CN107963617A - The production method and system of a kind of nitrosyl sulfuric acid - Google Patents
The production method and system of a kind of nitrosyl sulfuric acid Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
- C01B21/094—Nitrosyl containing acids
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Abstract
The invention discloses a kind of green continuous production method of nitrosyl sulfuric acid, comprise the following steps：(1) spent acid obtains concentrating waste acid by concentration；(2) concentrating waste acid is continuously passed through absorption tower, absorbs the mixed tail gas produced in nitrosyl sulfuric acid production process, be absorbed sulfuric acid；(3) absorb sulfuric acid and be configured to the sulfuric acid solution of demand concentration with water and/or the concentrated sulfuric acid, and nitration mixture is mixedly configured into concentrated nitric acid；(4) nitration mixture, the gas containing sulfur dioxide are reacted by continuous feed into reaction tower, finally obtain nitrosyl sulfuric acid finished product.The invention also discloses a kind of production system of nitrosyl sulfuric acid, and absorption reuse, nitrosyl sulfuric acid finished product preheating nitration mixture, and the method for synthesizing nitrosyl sulfuric acid using the control of serialization automatic linkage are carried out to the tail gas in nitrosyl sulfuric acid production process using concentrating waste acid.This method combines automation chain control, heat exchange and tail gas recycling, realizes tail gas decrement discharge, energy-saving, improves yield.
Description
Technical field
The present invention relates to dyestuff intermediate production field, and in particular to a kind of green of dyestuff intermediate nitrosyl sulfuric acid is raw
Produce method and system.
Background technology
Nitrosyl sulfuric acid is a kind of important diazotising raw material.Compared with sodium nitrite, it possesses the activity of higher, can be with
Some low activity amino carry out diazo-reaction.And salt will not be produced in diazo process, facilitates subsequent treatment.
Since nitrosyl sulfuric acid easily decomposes, being stored and transported using the concentrated sulfuric acid as solvent in the industry (is had
Production technology also directly uses sulfuric acid to participate in reacting as raw material).Since reaction raw materials have volatile components and gaseous component, make
It produces the exhaust gas such as nitric acid acid mist, nitrogen oxides, sulfur dioxide, sulfur trioxide in process of production, these exhaust gas be required into
End of line gas disposal, otherwise can cause extreme influence to environment.
The Chinese patent literature of Publication No. CN106379875A discloses a kind of production method of nitrosylsulfuric acid and answers
With, which absorbs tail gas first by nitration mixture, but due in nitration mixture volatility nitric acid and amount of nitrogen oxides it is higher,
Absorbed absorbing tail gas and having new tail gas at the same time and produce, it is necessary to reuse sodium hydrate aqueous solution, absorb also needs later
Sour alkali tune and evaporative crystallization are adjusted, though obtaining the resource product of sodium nitrate and sodium chloride, technique is cumbersome, and energy consumption is higher.
Nitric acid acid mist, sulfur dioxide, sulfur trioxide and water and nitrogen oxides can be produced in nitrosyl sulfuric acid production process
Deng exhaust gas, processing for these tail gas generally carries out pre-absorption using nitration mixture, but due in nitration mixture nitric acid content it is very high, from
Body volatility is stronger, so incomplete to tail gas absorption, follow-up tail gas stills need other processing modes, increase energy consumption, discharge.And
The reaction raw materials lost in tail gas can cause the loss of product.So finding a kind of method of green production nitrosyl sulfuric acid has very
Big industrial application value.
The content of the invention
It is an object of the invention to：A kind of Green production method of nitrosyl sulfuric acid is provided, vent gas treatment is greatly reduced and throws
Enter, cut down the consumption of raw materials, improve production efficiency and product quality.
The technical solution adopted by the present invention is as follows：
A kind of production method of nitrosyl sulfuric acid, comprises the following steps：
(1) spent acid obtains concentrating waste acid by concentration；
(2) concentrating waste acid is continuously passed through absorption tower, and what is produced during the production of absorption nitrosyl sulfuric acid or waste acid concentration is mixed
Tail gas is closed, be absorbed sulfuric acid；
(3) concentrated vitriol and water and/or the concentrated sulfuric acid are configured to the sulfuric acid solution of demand concentration, and with concentrated nitric acid mixed configuration
Into nitration mixture；
(4) nitration mixture, the gas containing sulfur dioxide are reacted by continuous feed into reaction tower, finally obtain nitrosyl
Sulfuric acid finished product；
The spent acid is chlorobenzene, nitro-chlorobenzene, 2- amino -4- acetyl-anisidines, disperse blue 284# intermediates nitrification
The spent acid that process produces, or the spent acid produced in azo dyes coupled processes.The main component of spent acid is sulfuric acid or nitrogenous oxygen
Compound.
Preferably, in step (1), for the control of the mass fraction of concentrating waste acid 30~85%, the concentration of concentrating waste acid is too low,
The demand of the concentrated sulfuric acid can be caused to increase, waste acid reuse rate declines；The excessive concentration of concentrating waste acid, can cause tail gas absorption effect
Decline.
Unless otherwise specified, mass fraction of the present invention refers both to the mass fraction of active ingredient, such as concentrating waste acid
Mass fraction refers to the mass fraction of the sulfuric acid in concentrating waste acid.
In step (2), the mixed tail gas refer to nitrosyl sulfuric acid production in complex acid process, reaction process and raw material and
The exhaust gas produced in finished product storage is total and/or refers to the exhaust gas summation produced during waste acid concentration, predominantly sulfur dioxide, nitrogen oxygen
Compound, nitric acid acid mist, sulfuric acid mist etc.；
Due to the effumability and unstability of nitric acid, a small amount of nitrogen oxides and nitric acid can be produced in storage and reaction process
Acid mist, can be by sulfuric acid absorption, and wherein nitrogen oxides is the catalyst and initiator of nitrosyl sulfuric acid reaction, by increasing capacitance it is possible to increase initial stage
Reactivity；Nitric acid acid mist, which is again dissolved in sulfuric acid, can improve must measuring for product nitrosyl sulfuric acid, so as to improve product yield.
In addition, excessive SO is had in nitrosyl sulfuric acid reaction process2Have neither part nor lot in reaction so that contain SO in mixed tail gas2With
SO3, they can produce sulfuric acid with water and oxygen reaction and then improve the concentration of sulfuric acid in spent acid, so as to concentrating waste acid concentration
Demand reduces, and reduces spent acid processing cost.
Preferably, in step (3), according to sulfuric acid demand, by automated control, continuous configuration obtains demand concentration
Sulfuric acid solution, the mass fraction of gained sulfuric acid solution is 60~90%, if sulfuric acid content is too low, nitrosyl sulfuric acid can be caused steady
Qualitative reduction；Excessive concentration, then can increase reaction cost.
Preferably, in step (3), carry out continuously being mixed to get nitration mixture by automated control, the quality of nitric acid in nitration mixture
Fraction is 12~33%, and content is too low to cause product cost to raise；It is incomplete that too high levels can cause reaction to carry out, and influences to produce
Quality.
Preferably, in step (4), reaction tower is continuous reacting device, nitration mixture charging rate and the gas containing sulfur dioxide
Body charging rate carries out continuous and automatic chain control, the charge-mass ratio of nitration mixture and the gas containing sulfur dioxide for 80~
85.6：14.4~20.
Preferably, in step (4), reaction temperature is 45~70 DEG C.
In step (4), the mass percent of the nitrosyl sulfuric acid finished product finally obtained is 27.5~40.5%.
Preferably, in step (4), can use in Red-1 200 45,53 thiocarbamide technique of Red-1 200 produced by ring-closure reaction
Form waste gas of sulfur dioxide replace a part of raw material sulfur dioxide participate in nitrosyl sulfuric acid reaction.
Preferably, in step (4), the gas containing sulfur dioxide is 2- amino-6-nitrobenzothiazoles or 2- ammonia
The exhaust gas that base -5,6- dichlorobenzothiazole production workshop section produces, in the workshop section, with the concentrated sulfuric acid, p-nitrophenyl thiocarbamide or 3,4-
Dichlorophenyl thiocarbamide is raw material, reaction generation dyestuff intermediate 2- amino-6-nitrobenzothiazoles or 2- ammonia under the catalysis of bromine
Base -5,6- dichlorobenzothiazole, the exhaust gas which produces is mainly sulfur dioxide, sulfuric acid and mist bromine.
Present invention also offers a kind of production system of nitrosyl sulfuric acid, including absorption tower, absorption sulfuric acid storage tank, sulfuric acid storage
Groove, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction tower and pan tank；
Enter absorption tower after spent acid is concentrated, enter absorption sulfuric acid storage tank after absorbing mixed tail gas, absorb sulfuric acid in sulfuric acid
Configure and water and/or the concentrated sulfuric acid from sulfuric acid storage tank are added in pot, the sulfuric acid solution configured enters nitration mixture configuration pot, adds
Concentrated nitric acid from nitric acid storage tank, the nitration mixture configured enter reaction tower, the gas containing sulfur dioxide are passed through in reaction tower
Reacted, the product after reaction is passed through pan tank, absorbs sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid and configures pot, mixes
The gas composition mixed tail gas produced in acid configuration pot, reaction tower and pan tank is passed through in absorption tower.
Preferably, the absorption tower is filler tower reactor, and wherein filler is alumina silicate, aluminum phosphate, anthracite, five
Aoxidize the not solid matter with sulfuric acid reaction such as two ladders, barium sulfate.
Preferably, mixed tail gas enters absorption tower from bottom to top, and concentrating waste acid enters absorption tower from top to bottom, and absorption tower is put
Sky is arranged on absorption tower tower top, and accesses emission-control equipment and handled；Absorb sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulphur
Acid configuration pot, nitration mixture configuration pot, reaction tower and pan tank emptying are connected with absorption tower.
Preferably, the reaction temperature of the reaction tower with external refrigerant temperature automate chain, controls temperature 45
~70 DEG C.
Preferably, heat exchanger is additionally provided between the nitration mixture configuration pot and reaction tower, the product finally obtained is sub-
Nitryl sulfuric acid after carrying out heat exchange in heat exchanger into the nitration mixture before reaction tower with entering back into pan tank.
Compared with prior art, the present invention has the following advantages：
1st, spent acid discharge capacity is reduced, realizes that coupling waste acid resourceization utilizes.
2nd, tail gas is recycled, improves reaction rate.
3rd, sulfuric acid dosage is reduced, reduces cost of material.
4th, produced without other exhaust gas processing devices, no extra solid, liquid waste material.
5th, tail gas recycles completely, realizes the green production of nitrosyl sulfuric acid.
6th, absorbed by circulation of tail gas, improve product yield.
7th, the by-product sulfur dioxide of specific intermediate can be used to replace for a part of sulfur dioxide, reduce vent gas treatment cost and
Cost of material.
8th, this method whole-course automation chain control, realizes nitrosyl sulfuric acid continuous production, ensures product quality.
Brief description of the drawings
Fig. 1 is the schematic diagram of the production system of nitrosyl sulfuric acid of the present invention.
Embodiment
The schematic diagram of the production system of nitrosyl sulfuric acid of the present invention is as shown in Figure 1.Production system includes absorption tower, absorbs sulphur
Acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction tower and pan tank；
Enter absorption tower after spent acid is concentrated, enter absorption sulfuric acid storage tank after absorbing mixed tail gas, absorb sulfuric acid in sulfuric acid
Configure and water and/or the concentrated sulfuric acid from sulfuric acid storage tank are added in pot, the sulfuric acid solution configured enters nitration mixture configuration pot, adds
Concentrated nitric acid from nitric acid storage tank, the nitration mixture configured enter reaction tower, the gas containing sulfur dioxide are passed through in reaction tower
Being reacted, the product after reaction enters pan tank after heat exchange is carried out in heat exchanger with the nitration mixture before entrance reaction tower,
Absorb the gas produced in sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction tower and pan tank
Body composition mixed tail gas is passed through in absorption tower.
Embodiment 1
A kind of production method of nitrosyl sulfuric acid, comprises the following steps：
(1) spent acid is by being concentrated to give the concentrating waste acid that sulfuric acid mass fraction is 30%；
(2) concentrating waste acid that flow is 1.0t/h is continuously passed through absorption tower from top to bottom, absorbs nitrosyl sulfuric acid and produced
The mixed tail gas produced in journey, mixed tail gas enter absorption tower from bottom to top, and be absorbed sulfuric acid, and absorption tower exports the matter of sulfuric acid
It is 31.5% to measure fraction；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is arranged on absorption tower tower top, and accesses useless
Flash Gas Compression Skid System is handled；Absorb sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction
Tower and pan tank emptying are connected with absorption tower；
(3) absorb sulfuric acid and be continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automated control, with 752kg/h
Speed be passed through the concentrated sulfuric acid that mass fraction is 98%, continuous configuration obtains the sulfuric acid solution that mass fraction is 60%, and sulfuric acid is matched somebody with somebody
Pot outlet sulfuric acid mass fraction control is put 60%, is subsequently passed nitration mixture configuration pot, and quality point is passed through with the speed of 245kg/h
Number is made into nitration mixture for 98% concentrated nitric acid, and the mass fraction of nitration mixture configuration pot outlet nitric acid is controlled 12%；
(4) nitration mixture, sulfur dioxide gas are reacted by continuous feed into reaction tower, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, 55~65 DEG C of reaction tower temperature control, the charging of reaction tower nitration mixture
Speed control is in 2.0t/h, SO2After flow control 317.5kg/h, successive reaction 4h, to product quality and corresponding consumption of raw materials
Analyzed.Final to obtain nitrosyl sulfuric acid finished product 8970kg, content 21.50%, converts yield 99.6%.Emission-free generation.
Embodiment 2
A kind of production method of nitrosyl sulfuric acid, comprises the following steps：
(1) spent acid is by being concentrated to give the concentrating waste acid that sulfuric acid mass fraction is 85%；
(2) concentrating waste acid is continuously passed through to absorption tower from top to bottom with 355kg/h flow velocitys, absorbs nitrosyl sulfuric acid and produced
The mixed tail gas produced in journey, mixed tail gas enter absorption tower from bottom to top, and be absorbed sulfuric acid, absorbs the mass fraction of sulfuric acid
For 87.5%；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is arranged on absorption tower tower top, and accesses useless
Flash Gas Compression Skid System is handled；Absorb sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction
Tower and pan tank emptying are connected with absorption tower；
(3) absorb sulfuric acid and be continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automated control, with 160kg/h
Speed add the concentrated sulfuric acid that mass fraction is 98%, continuous configuration obtains the sulfuric acid solution that mass fraction is 90%, and sulfuric acid is matched somebody with somebody
Pot outlet sulfuric acid mass fraction control is put 90%, is subsequently passed nitration mixture configuration pot, and quality point is added with the speed of 270kg/h
Number is made into nitration mixture for 98% concentrated nitric acid, and the outlet nitric acid mass fraction control of nitration mixture configuration pot is 33%；
(4) nitration mixture, sulfur dioxide gas are reacted by continuous feed into reaction tower, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, 55~65 DEG C of reaction tower temperature control, the charging of reaction tower nitration mixture
Speed control is in 0.8t/h, SO2Speed 282.5kg/h is passed through, after successive reaction 4h, to product quality and corresponding consumption of raw materials
Analyzed.Final to obtain nitrosyl sulfuric acid finished product 4265kg, content 49.82%, converts yield 99.6%.Emission-free generation.
Embodiment 3
A kind of production method of nitrosyl sulfuric acid, comprises the following steps：
(1) spent acid is concentrated to give the concentrating waste acid that mass fraction is 60% by pretreatment；
(2) concentrating waste acid is continuously passed through to absorption tower from top to bottom with 555kg/h flow velocitys, absorbs nitrosyl sulfuric acid and produced
The mixed tail gas produced in journey, mixed tail gas enter absorption tower from bottom to top, and be absorbed sulfuric acid, absorbs the mass fraction of sulfuric acid
For 61.6%；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is arranged on absorption tower tower top, and accesses useless
Flash Gas Compression Skid System is handled；Absorb sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction
Tower and pan tank emptying are connected with absorption tower；
(3) absorb sulfuric acid and be continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automated control, with
The speed of 577.5kg/h adds the concentrated sulfuric acid that mass fraction is 98%, and it is molten that continuous configuration obtains the sulfuric acid that mass fraction is 80%
Liquid, the outlet sulfuric acid mass fraction control of sulfuric acid configuration pot are subsequently passed nitration mixture configuration pot 80%, and with the speed of 257.5kg/h
Degree adds the concentrated nitric acid that mass fraction is 98% and is made into nitration mixture, and the outlet nitric acid content control of nitration mixture configuration pot is 18%；
(4) nitration mixture, sulfur dioxide gas are reacted by continuous feed into reaction tower, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, 55~65 DEG C of reaction tower temperature control, the charging of reaction tower nitration mixture
Speed control is in 1.4t/h, SO2It is 266.5kg/h to be passed through speed, after successive reaction 4h, is disappeared to product quality and corresponding raw material
Consumption is analyzed.Final to obtain nitrosyl sulfuric acid finished product 6620kg, content 30.66%, converts yield 99.8%.Emission-free generation.
Embodiment 4
Compared with Example 3, differ only in step (4), produced using ring-closure reaction in 53 thiocarbamide technique of Red-1 200
Raw form waste gas of sulfur dioxide alternative materials sulfur dioxide participates in reaction, and the flow-rate ratio of form waste gas of sulfur dioxide and raw material sulfur dioxide is
1:1.Other steps and reaction condition are same as Example 3.
Final to obtain nitrosyl sulfuric acid finished product 6675kg, content 30.44%, converts yield 99.9%.Emission-free generation.Thus
As it can be seen that form waste gas of sulfur dioxide caused by ring-closure reaction includes the activity for being conducive to reaction progress in 53 thiocarbamide technique of Red-1 200
Component, catalytic action is played to reaction, and not only without yield and content is reduced, a part of raw material sulfur dioxide is replaced using exhaust gas
Afterwards, the progress of reaction is conducive on the contrary.
Embodiment 5
Compared with Example 3, differ only in step (4), using the production of 2- amino-6-nitrobenzothiazoles, workshop section produces
The complete alternative materials sulfur dioxide of raw exhaust gas participates in reaction.Other steps and reaction condition are same as Example 3.
The production process of the production workshop section is as follows：The 1000kg concentrated sulfuric acids and 1200kg p-nitrophenyls are added in reactor
Thiocarbamide, control temperature add 2.4kg bromines less than 70 DEG C, control temperature to react 2h between 85~100 DEG C, heat up and control temperature
Degree obtains 1824.5kg dyestuff intermediate 2- amino-6-nitrobenzothiazole sulfuric acid in 115~120 DEG C of the reaction was continued 12h, reaction
Solution, the exhaust gas of generation is mainly sulfur dioxide, sulfuric acid mist and mist bromine.
Final to obtain nitrosyl sulfuric acid finished product 6724kg, content 30.22%, converts yield 99.9%.Emission-free generation.Thus
As it can be seen that the exhaust gas that 2- amino-6-nitrobenzothiazoles production workshop section produces includes and is conducive to the active component that reaction carries out, to anti-
Catalytic action should be played, not only without yield and content is reduced, after replacing a part of raw material sulfur dioxide using exhaust gas, is had on the contrary
Beneficial to the progress of reaction.
Comparative example 1
(1) it is 98% to be continuously passed through mass fraction according to the speed of 990kg/h and 152.5kg/h in sulfuric acid configures pot
The concentrated sulfuric acid and water, configuration concentration are 85% sulfuric acid solution, and sulfuric acid configuration pot outlet sulfuric acid concentration control 85%, is subsequently passed mixed
Acid configuration pot, and mass fraction is added using the speed of 257.5kg/h and is made into nitration mixture, the outlet of nitration mixture configuration pot as 98% concentrated nitric acid
Nitric acid mass fraction is controlled 18%；
(2) nitration mixture, sulfur dioxide gas are reacted by continuous feed into reaction tower, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, 55~65 DEG C of reaction tower temperature control, the charging of reaction tower nitration mixture
Speed control is in 1.4t/h, SO2It is 270kg/h to be passed through speed, after successive reaction 4h, to product quality and corresponding consumption of raw materials
Analyzed.Final nitrosyl sulfuric acid finished product 6585kg, content 30.32% convert yield 98.2%, tail gas by liquid caustic soda into
Row absorbs.
The embodiment of the present invention is described the production method of nitrosyl sulfuric acid and system that are provided above, for
Those of ordinary skill in the art, according to the thought of the embodiment of the present invention, have in specific embodiments and applications
Change part, in conclusion this specification content should not be construed as limiting the invention.
Claims (9)
1. a kind of production method of nitrosyl sulfuric acid, it is characterised in that comprise the following steps：
(1) spent acid obtains concentrating waste acid by concentration；
(2) concentrating waste acid is continuously passed through absorption tower, absorbs the mixing tail produced during nitrosyl sulfuric acid production or waste acid concentration
Gas, be absorbed sulfuric acid；
(3) concentrated vitriol and water and/or the concentrated sulfuric acid are configured to the sulfuric acid solution of demand concentration, and are mixedly configured into concentrated nitric acid mixed
Acid；
(4) nitration mixture, the gas containing sulfur dioxide are reacted by continuous feed into reaction tower, are continuously available nitrosyl sulfuric acid
Finished product；
The spent acid is chlorobenzene, nitro-chlorobenzene, 2- amino -4- acetyl-anisidines, disperse blue 284# intermediate nitrifying processes
The spent acid produced in the spent acid of generation, or azo dyes coupled processes.
2. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (1), concentrating waste acid
Mass fraction is controlled 30~85%.
3. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (3), according to sulfuric acid need
The amount of asking, by automated control, continuous configuration obtains the sulfuric acid solution of demand concentration, and the mass fraction of gained sulfuric acid solution is 60
~90%.
4. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (3), pass through automation
Control carries out continuously being mixed to get nitration mixture, and the mass fraction of nitric acid is 12~33% in nitration mixture.
5. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (4), reaction tower is company
Continuousization reaction unit, nitration mixture charging rate carry out continuous and automatic chain control with the gas feed speed containing sulfur dioxide, mix
The charge-mass ratio of acid and the gas containing sulfur dioxide is 80~85.6：14.4~20.
6. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (4), use disperse red
145th, form waste gas of sulfur dioxide caused by ring-closure reaction is participated in instead of a part of raw material sulfur dioxide in 53 thiocarbamide technique of Red-1 200
The reaction of nitrosyl sulfuric acid.
7. the production method of nitrosyl sulfuric acid according to claim 1, it is characterised in that in step (4), described contains two
The gas of sulfur oxide produces the useless of workshop section's generation for 2- amino-6-nitrobenzothiazoles or 2- amino -5,6- dichlorobenzothiazoles
Gas.
8. a kind of production system of nitrosyl sulfuric acid, it is characterised in that the production system includes absorption tower, absorbs sulfuric acid storage
Groove, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture configuration pot, reaction tower and pan tank；
Enter absorption tower after spent acid is concentrated, enter absorption sulfuric acid storage tank after absorbing mixed tail gas, absorb sulfuric acid and configured in sulfuric acid
Water and/or the concentrated sulfuric acid from sulfuric acid storage tank are added in pot, the sulfuric acid solution configured enters nitration mixture configuration pot, and addition comes from
The concentrated nitric acid of nitric acid storage tank, the nitration mixture configured enter reaction tower, and the gas containing sulfur dioxide is passed through in reaction tower and is carried out
Reaction, the product after reaction are passed through pan tank, absorb sulfuric acid storage tank, sulfuric acid storage tank, nitric acid storage tank, sulfuric acid configuration pot, nitration mixture and match somebody with somebody
The gas composition mixed tail gas produced in pot, reaction tower and pan tank is put to be passed through in absorption tower.
9. the production system of nitrosyl sulfuric acid according to claim 8, it is characterised in that the reaction temperature of the reaction tower
Degree with external refrigerant temperature automate chain, 45~70 DEG C of temperature of control.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109485025A (en) * | 2018-12-10 | 2019-03-19 | 杭州申航新材料有限公司 | The continuous production device and method of 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 |
| CN111672276A (en) * | 2020-06-01 | 2020-09-18 | 深圳市长隆科技有限公司 | Resource utilization process of waste gas in production process of polymeric ferric sulfate |
| CN112456450A (en) * | 2020-10-15 | 2021-03-09 | 浙江迪邦化工有限公司 | System and method for resource utilization of waste sulfuric acid containing organic matters |
| CN112500295A (en) * | 2020-10-30 | 2021-03-16 | 德兴市德邦化工有限公司 | Production process of 3, 5-dichloronitrobenzene |
| CN114163057A (en) * | 2021-12-23 | 2022-03-11 | 南京信息工程大学 | Method for catalytically degrading organic matters in waste water containing nitrosyl sulfuric acid dye by using tungsten oxide |
| CN114314532A (en) * | 2022-01-11 | 2022-04-12 | 江苏飞宇医药科技股份有限公司 | Process for preparing nitroso-sulfuric acid by recycling sulfur dioxide in tail gas generated in production of cyclopropylamine |
| CN115463519A (en) * | 2022-10-14 | 2022-12-13 | 安徽省海徽化工有限公司 | Method and system for efficiently producing nitroso-sulfuric acid |
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