CN103432978B - Sulfonation reactor and use method thereof - Google Patents
Sulfonation reactor and use method thereof Download PDFInfo
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- CN103432978B CN103432978B CN201310249751.2A CN201310249751A CN103432978B CN 103432978 B CN103432978 B CN 103432978B CN 201310249751 A CN201310249751 A CN 201310249751A CN 103432978 B CN103432978 B CN 103432978B
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- reaction
- pipe
- flow
- valve
- circulating line
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- 238000006277 sulfonation reaction Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 95
- 239000000523 sample Substances 0.000 claims description 32
- 239000000498 cooling water Substances 0.000 claims description 15
- 210000004916 vomit Anatomy 0.000 claims description 15
- 230000008673 vomiting Effects 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 14
- 239000002826 coolant Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 8
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 16
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract description 11
- 238000009423 ventilation Methods 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a sulfonation reactor and a use method thereof, and belongs to the field of sulfonation reaction equipment. The sulfonation reactor comprises a sealed reaction container, wherein the top of the reaction container is provided with a plurality of material inlet pipes, the bottom of the reaction container is provided with a material outlet, the top of the reaction container is vertically provided with an emptying pipe, and is further vertically provided with a co-current pipe, the top of the co-current pipe is sealed and is provided with a ventilation pipe, the side wall of the co-current pipe is provided with a material inlet, a circulation pipeline is connected and arranged between the material inlet and the material outlet, one circulation pipeline end close to the material outlet is provided with a material discharge valve, the circulation pipeline is further provided with a material feeding pipe, and the material feeding pipe is provided with a material feeding valve. According to the sulfonation reactor with the structure, during use, a material is subjected to a circulation reaction in the reactor through the circulation pipeline so as to increase a sulfonic acid concentration and improve product quality, and the sulfonation reactor is provided with a thermometer casing and a temperature control device so as to ensure a reaction rate and reaction quality of the sulfonation reaction.
Description
Technical field
The present invention relates to sulfonating reaction apparatus field, particularly a kind of sulfonation reactor, the invention still further relates to a kind of method using sulfonation reactor.
Background technology
Sulfonation reactor has pot type and the large class of membrane type two.Film reactor is divided into again monofilm, two film and two-tube three kinds, and wherein dual-membrane type sulphonator uses maximum a kind of film sulfonators at present, and whole reactor is divided into three parts: top is distribution portion, forms liquid film in order to distribute material; Centre is reactive moieties, and material completes reaction at annular space; Bottom is tail gas separation part, and product sulfonic acid is separated at this with tail gas, the sulfonation reactor of this structure, product sulfonic acid, and reaction is thorough not, cannot ensure product quality.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of sulfonation reactor of reaction capable of circulation, present invention also offers a kind of method using this sulfonation reactor for this reason.
For achieving the above object, the invention provides following technical scheme: a kind of sulfonation reactor, comprise the reaction vessel of sealing, reaction vessel top is provided with multiple feed pipe, reaction container bottom is provided with discharging opening, the plan vertical of reaction vessel is provided with blow-down pipe, reaction vessel top is also vertically provided with and flows pipe, and flow pipe top seal and be provided with breather pipe, and flow pipe sidewall and be provided with charging aperture, circulating line is connected with between charging aperture and discharging opening, one end near discharging opening on circulating line is provided with baiting valve, circulating line is also provided with vomit pipe, vomit pipe is provided with baiting valve, reaction vessel is provided with reaction temperature control device, and flow pipeline and to be provided with and flow cooling device.
Preferably, described reaction temperature control device comprises the reaction jacket pipe being socketed on reaction vessel lateral wall, steam entry and reaction coolant outlet is provided with above the lateral wall of reaction jacket pipe, steam outlet and reaction cooling water inlet is provided with below the lateral wall of reaction jacket pipe, be provided with the reaction cooling water circulation pipeline of coupled reaction cooling water inlet and reaction coolant outlet in reaction jacket pipe, in reaction jacket pipe, be also provided with the water steam pipeline connecting steam entry and steam outlet.
Preferably, described and flow cooling device comprise be socketed on and flow pipeline lateral wall and flow jacket pipe, and be provided with above the lateral wall flowing jacket pipe and flow coolant outlet, and be provided with below the lateral wall flowing jacket pipe and flow cooling water inlet.
Preferably, described circulating line is provided with circulating pump, and circulating pump is arranged on the circulating line between discharging opening and vomit pipe, circulating line is also provided with and flows valve, and flows on circulating line that valve is arranged on away from vomit pipe side.
Preferably, described circulating line is provided with sample tap, and sample tap is connected with probe tube, and probe tube is provided with sample valve.
Preferably, described circulating line is provided with shower nozzle near one end of charging aperture, and shower nozzle is positioned at and flows pipe, and shower nozzle is arranged vertically downward.
Preferably, described and flow pipe sidewall and be provided with observation panel, observation panel is coated with glass.
Preferably, described reaction vessel is provided with agitator in the axial direction.
Preferably, described reaction vessel is provided with the thermometer boss passing perpendicularly through top.
Use a method for sulfonation reactor, comprise the steps:
1) sulfonation reactor is checked, close baiting valve, baiting valve and sample valve, open and flow valve;
2) add reaction mass by feed pipe, add sulfur trioxide by breather pipe;
3) open agitator, and thermometer is injected thermometer boss;
4) according to the number of degrees of thermometer test, use reaction temperature control device and also flow cooling device regulate reaction temperature;
5) react a period of time, open baiting valve, reactant liquor enters reactor by circulating line backflow;
6) open sample valve, reactant liquor is sampled, close sample valve, sample liquid is detected;
7) when testing result is up to standard, close and flow valve, opening baiting valve.
The beneficial effect of above technical scheme is adopted to be: the sulfonation reactor of structure of the present invention, comprise the reaction vessel of sealing, reaction vessel top is provided with multiple feed pipe, reaction container bottom is provided with discharging opening, the plan vertical of reaction vessel is provided with blow-down pipe, reaction vessel top is also vertically provided with and flows pipe, reaction mass passes through feed pipe, sulfur trioxide gas passes through and flows pipe to enter reaction vessel, there is sulfonating reaction, reactor bottom and and flow between pipe and be provided with circulating line, circulating line is provided with the vomit pipe of band valve, be provided with probe tube and the circulating pump of band valve, product sulfonic acid is back in reactor by circulating pump along circulating line, make sulfonic acid can in reactor repeatedly circular response, by probe tube, the sulfonic acid blowing in reaction is detected in cyclic process, after sulfonic acid is up to standard, by vomit pipe, sulfonic acid is put into container, circulating line one end is stretched into and is flowed in pipe, be provided with shower nozzle vertically downward, the sulfonic acid of circulation passes through shower nozzle, reactor is entered in vaporific, material is incorporated in reactant liquor fast, increase its reaction rate, and flow pipe and be provided with observation panel, be used for observing the mobility of material and viscosity.
Reaction vessel is provided with agitator in the axial direction, be used for increasing the reaction rate of whole reaction, reaction vessel is provided with the thermometer boss passing perpendicularly through top and is used for installing thermometer, variations in temperature in monitoring course of reaction, reaction vessel is provided with reaction temperature control device, it is the reaction jacket pipe being socketed on reaction vessel lateral wall, inside be provided with cooling water circulation pipeline and water steam pipeline, sulfonation is exothermic reaction, cooling is needed during low-temperature sulfonation, high temperature sulfonation then needs heating and thermal insulation, and flow pipeline and to be provided with and flow cooling device, be socketed on and flow pipeline lateral wall and flow jacket pipe, sulfonic acid circulating reflux being entered to reactor cools.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is top view of the present invention.
Wherein, 1--reactor, 2--feed pipe, 3--discharging opening, 4--blow-down pipe, 5--also flows pipe, 6--breather pipe, 7--charging aperture, 8--circulating line, 9--baiting valve, 10--vomit pipe, 11--baiting valve, 12--reacts clamp cover, 13--steam entry, 14--steam outlet, 15--reacts cooling water inlet, 16--reacts coolant outlet, 17--also flows jacket pipe, 18--also flows cooling water inlet, 19--also flows coolant outlet, 20--circulating pump, 21--also flows valve, 22--sample tap, 23--probe tube, 24-sample valve, 25--shower nozzle, 26--observation panel, 27--agitator, 28--thermometer boss.
Detailed description of the invention
The preferred embodiment of the present invention is described in detail below in conjunction with accompanying drawing.
Fig. 1 and Fig. 2 shows the detailed description of the invention of a kind of sulfonation reactor of the present invention: this sulfonation reactor, comprise the reactor 1 of sealing, reactor 1 top is provided with multiple feed pipe 2, discharging opening 3 is provided with bottom reactor 1, the plan vertical of reactor 1 is provided with blow-down pipe 4, reactor 1 top is also vertically provided with and flows pipe 5, and flow pipe 5 top seal and be provided with breather pipe 6, and flow pipe 5 sidewall and be provided with charging aperture 7, circulating line 8 is connected with between charging aperture 7 and discharging opening 3, one end near discharging opening 7 on circulating line 8 is provided with baiting valve 9, circulating line 8 is also provided with vomit pipe 10, vomit pipe 10 is provided with baiting valve 11, reactor 1 is provided with reaction temperature control device, and flow pipe 5 and to be provided with and flow cooling device, reaction temperature control device comprises the reaction jacket pipe 12 being socketed on reactor 1 lateral wall, steam entry 13 and reaction coolant outlet 16 is provided with above the lateral wall of reaction jacket pipe 12, steam outlet 14 and reaction cooling water inlet 15 is provided with below the lateral wall of reaction jacket pipe 12, the reaction cooling water circulation pipeline of coupled reaction cooling water inlet 15 and reaction coolant outlet 16 is provided with in reaction jacket pipe 12, the water steam pipeline connecting steam entry 13 and steam outlet 14 is also provided with in reaction jacket pipe 12, and flow cooling device comprise be socketed on and flow pipe 5 lateral wall and flow jacket pipe 17, and be provided with above the lateral wall flowing jacket pipe 17 and flow coolant outlet 19, and be provided with below the lateral wall flowing jacket pipe 17 and flow cooling water inlet 18, circulating line 8 is provided with circulating pump 20, circulating pump 20 is arranged on the circulating line 8 between discharging opening 3 and vomit pipe 10, circulating line 8 is also provided with and flows valve 21, and flow on circulating line 8 that valve 21 is arranged on away from vomit pipe 10 side, circulating line 8 is provided with sample tap 22, sample tap 22 is connected with probe tube 23, probe tube 23 is provided with sample valve 24, circulating line 8 is provided with shower nozzle 25 near one end of charging aperture 7, shower nozzle 25 is positioned at and flows pipe 5, shower nozzle 25 is arranged vertically downward, and flow pipe 5 sidewall and be provided with observation panel 26, observation panel 26 is coated with glass, reactor 1 is provided with agitator 27 in the axial direction, reactor 2 is provided with the thermometer boss 28 passing perpendicularly through top.
Use a method for sulfonation reactor, comprise the steps: first to check reactor 1, close baiting valve 9, baiting valve 11 and sample valve 24, open and flow valve 21; Secondly add reaction mass by feed pipe 2, add sulfur trioxide by breather pipe 6, react in reactor 1; Open agitator 27, and thermometer is injected thermometer boss 28; According to the number of degrees of thermometer test, use reaction temperature control device and also flow cooling device regulate reaction temperature; After reaction a period of time, open baiting valve 9, reactant liquor enters reactor 1 by the pressurization of circulating pump 20 along circulating line 8 backflow; Again open sample valve 24, reactant liquor is sampled, close sample valve 24, sample liquid is detected; Finally when testing result is up to standard, close and flow valve 21, opening baiting valve 24, reactant liquor is flowed in container along vomit pipe 10 by the pressurization of circulating pump 20.
The beneficial effect of above technical scheme is adopted to be: the sulfonation reactor of this invention structure, make material, in reactor, circular response occur by circulating line, the concentration improving sulfonic acid improves quality, sulfonation reactor is provided with thermometer boss and temperature control equipment, ensure that reaction rate and the reaction mass of sulfonating reaction.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (2)
1. a sulfonation reactor, it is characterized in that: the reaction vessel comprising sealing, reaction vessel top is provided with multiple feed pipe, reaction container bottom is provided with discharging opening, the plan vertical of reaction vessel is provided with blow-down pipe, reaction vessel top is also vertically provided with and flows pipe, and flow pipe top seal and be provided with breather pipe, and flow pipe sidewall and be provided with charging aperture, circulating line is connected with between charging aperture and discharging opening, one end near discharging opening on circulating line is provided with baiting valve, circulating line is also provided with vomit pipe, vomit pipe is provided with baiting valve, reaction vessel is provided with reaction temperature control device, and flow pipeline and to be provided with and flow cooling device, described reaction temperature control device comprises the reaction jacket pipe being socketed on reaction vessel lateral wall, steam entry and reaction coolant outlet is provided with above the lateral wall of reaction jacket pipe, steam outlet and reaction cooling water inlet is provided with below the lateral wall of reaction jacket pipe, the reaction cooling water circulation pipeline of coupled reaction cooling water inlet and reaction coolant outlet is provided with in reaction jacket pipe, the water steam pipeline connecting steam entry and steam outlet is also provided with in reaction jacket pipe, described and flow cooling device comprise be socketed on and flow pipeline lateral wall and flow jacket pipe, and be provided with above the lateral wall flowing jacket pipe and flow coolant outlet, and be provided with below the lateral wall flowing jacket pipe and flow cooling water inlet, described circulating line is provided with circulating pump, circulating pump is arranged on the circulating line between discharging opening and vomit pipe, circulating line is also provided with and flows valve, and flow on circulating line that valve is arranged on away from vomit pipe side, described circulating line is provided with sample tap, sample tap is connected with probe tube, probe tube is provided with sample valve, described circulating line is provided with shower nozzle near one end of charging aperture, shower nozzle is positioned at and flows pipe, shower nozzle is arranged vertically downward, described and flow pipe sidewall and be provided with observation panel, observation panel is coated with glass, described reaction vessel is provided with agitator in the axial direction, described reaction vessel is provided with the thermometer boss passing perpendicularly through top.
2. use a method for the sulfonation reactor described in claim 1, it is characterized in that: comprise the steps:
1) sulfonation reactor is checked, close baiting valve, baiting valve and sample valve, open and flow valve;
2) add reaction mass by feed pipe, add sulfur trioxide by breather pipe;
3) open agitator, and thermometer is injected thermometer boss;
4) according to the number of degrees of thermometer test, use reaction temperature control device and also flow cooling device regulate reaction temperature;
5) react a period of time, open baiting valve, reactant liquor enters reactor by circulating line backflow;
6) open sample valve, reactant liquor is sampled, close sample valve, sample liquid is detected;
7) when testing result is up to standard, close and flow valve, opening baiting valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310249751.2A CN103432978B (en) | 2013-06-22 | 2013-06-22 | Sulfonation reactor and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310249751.2A CN103432978B (en) | 2013-06-22 | 2013-06-22 | Sulfonation reactor and use method thereof |
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| Publication Number | Publication Date |
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| CN103432978A CN103432978A (en) | 2013-12-11 |
| CN103432978B true CN103432978B (en) | 2015-02-04 |
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| CN201310249751.2A Expired - Fee Related CN103432978B (en) | 2013-06-22 | 2013-06-22 | Sulfonation reactor and use method thereof |
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| CN109293534B (en) * | 2018-09-19 | 2021-10-12 | 中国日用化学研究院有限公司 | Preparation method and device of alkyl diphenyl ether sulfonate |
| CN109876758A (en) * | 2019-04-02 | 2019-06-14 | 天津市科德化工有限公司 | Sulpho Tobias Acid sulfonating reaction kettle |
| CN109939635A (en) * | 2019-04-11 | 2019-06-28 | 淄博询知方技术开发有限公司 | A kind of highly effective reaction kettle facilitating sampling |
| CN109999746A (en) * | 2019-05-10 | 2019-07-12 | 海安艾拉新材料有限公司 | Solid-liquid circular response device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100584443C (en) * | 2006-11-10 | 2010-01-27 | 中国日用化学工业研究院 | SO3 gas jetting sulfonation reactor and process |
| CN202044959U (en) * | 2011-02-14 | 2011-11-23 | 濮阳市联众兴业化工有限公司 | Novel acetyl ketene injection and absorption device |
| CN102188942B (en) * | 2011-04-01 | 2013-04-24 | 沈阳化工大学 | Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor |
| CN202151566U (en) * | 2011-07-15 | 2012-02-29 | 山东星之联生物科技股份有限公司 | Liquid membrane absorption sulphonation reactor |
| CN202893333U (en) * | 2012-11-02 | 2013-04-24 | 湖北神舟化工有限公司 | Gas-liquid reaction device |
| CN202942885U (en) * | 2012-11-21 | 2013-05-22 | 淮安嘉诚高新化工股份有限公司 | Liquid phase catalysis hydrogenation reaction device |
| CN103011110B (en) * | 2012-12-27 | 2014-05-28 | 广西明利化工有限公司 | Injection type arsenic removal reactor |
| CN203329729U (en) * | 2013-06-22 | 2013-12-11 | 安阳市双环助剂有限责任公司 | Sulfonation reactor |
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Granted publication date: 20150204 |