CN102188942A - Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor - Google Patents
Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor Download PDFInfo
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Abstract
管式磺化反应制取间硝基苯磺酸的生产方法，涉及一种化工产品的生产方法，包括硝基苯贮罐（1）、三氧化硫贮罐（2）、管式磺化反应器（3）、釜式磺化反应器（4）、物料输送泵（5）、喷射泵（6）及连接管线和附件（阀门、流量计、温度计、防爆膜、视镜等）。硝基苯与三氧化硫磺化剂按比例进入管式磺化反应器（3），管式磺化反应器（3）与釜式磺化反应器（4）串联使用或管式磺化反应器（3）独立使用。本发明适用于连续或间歇的磺化反应，混合与传热效果好，反应速度快，生产效率高，操作弹性大。本发明提出的生产装置和生产方法适用于各种磺化反应生产过程。
A production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reaction, relating to a production method for chemical products, including a nitrobenzene storage tank (1), a sulfur trioxide storage tank (2), a tubular sulfonation reaction device (3), tank-type sulfonation reactor (4), material transfer pump (5), jet pump (6) and connecting pipelines and accessories (valve, flow meter, thermometer, explosion-proof membrane, sight glass, etc.). Nitrobenzene and sulfur trioxide sulfonating agent enter the tubular sulfonation reactor (3) in proportion, and the tubular sulfonation reactor (3) is used in series with the kettle type sulfonation reactor (4) or the tubular sulfonation reactor (3) Independent use. The invention is suitable for continuous or intermittent sulfonation reaction, has good mixing and heat transfer effects, fast reaction speed, high production efficiency and large operation flexibility. The production device and production method proposed by the invention are suitable for various sulfonation reaction production processes.
Description
Technical field
The present invention relates to a kind of production method of chemical products, what be specifically related to is that nitrobenzene and sulfur trioxide carry out the production method that sulfonating reaction is produced m-nitrobenzene sulfonic acid.
Background technology
The industrial in the past process units that carries out the nitrobenzene sulfonating reaction is the still formula sulfonation reactor that has chuck, production method is for dropping into nitrobenzene in the still formula sulfonation reactor earlier, start the stirring back and in still formula sulfonation reactor, drip sulfur trioxide, feed cooling agent in the still formula sulfonation reactor chuck and take out reaction heat, to keep suitable reaction temperature.The heat transfer area of this still formula sulfonation reactor is little, and heat transfer coefficient is low, can not effectively shift out reaction heat, has limited the rate of addition of sulfur trioxide, and the production cycle is long, and production efficiency is low; Sulfur trioxide adopts the dropping mode to enter in the still in the still formula sulfonating reaction production method, exists even have to stir, and also can't realize dripping the rapid dispersion of thing, so material concentration skewness in the still, hot-spot can't be avoided; In the still formula sulfonating reaction production method, the time of staying inequality of product in still, the in-depth reaction very easily appears in the early stage product that generates.Hot-spot and reactant time of staying inequality in still are the shortcomings that still formula sulfonating reaction can't overcome in the still.
Therefore, provide a kind of novel, sulfonation reaction device and production method are very significant efficiently.
Summary of the invention
The object of the present invention is to provide a kind of tubular type sulfonating reaction to produce the production method of m-nitrobenzene sulfonic acid, adopt tubular type nitrator and kettle type nitrating reactor to unite and carry out sulfonating reaction, reaction is mainly finished in the tubular type nitrator, also can use the tubular type sulfonation reactor to finish sulfonating reaction separately.Make it the purpose that realizes that heat and mass transport is effective, production efficiency is high, the product accessory substance is few.
The objective of the invention is to be achieved through the following technical solutions:
The tubular type sulfonating reaction is produced the production method of m-nitrobenzene sulfonic acid, and this method comprises:
A. adjust flow direction of material: make nitrobenzene return the nitrobenzene basin through tubular type sulfonation reactor, the heating of still formula sulfonation reactor or after being cooled to set point of temperature; Make SO 3 sulfonated dose after tubular type sulfonation reactor, still formula sulfonation reactor heat or be cooled to set point of temperature, to return the sulfur trioxide basin; Make nitrobenzene and SO 3 sulfonated dose enter the tubular type sulfonation reactor in proportion through product pump and jet pump and carry out sulfonating reaction, reactant is formed and is qualifiedly gone subsequent processing or reactant to enter still formula sulfonation reactor to continue to react to reactant and form the qualified subsequent processing that goes;
B. make the circulation of reaction product m-nitrobenzene sulfonic acid enter the tubular type sulfonation reactor once more;
C. adjust nitrobenzene, SO 3 sulfonated dose, circulation m-nitrobenzene sulfonic acid temperature and circulation m-nitrobenzene sulfonic acid flow-control initial reaction state.
Described tubular type sulfonating reaction is produced the production method of m-nitrobenzene sulfonic acid, and the equipment that adopts in its described production method includes nitrobenzene basin, sulfur trioxide basin, tubular type sulfonation reactor, still formula sulfonation reactor, material-handling pump, jet pump and pipeline, annex; The use of independently using or connect of its tubular type sulfonation reactor with still formula sulfonation reactor; The tubular type sulfonation reactor is that separate unit uses or multi-platform combined use.
Described tubular type sulfonating reaction is produced the production method of m-nitrobenzene sulfonic acid, the tubular type sulfonation reactor is blank pipe or chemical filler is set in pipe and convection cell has the hybrid element of perturbation action in the equipment that its described production method adopts, or select commercially available static mixer for use, or blank pipe, chemical filler is set in pipe and convection cell has the hybrid element of perturbation action, the combination of static mixer; The tubular type sulfonation reactor installs chuck outward or chuck is not set.
Described tubular type sulfonating reaction is produced the production method of m-nitrobenzene sulfonic acid, and SO 3 sulfonated dose of its described production method raw material enters the tubular type sulfonation reactor through jet pump or pressured poor, potential difference.
The present invention has following advantage:
1. the present invention both can be used for continuous production, also can be used for Batch Process.
2. tubular type sulfonation reactor heat transfer efficiency can in time shift out reaction heat far above still formula sulfonation reactor.
3. tubular type sulfonation reactor good mixing effect, reaction speed is fast, the production efficiency height.
4. when being used for producing continuously, material time of staying in the tubular type sulfonation reactor is even, can realize the laminar flow reaction, can overcome the uneven shortcoming of residence time of material in the batch still formula sulfonation reactor, obviously reduces accessory substance and generates.
5. when being used for intermittent reaction, owing to set up the tubular type sulfonation reactor, can realize rapidly mixing the material that participates in reaction is established member in jet pump and tubular type sulfonation reactor after, can overcome that traditional still formula sulfonation reactor drips charging and the fatal shortcoming of density unevenness and hot-spot in the still that causes.
6. the nitrobenzene sulfonating reaction of the present invention's proposition is produced m-nitrobenzene sulfonic acid process units production efficiency height, operating flexibility is big, accessory substance is few, good product quality.
Description of drawings
Fig. 1 is that the tubular type nitrobenzene sulfonating reaction that the tubular type sulfonation reactor is connected with still formula sulfonation reactor is produced m-nitrobenzene sulfonic acid production procedure schematic diagram.
Fig. 2 is that the tubular type nitrobenzene sulfonating reaction of no still formula sulfonation reactor is produced m-nitrobenzene sulfonic acid production procedure schematic diagram.
Fig. 3 is that the tubular type nitrobenzene sulfonating reaction of no still formula sulfonation reactor, the circulation of reactionless product m-nitrobenzene sulfonic acid is produced m-nitrobenzene sulfonic acid production procedure schematic diagram.
The specific embodiment
The present invention is described in detail with reference to the accompanying drawings.
The tubular type nitrobenzene sulfonating reaction that the present invention proposes is produced the m-nitrobenzene sulfonic acid production method and is carried out the sulfonating reaction production process applicable to various organic compounds and sulfonating agent.
Tubular type nitrobenzene sulfonating reaction is produced the process units in the m-nitrobenzene sulfonic acid production method, comprises nitrobenzene basin, sulfur trioxide basin, tubular type sulfonation reactor, still formula sulfonation reactor, material-handling pump, jet pump and connecting line and annex (valve, flowmeter, thermometer, rupture pressure disc, visor etc.).The tubular type sulfonation reactor is connected with still formula sulfonation reactor and is used or the tubular type sulfonation reactor independently uses.
But its tubular type sulfonation reactor separate unit uses or multi-platform combined use; The tubular type sulfonation reactor is blank pipe or chemical filler is set in pipe and convection cell has the hybrid element of perturbation action; Or select commercially available static mixer for use; Or blank pipe, chemical filler is set in pipe and convection cell has the hybrid element of perturbation action, the combination of static mixer; The tubular type sulfonation reactor installs chuck outward or chuck is not set.
Tubular type nitrobenzene sulfonating reaction of the present invention is produced the m-nitrobenzene sulfonic acid production method, comprises the adjustment flow direction of material, makes nitrobenzene return the nitrobenzene basin through tubular type sulfonation reactor and the heating of still formula sulfonation reactor or after being cooled to set point of temperature; Adjust flow direction of material, make SO 3 sulfonated dose to return the sulfur trioxide basin through tubular type sulfonation reactor and the heating of still formula sulfonation reactor or after being cooled to set point of temperature; Adjust flow direction of material, make nitrobenzene and SO 3 sulfonated dose enter the tubular type sulfonation reactor in proportion and carry out sulfonating reaction through product pump and jet pump, removes reaction heat by cooling medium in the tubular type sulfonation reactor chuck, reactant is formed and is qualifiedly gone subsequent processing or reactant to enter still formula sulfonation reactor to continue to react to reactant and form the qualified subsequent processing that goes.
Tubular type nitrobenzene sulfonating reaction of the present invention is produced the m-nitrobenzene sulfonic acid production method and is comprised that partial reaction product m-nitrobenzene sulfonic acid is circulated enters the tubular type sulfonation reactor once more.
Tubular type nitrobenzene sulfonating reaction of the present invention is produced the m-nitrobenzene sulfonic acid production method and is comprised nitrobenzene, SO 3 sulfonated dose, circulation m-nitrobenzene sulfonic acid temperature and the circulation m-nitrobenzene sulfonic acid flow-control initial reaction state adjusted.
Tubular type nitrobenzene sulfonating reaction of the present invention is produced the m-nitrobenzene sulfonic acid production method and is comprised that SO 3 sulfonated dose enters the tubular type sulfonation reactor through jet pump or pressured poor, potential difference.
The above tubular type nitrobenzene sulfonating reaction is produced the m-nitrobenzene sulfonic acid production method and is applicable to various sulfonating reaction production processes.
Embodiment one
Tubular type nitrobenzene sulfonating reaction produces that process units in the m-nitrobenzene sulfonic acid production method and process comprise that nitrobenzene basin (1), sulfur trioxide basin (2), tubular type sulfonation reactor (3) are that 5 series connection are arranged vertically, still formula sulfonation reactor (4), material-handling pump (5), jet pump (6) and connecting line and annex.Tubular type sulfonation reactor (3) is connected with still formula sulfonation reactor (4), and the circulation of partial reaction product m-nitrobenzene sulfonic acid enters tubular type sulfonation reactor (3) once more, as Fig. 1.
Embodiment two
Embodiment two and embodiment one are basic identical, and difference is that tubular type sulfonation reactor (3) is arranged vertically for separate unit.
Embodiment three
Embodiment three and embodiment one are basic identical, and difference is that tubular type sulfonation reactor (3) is that 5 series connection are horizontally disposed.
Embodiment four
Embodiment four and embodiment one are basic identical, and difference is that tubular type sulfonation reactor (3) is that 5 parallel connections are arranged vertically.
Embodiment five
Embodiment five and embodiment one are basic identical, and difference is that tubular type sulfonation reactor (3) is that 12 series connection are arranged vertically, and no still formula sulfonation reactor (4) is as Fig. 2.
Embodiment six
Embodiment six and embodiment one are basic identical, and difference is that tubular type sulfonation reactor (3) is that 12 series connection are arranged vertically, no still formula sulfonation reactor (4), and reactionless product m-nitrobenzene sulfonic acid circulation is as Fig. 3.
Claims (4)
1. the tubular type sulfonating reaction is produced the production method of m-nitrobenzene sulfonic acid, it is characterized in that this method comprises:
A. adjust flow direction of material: make nitrobenzene after tubular type sulfonation reactor (3), still formula sulfonation reactor (4) heat or be cooled to set point of temperature, return nitrobenzene basin (1); Make SO 3 sulfonated dose after tubular type sulfonation reactor (3), still formula sulfonation reactor (4) heat or be cooled to set point of temperature, to return sulfur trioxide basin (2); Make nitrobenzene and SO 3 sulfonated dose enter tubular type sulfonation reactor (3) in proportion through product pump (5) and jet pump (6) and carry out sulfonating reaction, reactant is formed and is qualifiedly gone subsequent processing or reactant to enter still formula sulfonation reactor (4) to continue to react to reactant and form the qualified subsequent processing that goes;
B. make the circulation of reaction product m-nitrobenzene sulfonic acid enter tubular type sulfonation reactor (3) once more;
C. adjust nitrobenzene, SO 3 sulfonated dose, circulation m-nitrobenzene sulfonic acid temperature and circulation m-nitrobenzene sulfonic acid flow-control initial reaction state.
2. tubular type sulfonating reaction according to claim 1 is produced the production method of m-nitrobenzene sulfonic acid, it is characterized in that the equipment that adopts in the described production method includes nitrobenzene basin (1), sulfur trioxide basin (2), tubular type sulfonation reactor (3), still formula sulfonation reactor (4), material-handling pump (5), jet pump (6) and pipeline, annex; The use of using or connect that its tubular type sulfonation reactor (3) is independent with still formula sulfonation reactor (4); Tubular type sulfonation reactor (3) uses or multi-platform combined use for separate unit.
3. tubular type sulfonating reaction according to claim 2 is produced the production method of m-nitrobenzene sulfonic acid, it is characterized in that tubular type sulfonation reactor (3) in the equipment that described production method adopts is for blank pipe or chemical filler is set in pipe and convection cell has the hybrid element of perturbation action, or select commercially available static mixer for use, or blank pipe, chemical filler is set in pipe and convection cell has the hybrid element of perturbation action, the combination of static mixer; Tubular type sulfonation reactor (3) is outer to be installed chuck or chuck not to be set.
4. tubular type sulfonating reaction according to claim 1 and 2 is produced the production method of m-nitrobenzene sulfonic acid, it is characterized in that SO 3 sulfonated dose of described production method raw material enters tubular type sulfonation reactor (3) through jet pump (6) or pressured poor, potential difference.
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| CN 201110081746 CN102188942B (en) | 2011-04-01 | 2011-04-01 | Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor |
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| CN 201110081746 CN102188942B (en) | 2011-04-01 | 2011-04-01 | Production method for preparing m-nitrobenzenesulfonic acid by tubular sulfonation reactor |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816092A (en) * | 2012-08-31 | 2012-12-12 | 江苏中丹集团股份有限公司 | Device for continuously preparing m-benzenedisulfonic acid |
| CN103432978A (en) * | 2013-06-22 | 2013-12-11 | 安阳市双环助剂有限责任公司 | Sulfonation reactor and use method thereof |
| CN103752336A (en) * | 2014-01-07 | 2014-04-30 | 南京云高新型材料有限公司 | Vanadium catalyst for nitrobenzene sulfonation and preparation method thereof |
| CN105541667A (en) * | 2016-01-14 | 2016-05-04 | 浙江秦燕科技股份有限公司 | Method for producing CLT acid nitride in continuous pipelization mode |
| CN105541668A (en) * | 2016-01-14 | 2016-05-04 | 浙江秦燕科技股份有限公司 | Method for achieving pipe-type continuous production of CLT acid chloride |
| CN106674062A (en) * | 2016-12-27 | 2017-05-17 | 沈阳化工研究院有限公司 | Method for preparing sodium 3-nitrobenzenesulfonate through catalytic sulfonation |
| CN106749096A (en) * | 2017-02-21 | 2017-05-31 | 山东尚舜化工有限公司 | The preparation method and device of a kind of rubber vulcanization accelerator DZ |
| CN106946745A (en) * | 2017-04-27 | 2017-07-14 | 山东星之联生物科技股份有限公司 | The preparation method of sodium p styrene sulfonate |
| CN111620797A (en) * | 2020-06-12 | 2020-09-04 | 河北建新化工股份有限公司 | Method for synthesizing m-nitrobenzenesulfonic acid by adopting micro-channel continuous flow reactor |
| CN111960971A (en) * | 2020-09-19 | 2020-11-20 | 寿光市荣晟新材料有限公司 | Production process and production equipment of 2-acrylamide-2-methylpropanesulfonic acid |
| CN113372280A (en) * | 2021-05-25 | 2021-09-10 | 黄冈银河阿迪药业有限公司 | 2-methylimidazole continuous nitration reaction system and continuous nitration process |
| CN114797738A (en) * | 2022-04-30 | 2022-07-29 | 河北兰升生物科技有限公司 | Improved tubular reactor, production apparatus using the same, and process for producing sulfonyl compound using the same |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816092B (en) * | 2012-08-31 | 2015-10-14 | 江苏中丹集团股份有限公司 | The device of benzene disulfonic acid between a kind of serialization preparation |
| CN102816092A (en) * | 2012-08-31 | 2012-12-12 | 江苏中丹集团股份有限公司 | Device for continuously preparing m-benzenedisulfonic acid |
| CN103432978A (en) * | 2013-06-22 | 2013-12-11 | 安阳市双环助剂有限责任公司 | Sulfonation reactor and use method thereof |
| CN103752336A (en) * | 2014-01-07 | 2014-04-30 | 南京云高新型材料有限公司 | Vanadium catalyst for nitrobenzene sulfonation and preparation method thereof |
| CN103752336B (en) * | 2014-01-07 | 2015-12-09 | 南京云高新型材料有限公司 | A kind of vanadium catalyst for nitrobenzene sulfonation and preparation method thereof |
| CN105541668B (en) * | 2016-01-14 | 2017-11-24 | 浙江秦燕科技股份有限公司 | A kind of method of duct type continuous production CLT acid chloride |
| CN105541667A (en) * | 2016-01-14 | 2016-05-04 | 浙江秦燕科技股份有限公司 | Method for producing CLT acid nitride in continuous pipelization mode |
| CN105541668A (en) * | 2016-01-14 | 2016-05-04 | 浙江秦燕科技股份有限公司 | Method for achieving pipe-type continuous production of CLT acid chloride |
| CN106674062A (en) * | 2016-12-27 | 2017-05-17 | 沈阳化工研究院有限公司 | Method for preparing sodium 3-nitrobenzenesulfonate through catalytic sulfonation |
| CN106749096A (en) * | 2017-02-21 | 2017-05-31 | 山东尚舜化工有限公司 | The preparation method and device of a kind of rubber vulcanization accelerator DZ |
| CN106946745A (en) * | 2017-04-27 | 2017-07-14 | 山东星之联生物科技股份有限公司 | The preparation method of sodium p styrene sulfonate |
| CN111620797A (en) * | 2020-06-12 | 2020-09-04 | 河北建新化工股份有限公司 | Method for synthesizing m-nitrobenzenesulfonic acid by adopting micro-channel continuous flow reactor |
| CN111620797B (en) * | 2020-06-12 | 2022-08-09 | 河北建新化工股份有限公司 | Method for synthesizing m-nitrobenzenesulfonic acid by adopting micro-channel continuous flow reactor |
| CN111960971A (en) * | 2020-09-19 | 2020-11-20 | 寿光市荣晟新材料有限公司 | Production process and production equipment of 2-acrylamide-2-methylpropanesulfonic acid |
| CN113372280A (en) * | 2021-05-25 | 2021-09-10 | 黄冈银河阿迪药业有限公司 | 2-methylimidazole continuous nitration reaction system and continuous nitration process |
| CN114797738A (en) * | 2022-04-30 | 2022-07-29 | 河北兰升生物科技有限公司 | Improved tubular reactor, production apparatus using the same, and process for producing sulfonyl compound using the same |
| CN114797738B (en) * | 2022-04-30 | 2024-04-02 | 兰升生物科技集团股份有限公司 | Improved tubular reactor, production equipment using the same, and method for producing sulfonyl compound using the same |
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