CN103435018A - Method and device for tower-type continuous production of nitrosyl sulfuric acid - Google Patents
Method and device for tower-type continuous production of nitrosyl sulfuric acid Download PDFInfo
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- CN103435018A CN103435018A CN2013103663666A CN201310366366A CN103435018A CN 103435018 A CN103435018 A CN 103435018A CN 2013103663666 A CN2013103663666 A CN 2013103663666A CN 201310366366 A CN201310366366 A CN 201310366366A CN 103435018 A CN103435018 A CN 103435018A
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- finished product
- tower
- sulfuric acid
- medial launder
- reaction tower
- Prior art date
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Links
- RXQNKKRGJJRMKD-UHFFFAOYSA-N 5-bromo-2-methylaniline Chemical compound CC1=CC=C(Br)C=C1N RXQNKKRGJJRMKD-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000010924 continuous production Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 58
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 52
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000006396 nitration reaction Methods 0.000 claims description 57
- 230000008676 import Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 7
- 239000002826 coolant Substances 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 6
- 239000000498 cooling water Substances 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 29
- 238000006193 diazotization reaction Methods 0.000 description 5
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 compare Chemical compound 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method and a device for tower-type continuous production of nitrosyl sulfuric acid. The production is performed between a reaction tower (1) and a finished product middle tank (3). Sulfuric acid and nitric acid are mixed to be a mixed acid with the mass ratio of more than 1.7 in the finished product middle tank (3); the prepared mixed acid is delivered to a mixed acid inlet in the top of the reaction tower (1) through a circulation pump (4) and a pipe side of a heat exchanger (5), and flows into the finished product middle tank (3) from the reaction tower (1); after the circulation of acid mixture is formed, sulfur dioxide gas is introduced into the finished product middle tank (3), the cooling water on the shell side of the heat exchanger (5) is started, and the tower bottom temperature of the reaction tower is controlled below 70 DEG C; when the sulfur dioxide gas is introduced, a certain amount of the mixed acid is distributed to an injection pump (6) through a branch pipe; when color of the mixed acid in a pipe viewing mirror (2) turns to blue, the finished product of nitrosyl sulfuric acid is obtained in the finished product middle tank (3). The method disclosed in the invention achieves continuous industrial production, the method and device are safe and environment-friendly, and the yield of sulfur dioxide is high.
Description
Technical field
The present invention relates to production method and the device of nitrosyl sulfuric acid, the particularly method of tower continuous production nitrosyl sulfuric acid and device.
Background technology
Diazotization is the important reaction member of organic synthesis, and Sodium Nitrite is diazotization reaction raw material commonly used.While having other group to exist on phenyl ring, amino activity decreased, at this moment need active higher diazotization raw material nitrosyl sulfuric acid.With Sodium Nitrite, compare, nitrosyl sulfuric acid can not generate sodium sulfate salt as diazotization agent when the diazotization reaction, is convenient to the concentration and recovery of the dilute sulphuric acid of subsequent handling.In addition, nitrosyl sulfuric acid is very unsettled compound still, usually need to be dissolved in certain density sulfuric acid and could store safely and transport.
Summary of the invention
The object of the invention is to: a kind of method and device of tower continuous production nitrosyl sulfuric acid are provided, continuous industrial production, method and equipment safety, environmental protection, the sulfurous gas yield is high.
Technical solution of the present invention is: the production of this nitrosyl sulfuric acid is carried out between reaction tower and finished product medial launder, comprise the following steps: in the finished product medial launder, certain density sulfuric acid and nitric acid are made into to nitration mixture, the nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower by the heat exchanger tube pass on the circulating-pump outlet pipeline by recycle pump, nitration mixture flows to the finished product medial launder from reaction tower; After nitration mixture forms circulation, pass into sulfur dioxide gas in the finished product medial launder, simultaneously the water coolant of the heat exchanger shell pass on ON cycle pump discharge pipeline; Control reaction and carry out at a certain temperature, sulfur dioxide gas in the finished product medial launder with the nitration mixture initial reaction after, enter in reaction tower and continue to react with nitration mixture by finished product medial launder and gas tube between reaction tower; Be reaction end when liquid nitration mixture color becomes blueness, now in the finished product medial launder, be qualified nitrosyl sulfuric acid product.
Wherein, control temperature of reaction below 70 ℃.
Wherein, in nitration mixture, the mass ratio of sulfuric acid and nitric acid is more than or equal to 1.7, and in nitration mixture, water content is less than or equal to 12%.
Wherein, pass into the speed of sulfurous gas to control the reaction tower column bottom temperature not higher than 70 ℃.
Wherein, production equipment of the present invention comprises reaction tower, the finished product medial launder, recycle pump, interchanger, the bottom of reaction tower and finished product medial launder top connecting tube, the lower side of reaction tower connects the top of finished product medial launder through gas pipeline, connecting tube between finished product medial launder bottom sides and pump inlet, the tube side inlet connecting branch road of circulation pump outlet and interchanger, the tube side outlet of interchanger and the upper side connecting tube of reaction tower, the top of finished product medial launder is provided with the sulfur dioxide gas import, the sulfur dioxide gas import is to finished product medial launder liquid level.
Wherein, reaction tower is packing tower or tray column.
Wherein, the bottom of reaction tower and finished product medial launder top connecting tube, be equipped with pipeline viewing mirror on pipeline, in order to observe the color of liquid, when liquid nitration mixture color becomes blueness, is reaction end, now in the finished product medial launder, is qualified nitrosyl sulfuric acid product.
Wherein, pipeline between heat exchanger tube pass outlet and reaction tower upper side is provided with branch pipeline, branch pipeline is connected with the liquid-inlet of squirt pump, spraying pump outlet is connected by pipeline with the top of finished product medial launder, the top connecting tube of the gas feed of squirt pump and reaction tower, the sulfur dioxide gas that reaction tower tower top unreacted is complete and the nitrogen oxide gas evaporated suck the reaction of finished product medial launder sustainable participation by squirt pump.
The present invention has the following advantages: 1, equipment safety, can control temperature of reaction as long as control the intake velocity of sulfurous gas; 2, emission-free discharge, belong to environment-protective process; 3, the sulfurous gas yield is high; 4, produce continuously, labour intensity is little.
The accompanying drawing explanation
Fig. 1 is production equipment block diagram of the present invention.
In figure: 1 reaction tower, 2 pipeline viewing mirrors, 3 finished product medial launders, 4 recycle pumps, 5 interchanger, 6 squirt pumps.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these examples just in order to demonstrate the invention, but not limit the scope of the invention by any way.Easy in order to narrate, omitted the annexes such as the mouth of pipe conventional on valve conventional on the pipeline, storage tank, manhole, instrumentation tap, bearing in explanation of the present invention, the those skilled in the art of the industry can be designed as required.The those of ordinary skill of the industry can be made many modification and improvement, for example changes the charging metering method, and the mouth of pipe of device is adjusted, and increases the quantity of reaction tower, and all these modification, adjustment, improvement all should be considered as protection scope of the present invention.
As shown in Figure 1, production equipment of the present invention comprises reaction tower 1, pipeline viewing mirror 2, finished product medial launder 3, recycle pump 4, interchanger 5, squirt pump 6, and the bottom of reaction tower 1 and finished product medial launder 3 top connecting tubes, be equipped with pipeline viewing mirror 2 on pipeline; The lower side of reaction tower 1 is connected with the top of finished product medial launder 3 through gas pipeline; Connecting tube between finished product medial launder 3 bottom sides and recycle pump 4 imports, the tube side inlet connecting branch road of the outlet of recycle pump 4 and interchanger 5; The tube side outlet of interchanger 5 and the upper side connecting tube of reaction tower 1; Pipeline between interchanger 5 tube side outlets and reaction tower 1 upper side is provided with branch pipeline, and branch pipeline is connected with the liquid-inlet of squirt pump 6; The outlet of squirt pump 6 is connected by pipeline with the top of finished product medial launder 3; The top connecting tube of the gas feed of squirt pump 6 and reaction tower 1; The top of finished product medial launder 3 is provided with the sulfur dioxide gas import, and the sulfur dioxide gas import is to finished product medial launder 3 liquid levels.
Wherein, production method comprises the following steps: in finished product medial launder 1, certain density sulfuric acid and nitric acid are made into to nitration mixture, in nitration mixture, sulfuric acid and nitric acid mass ratio are greater than 1.7, and in nitration mixture, water content is less than 12%; The nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower 1 by the tube side of the interchanger 5 on recycle pump 4 outlet lines by recycle pump 4, nitration mixture flows to finished product medial launder 3 from reaction tower 1; After nitration mixture forms circulation, pass into sulfur dioxide gas in finished product medial launder 3, the water coolant of interchanger 5 shell sides on ON cycle pump 4 outlet lines, control the reaction tower column bottom temperature below 70 ℃ simultaneously; When passing into sulfur dioxide gas, by branch pipeline, a certain amount of nitration mixture is assigned to squirt pump 6; When the nitration mixture color in pipeline viewing mirror 2 becomes blueness, stop passing into sulfur dioxide gas, obtain the finished product nitrosyl sulfuric acid.
embodiment 1: according to following steps, produce nitrosyl sulfuric acid
In finished product medial launder 1, sulfuric acid and nitric acid are made into to nitration mixture, in nitration mixture, sulfuric acid and nitric acid mass ratio are 1.7, and in nitration mixture, water content is 12%; The nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower 1 by the tube side of the interchanger 5 on recycle pump 4 outlet lines by recycle pump 4, nitration mixture flows to finished product medial launder 3 from reaction tower 1; After nitration mixture forms circulation, pass into sulfur dioxide gas in finished product medial launder 3, the water coolant of interchanger 5 shell sides on ON cycle pump 4 outlet lines, control reaction tower 1 column bottom temperature at 70 ℃ simultaneously; By branch pipeline, a certain amount of nitration mixture is assigned to squirt pump 6 when passing into sulfur dioxide gas; When the nitration mixture color in pipeline viewing mirror 3 becomes blueness, stop passing into sulfur dioxide gas, obtain the finished product nitrosyl sulfuric acid.
embodiment 2: according to following steps, produce nitrosyl sulfuric acid
In finished product medial launder 1, sulfuric acid and nitric acid are made into to nitration mixture, in nitration mixture, sulfuric acid and nitric acid mass ratio are 2.0, and in nitration mixture, water content is 9.6%; The nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower 1 by the tube side of the interchanger 5 on recycle pump 4 outlet lines by recycle pump 4, nitration mixture flows to finished product medial launder 3 from reaction tower 1; After nitration mixture forms circulation, pass into sulfur dioxide gas in finished product medial launder 3, the water coolant of interchanger 5 shell sides on ON cycle pump 4 outlet lines, control reaction tower 1 column bottom temperature at 50 ℃ simultaneously; By branch pipeline, a certain amount of nitration mixture is assigned to squirt pump 6 when passing into sulfur dioxide gas; When the nitration mixture color in pipeline viewing mirror 3 becomes blueness, stop passing into sulfur dioxide gas, obtain the finished product nitrosyl sulfuric acid.
embodiment 3: according to following steps, produce nitrosyl sulfuric acid
In finished product medial launder 1, sulfuric acid and nitric acid are made into to nitration mixture, in nitration mixture, sulfuric acid and nitric acid mass ratio are 2.5, and in nitration mixture, water content is 6.6%; The nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower 1 by the tube side of the interchanger 5 on recycle pump 4 outlet lines by recycle pump 4, nitration mixture flows to finished product medial launder 3 from reaction tower 1; After nitration mixture forms circulation, pass into sulfur dioxide gas in finished product medial launder 3, the water coolant of interchanger 5 shell sides on ON cycle pump 4 outlet lines, control reaction tower 1 column bottom temperature at 35 ℃ simultaneously; By branch pipeline, a certain amount of nitration mixture is assigned to squirt pump 6 when passing into sulfur dioxide gas; When the nitration mixture color in pipeline viewing mirror 3 becomes blueness, stop passing into sulfur dioxide gas, obtain the finished product nitrosyl sulfuric acid.
Claims (7)
1. the method for tower continuous production nitrosyl sulfuric acid, it is characterized in that: the production of this nitrosyl sulfuric acid is carried out between reaction tower and finished product medial launder, comprise the following steps: in the finished product medial launder, certain density sulfuric acid and nitric acid are made into to nitration mixture, the nitration mixture prepared is transported to the tower top nitration mixture import of reaction tower by the heat exchanger tube pass on the circulating-pump outlet pipeline by recycle pump, nitration mixture flows to the finished product medial launder from reaction tower; After nitration mixture forms circulation, pass into sulfur dioxide gas in the finished product medial launder, simultaneously the water coolant of the heat exchanger shell pass on ON cycle pump discharge pipeline; Control reaction and carry out at a certain temperature, sulfur dioxide gas in the finished product medial launder with the nitration mixture initial reaction after, enter in reaction tower and continue to react with nitration mixture by finished product medial launder and gas tube between reaction tower; Be reaction end when liquid nitration mixture color becomes blueness, now in the finished product medial launder, be qualified nitrosyl sulfuric acid product.
2. the method for tower continuous production nitrosyl sulfuric acid according to claim 1, is characterized in that: control temperature of reaction below 70 ℃.
3. the method for tower continuous production nitrosyl sulfuric acid according to claim 1, it is characterized in that: in nitration mixture, the mass ratio of sulfuric acid and nitric acid is more than or equal to 1.7, and in nitration mixture, water content is less than or equal to 12%.
4. the method for tower continuous production nitrosyl sulfuric acid according to claim 1, is characterized in that: pass into the speed of sulfurous gas to control the reaction tower column bottom temperature not higher than 70 ℃.
5. the device of tower continuous production nitrosyl sulfuric acid, it is characterized in that: this production equipment comprises reaction tower (1), finished product medial launder (3), recycle pump (4), interchanger (5), the bottom of reaction tower (1) and finished product medial launder (3) top connecting tube, the lower side of reaction tower (1) is connected with the top of finished product medial launder (3) through gas pipeline; Connecting tube between finished product medial launder (3) bottom sides and recycle pump (4) import, the tube side inlet connecting branch road of the outlet of recycle pump (4) and interchanger (5), the tube side outlet of interchanger (5) and the upper side connecting tube of reaction tower (1), the top of finished product medial launder (3) is provided with the sulfur dioxide gas import, and the sulfur dioxide gas import is to finished product medial launder (3) liquid level.
6. the device of tower continuous production nitrosyl sulfuric acid according to claim 5, it is characterized in that: reaction tower (1) is packing tower or tray column.
7. the device of tower continuous production nitrosyl sulfuric acid according to claim 5 is characterized in that: the bottom of reaction tower (1) and finished product medial launder (3) top connecting tube, be equipped with pipeline viewing mirror (2) on pipeline.
The device of tower continuous production nitrosyl sulfuric acid according to claim 5, it is characterized in that: the pipeline between the outlet of interchanger (5) tube side and reaction tower (1) upper side is provided with branch pipeline, branch pipeline is connected with the liquid-inlet of squirt pump (6), the outlet of squirt pump (6) is connected by pipeline with the top of finished product medial launder (3), the top connecting tube of the gas feed of squirt pump (6) and reaction tower (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310366366.6A CN103435018B (en) | 2013-08-21 | 2013-08-21 | Method and device for tower-type continuous production of nitrosyl sulfuric acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310366366.6A CN103435018B (en) | 2013-08-21 | 2013-08-21 | Method and device for tower-type continuous production of nitrosyl sulfuric acid |
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| CN103435018A true CN103435018A (en) | 2013-12-11 |
| CN103435018B CN103435018B (en) | 2015-07-01 |
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| CN201310366366.6A Active CN103435018B (en) | 2013-08-21 | 2013-08-21 | Method and device for tower-type continuous production of nitrosyl sulfuric acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417509A (en) * | 2015-11-30 | 2016-03-23 | 浙江林江化工股份有限公司 | Preparation method of nitrosyl sulfuric acid and method for separating sulfuric acid and phosphoric acid in industrial waste acid |
| CN105948002A (en) * | 2016-04-29 | 2016-09-21 | 解卫宇 | Production process for recovering waste acid for preparing nitrosyl sulfuric acid |
| CN107311127A (en) * | 2017-06-22 | 2017-11-03 | 江苏依柯化工有限公司 | A kind of production method of salt-free nitrosyl sulfuric acid |
| CN111268657A (en) * | 2020-01-22 | 2020-06-12 | 浙江迪邦化工有限公司 | Method and system for continuously producing nitrosyl sulfuric acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3149913A (en) * | 1961-06-14 | 1964-09-22 | California Research Corp | Process for producing nitrosylsulfuric acid |
| US3307904A (en) * | 1961-12-26 | 1967-03-07 | Toyo Rayon Co Ltd | Preparation of nitrosylsulfuric acid of high purity |
| US4128623A (en) * | 1977-02-15 | 1978-12-05 | Basf Aktiengesellschaft | Manufacture of a solution of nitrosylsulfuric acid in sulfuric acid |
-
2013
- 2013-08-21 CN CN201310366366.6A patent/CN103435018B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3149913A (en) * | 1961-06-14 | 1964-09-22 | California Research Corp | Process for producing nitrosylsulfuric acid |
| US3307904A (en) * | 1961-12-26 | 1967-03-07 | Toyo Rayon Co Ltd | Preparation of nitrosylsulfuric acid of high purity |
| US4128623A (en) * | 1977-02-15 | 1978-12-05 | Basf Aktiengesellschaft | Manufacture of a solution of nitrosylsulfuric acid in sulfuric acid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417509A (en) * | 2015-11-30 | 2016-03-23 | 浙江林江化工股份有限公司 | Preparation method of nitrosyl sulfuric acid and method for separating sulfuric acid and phosphoric acid in industrial waste acid |
| CN105417509B (en) * | 2015-11-30 | 2017-09-08 | 浙江林江化工股份有限公司 | The separation method of sulfuric acid and phosphoric acid in a kind of preparation of nitrosylsulfuric acid and industrial waste acid |
| CN105948002A (en) * | 2016-04-29 | 2016-09-21 | 解卫宇 | Production process for recovering waste acid for preparing nitrosyl sulfuric acid |
| CN107311127A (en) * | 2017-06-22 | 2017-11-03 | 江苏依柯化工有限公司 | A kind of production method of salt-free nitrosyl sulfuric acid |
| CN111268657A (en) * | 2020-01-22 | 2020-06-12 | 浙江迪邦化工有限公司 | Method and system for continuously producing nitrosyl sulfuric acid |
| CN111268657B (en) * | 2020-01-22 | 2021-07-23 | 浙江迪邦化工有限公司 | Method and system for continuously producing nitrosyl sulfuric acid |
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| CN103435018B (en) | 2015-07-01 |
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Address after: 223002 Huaian City, Jiangsu province Qingpu District West Road No. 40 Patentee after: Jiangsu Kesheng Intelligent Equipment Co.,Ltd. Address before: 223002 Huaian City, Jiangsu province Qingpu District West Road No. 40 Patentee before: JIANGSU KESHENG CHEMICAL MACHINERY Co.,Ltd. |