Sodium sulfate is added in tower reactor 4 by feeder for solid materials 11.Described sulfonation reactor, two tower reactor 4,5 sidepieces are equipped with side pipe 13,14, and 15 arrive next reactor.Described sulfonation reactor, tower reactor outer setting have heating, refrigerating unit.
Embodiment 2.
The present embodiment is identical with embodiment 1, is distinguished as described.Reaction production material squeezes into sulfonation reactor by pump 8 from the bottom of tower reactor 4.Tower reactor 5 carries out Matter Transfer by pump self.Sodium sulfate is added in tower reactor 5 by feeder for solid materials 11.Described sulfonation reactor, three tower reactors 4,5,6 sidepieces are equipped with side pipe 13, and 14,15 arrive next reactor.
Be 1:2 ~ 2.8 by benzene and sulphur trioxide according to molar ratio with volume pump, input speed controls the speed of 200 ~ 300L/h while to sulfonation reactor charging, sulfonation material is squeezed into sulfonation reactor from the bottom of tower 4 by recycle pump 9, flow control is at 20 ~ 40m3/h, and temperature of reaction controls at 120 ~ 180 DEG C.The speed of sodium sulfate 30 ~ 60kg/h adds in tower reactor 4, and reaction mass overflows to and carries out aging in tower reactor 6, and digestion time controlled at 12 ~ 24 hours.Benzene disulfonic acid content external standard 83 ~ 85% in the middle of sulfonation material.
Embodiment 3.
The device of benzene disulfonic acid between serialization preparation, the reactors in series of sulfonation reactor 3 and more than three, the reactor of series connection is by side pipe 12,13,14,15,16 connections; Described sulfonation reactor 3 arranges sulfonation material import A, benzene feedstock import B, raw material sulphur trioxide import C, material outlet D, sulfonation material import A, benzene feedstock import B are connected with benzene test tank 1, sulphur trioxide test tank 2 respectively, material outlet D is connected with A reactor 4, sulfonation material import A is connected with second reactor 5, and second reactor 5 is connected with three reactor 6.Sulfonation reactor 3 outer setting has heating, refrigerating unit.Reactor 4,5,6 is tank reactor, also arranges agitator.Under side pipe 14,15 between the sulfonation reactor 3 of series connection and reactor, between reactor is arranged on the liquid level of reactor.Feeder for solid materials 11 is arranged on the top of A reactor 4.Mixed cell in sulfonation reactor 3 is made up of two sections or more static mixers, and static mixer is SK, SL, SV or SX type.
Be 1:2 ~ 2.8 by benzene and sulphur trioxide according to molar ratio with volume pump, input speed controls speed at 100 ~ 150L/h simultaneously to sulfonation reactor charging, and the flow control of recycle pump 9 is at 10 ~ 20m3/h.Temperature of reaction controls at 120 ~ 180 DEG C, and the material reacted enters tank reactor 4, and 5 carry out continuation reaction.Reaction mass overflows to and carries out aging in tank reactor 6, and digestion time controlled at 18 ~ 36 hours.Benzene disulfonic acid content 83 ~ 85% in the middle of sulfonation material.
Embodiment 4.
The device of benzene disulfonic acid between serialization preparation, the reactors in series of sulfonation reactor 3 and more than three, the reactor of series connection is by side pipe 12,13,14,15,16 connections; Described sulfonation reactor 3 arranges sulfonation material import A, benzene feedstock import B, raw material sulphur trioxide import C, material outlet D, sulfonation material import A, benzene feedstock import B are connected with benzene test tank 1, sulphur trioxide test tank 2 respectively, material outlet D is connected with A reactor 4, sulfonation material import A is connected with second reactor 5, and second reactor 5 is connected with three reactor 6.Sulfonation reactor 3 outer setting has heating, refrigerating unit.Reactor 4,5,6 is tank reactor, also arranges agitator.Under side pipe 14,15 between the sulfonation reactor 3 of series connection and reactor, between reactor is arranged on the liquid level of reactor.Feeder for solid materials 11 is arranged on the top of A reactor 4.Mixed cell in sulfonation reactor 3 is provided with static mixer, and static mixer is SK type.
Be 1:2 ~ 2.8 by benzene and sulphur trioxide according to molar ratio with volume pump, input speed controls speed at 100 ~ 150L/h simultaneously to sulfonation reactor charging, and the flow control of recycle pump 9 is at 10 ~ 20m3/h.Temperature of reaction controls at 120 ~ 180 DEG C, and the material reacted enters tank reactor 4, and tower reactor 5 carries out continuation reaction.Reaction mass overflows to and carries out aging in tank reactor 6, and digestion time controlled at 12 ~ 6 hours.Benzene disulfonic acid content 81 ~ 83% in the middle of sulfonation material.
Embodiment 5.
The device of benzene disulfonic acid between serialization preparation, the reactors in series of sulfonation reactor 3 and more than three, the reactor of series connection is by side pipe 12,13,14,15,16 connections; Described sulfonation reactor 3 arranges sulfonation material import A, benzene feedstock import B, raw material sulphur trioxide import C, material outlet D, sulfonation material import A, benzene feedstock import B are connected with benzene test tank 1, sulphur trioxide test tank 2 respectively, material outlet D is connected with A reactor 4, sulfonation material import A is connected with second reactor 5, and second reactor 5 is connected with three reactor 6.Sulfonation reactor 3 outer setting has heating, refrigerating unit.Reactor 4,5,6 is tower reactor, also arranges agitator.Under side pipe 14,15 between the sulfonation reactor 3 of series connection and reactor, between reactor is arranged on the liquid level of reactor.Feeder for solid materials 11 is arranged on the top of A reactor 4.Mixed cell in sulfonation reactor 3 is made up of two sections or more static mixers, and static mixer is SX type.
Be 1:2 ~ 2.8 by benzene and sulphur trioxide according to molar ratio with volume pump, input speed controls speed at 100 ~ 150L/h simultaneously to sulfonation reactor charging, and the flow control of recycle pump 9 is at 10 ~ 20m3/h.Temperature of reaction controls at 120 ~ 180 DEG C, and the material reacted enters tower reactor 4, and tower reactor 5 carries out continuation reaction.Reaction mass overflows to and carries out aging in tower reactor 6, and digestion time controlled at 16 ~ 30 hours.Benzene disulfonic acid content 82 ~ 85% in the middle of sulfonation material.
Claims (5)
1. the device of benzene disulfonic acid between serialization preparation, it is characterized in that: sulfonation reactor (3) and at least plural reactors in series, described sulfonation reactor (3) arranges sulfonation material import (A), benzene feedstock import (C), raw material sulphur trioxide import (B), material outlet (D), material outlet (D) is connected with A reactor (4), sulfonation material import (A) is connected with pump (9) through pipeline (12), pump (9) is connected with second reactor (5) through piping (16) again, A reactor (4) and second reactor (5) are connected by side pipe (14),
Described benzene feedstock import (C), raw material sulphur trioxide import (B) are connected with benzene test tank (1), sulphur trioxide test tank (2) respectively;
The feeder for solid materials (11) of described reactor is arranged on the top of A reactor (4);
Mixed cell in described sulfonation reactor (3) is made up of two sections or more static mixers;
The static mixer of sulfonation reactor (3) is SK, SL, SV or SX type.
2. device according to claim 1, is characterized in that: described sulfonation reactor (3) outer setting has heating, refrigerating unit.
3. device according to claim 1, is characterized in that: described A reactor (4) and second reactor (5) are tank reactor or tower reactor.
4. according to the device described in claim 1, it is characterized in that: described A reactor (4) and second reactor (5) arrange and stir or force the auxiliary mixing of outer circulation.
5. the device according to claims 1 to 3 any one, is characterized in that: under the side pipe (14) between the sulfonation reactor (3) of described series connection and A reactor (4), between A reactor (4) and second reactor (5) is arranged on the liquid level of reactor.
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| CN201210317395.9A CN102816092B (en) | 2012-08-31 | 2012-08-31 | The device of benzene disulfonic acid between a kind of serialization preparation |
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| CN104628605B (en) * | 2015-02-16 | 2016-05-25 | 曲靖众一合成化工有限公司 | A kind of naphthalene continuous catalysis method of sulfonating and device thereof |
| CN107963984B (en) * | 2017-07-03 | 2023-12-22 | 襄阳汉元化工有限公司 | Continuous production system and method for p-toluenesulfonic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3198849A (en) * | 1960-07-04 | 1965-08-03 | Ballestra Mario | Method and apparatus for effecting sulfonation |
| CN201694976U (en) * | 2010-06-21 | 2011-01-05 | 曲靖众一精细化工股份有限公司 | Continuous production high-efficiency sulfonation synthesizer |
| CN102188942A (en) * | 2011-04-01 | 2011-09-21 | 沈阳化工大学 | Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor |
| CN202078889U (en) * | 2011-04-01 | 2011-12-21 | 沈阳化工大学 | Production device for preparing 3-nitrobenzenesulfonic acid through tubular nitrobenzene sulfonation reaction |
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| CN102180815B (en) * | 2011-03-23 | 2013-02-27 | 江苏中丹集团股份有限公司 | Process for producing benzene-m-disulfonic acid by using gas-phase sulfonation method |
| CN102180081A (en) * | 2011-04-12 | 2011-09-14 | 重庆长安汽车股份有限公司 | Rear car triangle window assembly |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3198849A (en) * | 1960-07-04 | 1965-08-03 | Ballestra Mario | Method and apparatus for effecting sulfonation |
| CN201694976U (en) * | 2010-06-21 | 2011-01-05 | 曲靖众一精细化工股份有限公司 | Continuous production high-efficiency sulfonation synthesizer |
| CN102188942A (en) * | 2011-04-01 | 2011-09-21 | 沈阳化工大学 | Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor |
| CN202078889U (en) * | 2011-04-01 | 2011-12-21 | 沈阳化工大学 | Production device for preparing 3-nitrobenzenesulfonic acid through tubular nitrobenzene sulfonation reaction |
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Inventor after: Li Liude Inventor after: Zhang Ling Inventor after: Jiang Zhenxiang Inventor after: Ling Xinjian Inventor after: Yang Wei Inventor after: Xue Min Inventor after: Qin Fakun Inventor after: Shi Bo Inventor after: Huang Zhenhong Inventor after: Sun Ruyou Inventor after: Ren Yunhua Inventor after: Dong Zejun Inventor after: Li Hongmei Inventor after: Yao Min Inventor after: Xu Zhuhua Inventor before: Li Liude Inventor before: Shi Bo Inventor before: Bian Xiaobao Inventor before: Wu Youjun Inventor before: Xue Jianjian Inventor before: Dong Zejun |
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Effective date of registration: 20160106 Address after: 225400, No. 8, Tongjiang Road, Yanjiang Economic Development Zone, Taixing, Jiangsu, Taizhou Patentee after: JIANGSU ZHONGDAN CHEMICAL TECHNOLOGY Co.,Ltd. Address before: Taixing City, Jiangsu province 225453 seven Wei Cun, Taizhou City Road West Patentee before: JIANGSU ZHONGDAN GROUP Co.,Ltd. Patentee before: JIANGSU ZHONGDAN CHEMICAL TECHNOLOGY Co.,Ltd. Patentee before: JIANGSU ZHONGDAN PHARMACEUTICAL RESEARCH Co.,Ltd. |
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Denomination of invention: A device for continuous preparation of meta phenylenedisulfonic acid Granted publication date: 20151014 Pledgee: Industrial Bank Co.,Ltd. Taizhou Branch Pledgor: JIANGSU ZHONGDAN CHEMICAL TECHNOLOGY Co.,Ltd. Registration number: Y2024980013262 |