CN107963617B - A kind of production method and system of nitrosyl sulfuric acid - Google Patents
A kind of production method and system of nitrosyl sulfuric acid Download PDFInfo
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Abstract
The invention discloses a kind of green continuous production methods of nitrosyl sulfuric acid, comprising 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 generated in nitrosyl sulfuric acid production process, be absorbed sulfuric acid；(3) it absorbs sulfuric acid and water and/or the concentrated sulfuric acid is configured to the sulfuric acid solution of demand concentration, and be mixedly configured into nitration mixture with concentrated nitric acid；(4) nitration mixture, the gas containing sulfur dioxide enter reaction tower by continuous feed and are reacted, and finally obtain nitrosyl sulfuric acid finished product.The invention also discloses a kind of production systems of nitrosyl sulfuric acid, carry out absorption reuse to the tail gas in nitrosyl sulfuric acid production process using concentrating waste acid, nitrosyl sulfuric acid finished product preheats nitration mixture, and using the method for serialization automatic linkage control synthesis nitrosyl sulfuric acid.This method combines automation chain control, heat exchange and tail gas resource utilization, realizes tail gas decrement discharge, energy-saving, improves yield.
Description
Technical field
The present invention relates to dyestuff intermediate production fields, and in particular to a kind of green of dyestuff intermediate nitrosyl sulfuric acid is raw
Produce method and system.
Background technique
Nitrosyl sulfuric acid is a kind of important diazotising raw material.Compared with sodium nitrite, possess higher activity, it can be with
Some low activity amino carry out diazo-reaction.And salt will not be generated in diazo process, facilitates subsequent processing.
Since nitrosyl sulfuric acid easily decomposes, using the concentrated sulfuric acid as solvent in the industry and being stored and transported (has
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 generates 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
Otherwise end of line gas disposal 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 first absorbs tail gas using nitration mixture, but due in nitration mixture volatility nitric acid and amount of nitrogen oxides it is higher,
New tail gas generation is had simultaneously absorbing tail gas, is needed to reuse sodium hydrate aqueous solution and is absorbed, 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, consumes energy higher.
Nitric acid acid mist, sulfur dioxide, sulfur trioxide and water and nitrogen oxides can be generated in nitrosyl sulfuric acid production process
Equal exhaust gas generally use nitration mixture to carry out pre-absorption the processing of these tail gas, but due in nitration mixture nitric acid content it is very high, from
Body volatility is stronger, so incomplete to tail gas absorption, there is still a need for other processing modes for subsequent tail gas, increases energy consumption, discharge.And
The reaction raw materials lost in tail gas will cause the loss of product.So a kind of method for finding green production nitrosyl sulfuric acid has very
Big industrial application value.
Summary 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, improves production efficiency and product quality.
The technical solution adopted by the invention is as follows:
A kind of production method of nitrosyl sulfuric acid, comprising 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 generated 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
At nitration mixture；
(4) nitration mixture, the gas containing sulfur dioxide enter reaction tower by continuous feed and are reacted, and finally obtain nitrosyl
Sulfuric acid finished product；
The spent acid is chlorobenzene, nitro-chlorobenzene, 2- amino -4- acetyl-anisidine, disperse blue 284# intermediate nitrification
The spent acid generated in the spent acid or azo dyes coupled processes that process generates.The main component of spent acid is sulfuric acid or nitrogenous oxygen
Compound.
Preferably, in step (1), the mass fraction of concentrating waste acid is controlled 30~85%, and the concentration of concentrating waste acid is too low,
The demand that will lead to the concentrated sulfuric acid increases, the decline of waste acid reuse rate；The excessive concentration of concentrating waste acid will lead to tail gas absorption effect
Decline.
Unless otherwise specified, mass fraction of the present invention refers both to the mass fraction of effective component, 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 generated in finished product storage is total and/or refers to the exhaust gas summation generated 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 generated 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, can increase initial stage
Reactivity；Nitric acid acid mist, which is again dissolved in sulfuric acid, can be improved must measuring for product nitrosyl sulfuric acid, to improve product yield.
In addition, having excessive SO in nitrosyl sulfuric acid reaction process2Reaction is had neither part nor lot in, so that containing SO in mixed tail gas2With
SO3, they react the concentration that can produce sulfuric acid and then improve sulfuric acid in spent acid with water and oxygen, thus to concentrating waste acid concentration
Demand reduces, and reduces waste acid treatment cost.
Preferably, in step (3), according to sulfuric acid demand, by automation control, continuous configuration obtains demand concentration
Sulfuric acid solution, the mass fraction of gained sulfuric acid solution are 60~90%, if sulfuric acid content is too low, it is steady to will lead to nitrosyl sulfuric acid
Qualitative reduction；Excessive concentration then will increase reaction cost.
Preferably, in step (3), nitration mixture is continuously mixed to get by automation control progress, the quality of nitric acid in nitration mixture
Score is 12~33%, and content is too low to will cause product cost raising；Too high levels will lead to reaction and carry out not exclusively, influencing 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, and the charge-mass ratio of nitration mixture and the gas containing sulfur dioxide is 80~
85.6:14.4~20.
Preferably, in step (4), reaction temperature is 45~70 DEG C.
In step (4), the mass percent of finally obtained nitrosyl sulfuric acid finished product is 27.5~40.5%.
Preferably, in step (4), Red-1 200 45 can be used, in 53 thiocarbamide technique of Red-1 200 produced by cyclization 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-nitrobenzothiazole or 2- ammonia
Base -5,6- dichlorobenzothiazole produces the exhaust gas that workshop section generates, in the workshop section, with the concentrated sulfuric acid, p-nitrophenyl thiocarbamide or 3,4-
Dichlorophenyl thiocarbamide is raw material, and reaction generates dyestuff intermediate 2- amino-6-nitrobenzothiazole or 2- ammonia under the catalysis of bromine
Base -5,6- dichlorobenzothiazole, the exhaust gas which generates is mainly sulfur dioxide, sulfuric acid and mist bromine.
The present invention also provides a kind of production systems of nitrosyl sulfuric acid, including absorption tower, absorption sulfuric acid storage tank, sulfuric acid storage
Slot, 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, enters absorption sulfuric acid storage tank after absorbing mixed tail gas, absorb sulfuric acid in sulfuric acid
It configures and water and/or the concentrated sulfuric acid from sulfuric acid storage tank is added in pot, the sulfuric acid solution configured enters nitration mixture configuration pot, is added
Concentrated nitric acid from nitric acid storage tank, the nitration mixture configured enter reaction tower, and the gas containing sulfur dioxide is passed through in reaction tower
It is 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 configuration pot, mixes
The gas composition mixed tail gas generated 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 two ladders, barium sulfate etc. not with the solid matter of sulfuric acid reaction.
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 set to 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 automate with external refrigerant temperature chain, controls temperature 45
~70 DEG C.
Preferably, heat exchanger is additionally provided between the nitration mixture configuration pot and reaction tower, finally obtained product is sub-
Nitryl sulfuric acid carries out entering back into pan tank after heat exchanges in heat exchanger with into the nitration mixture before reaction tower.
Compared with prior art, the invention has the following advantages that
1, spent acid discharge amount is reduced, realizes that coupling waste acid resourceization utilizes.
2, tail gas is recycled, improves reaction rate.
3, sulfuric acid dosage is reduced, cost of material is reduced.
4, other exhaust gas processing devices are not necessarily to, no additional solid, liquid waste material generates.
5, tail gas recycles completely, realizes the green production of nitrosyl sulfuric acid.
6, it is absorbed by circulation of tail gas, improves product yield.
7, 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.
8, this method whole-course automation chain control realizes nitrosyl sulfuric acid continuous production, guarantees product quality.
Detailed description of the invention
Fig. 1 is the schematic diagram of the production system of nitrosyl sulfuric acid of the present invention.
Specific 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, enters absorption sulfuric acid storage tank after absorbing mixed tail gas, absorb sulfuric acid in sulfuric acid
It configures and water and/or the concentrated sulfuric acid from sulfuric acid storage tank is added in pot, the sulfuric acid solution configured enters nitration mixture configuration pot, is added
Concentrated nitric acid from nitric acid storage tank, the nitration mixture configured enter reaction tower, and the gas containing sulfur dioxide is passed through in reaction tower
It being reacted, the product after reaction carries out entering pan tank after heat exchanges in heat exchanger with the nitration mixture before entrance reaction tower,
Absorb the gas generated 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, comprising the following steps:
(1) concentrating waste acid that spent acid is 30% by being concentrated to get sulfuric acid mass fraction；
(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 generated 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
Measuring score is 31.5%；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is set to 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) it absorbs sulfuric acid and is continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automation 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
Pot outlet sulfuric acid mass fraction control is set 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 that nitration mixture configures pot outlet nitric acid is controlled 12%；
(4) nitration mixture, sulfur dioxide gas enter reaction tower by continuous feed and are reacted, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, reaction tower temperature controls 55~65 DEG C, 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
It is analyzed.It is final that nitrosyl sulfuric acid finished product 8970kg, content 21.50% convert yield 99.6%.Emission-free generation.
Embodiment 2
A kind of production method of nitrosyl sulfuric acid, comprising the following steps:
(1) concentrating waste acid that spent acid is 85% by being concentrated to get sulfuric acid mass fraction；
(2) concentrating waste acid is continuously passed through to absorption tower from top to bottom with 355kg/h flow velocity, absorbs nitrosyl sulfuric acid and produced
The mixed tail gas generated in journey, mixed tail gas enter absorption tower from bottom to top, and be absorbed sulfuric acid, absorb the mass fraction of sulfuric acid
It is 87.5%；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is set to 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) it absorbs sulfuric acid and is continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automation control, with 160kg/h
Speed the concentrated sulfuric acid that mass fraction is 98% is added, continuous configuration obtains the sulfuric acid solution that mass fraction is 90%, and sulfuric acid is matched
Pot outlet sulfuric acid mass fraction control is set 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 nitration mixture configures pot outlet nitric acid mass fraction control 33%；
(4) nitration mixture, sulfur dioxide gas enter reaction tower by continuous feed and are reacted, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, reaction tower temperature controls 55~65 DEG C, 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
It is analyzed.It is final that nitrosyl sulfuric acid finished product 4265kg, content 49.82% convert yield 99.6%.Emission-free generation.
Embodiment 3
A kind of production method of nitrosyl sulfuric acid, comprising the following steps:
(1) spent acid is concentrated to get 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 velocity, absorbs nitrosyl sulfuric acid and produced
The mixed tail gas generated in journey, mixed tail gas enter absorption tower from bottom to top, and be absorbed sulfuric acid, absorb the mass fraction of sulfuric acid
It is 61.6%；
Absorption tower is filler tower reactor, and filler is alumina silicate, and absorption tower emptying is set to 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) it absorbs sulfuric acid and is continuously passed through sulfuric acid configuration pot, according to sulfuric acid demand, by automation control, with
The concentrated sulfuric acid that mass fraction is 98% is added in the speed of 577.5kg/h, and it is molten that continuous configuration obtains the sulfuric acid that mass fraction is 80%
Liquid, sulfuric acid configure pot outlet sulfuric acid mass fraction control 80%, are subsequently passed nitration mixture configuration pot, and with the speed of 257.5kg/h
Degree is added the concentrated nitric acid that mass fraction is 98% and is made into nitration mixture, and nitration mixture configures pot outlet nitric acid content control 18%；
(4) nitration mixture, sulfur dioxide gas enter reaction tower by continuous feed and are reacted, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, reaction tower temperature controls 55~65 DEG C, the charging of reaction tower nitration mixture
Speed control is in 1.4t/h, SO2Speed is passed through as 266.5kg/h, after successive reaction 4h, is disappeared to product quality and corresponding raw material
Consumption is analyzed.It is final that nitrosyl sulfuric acid finished product 6620kg, content 30.66% convert yield 99.8%.Emission-free generation.
Embodiment 4
Compared with Example 3, difference is only that in step (4), is produced using cyclization 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.
It is final that nitrosyl sulfuric acid finished product 6675kg, content 30.44% convert yield 99.9%.Emission-free generation.Thus
As it can be seen that form waste gas of sulfur dioxide caused by cyclization reaction includes the activity for being conducive to reaction and carrying out in 53 thiocarbamide technique of Red-1 200
Component plays catalytic action to reaction, not only without reducing yield and content, replaces a part of raw material sulfur dioxide using exhaust gas
Afterwards, be conducive to the progress of reaction instead.
Embodiment 5
Compared with Example 3, difference is only that in step (4), and using the production of 2- amino-6-nitrobenzothiazole, workshop section is produced
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 acid and 1200kg p-nitrophenyl being added in reactor
Thiocarbamide controls temperature at 70 DEG C hereinafter, 2.4kg bromine is added, and control temperature reacts 2h between 85~100 DEG C, heats up and controls temperature
Degree the reaction was continued at 115~120 DEG C 12h, reaction obtain 1824.5kg dyestuff intermediate 2- amino-6-nitrobenzothiazole sulfuric acid
Solution, the exhaust gas of generation are mainly sulfur dioxide, sulfuric acid mist and mist bromine.
It is final that nitrosyl sulfuric acid finished product 6724kg, content 30.22% convert yield 99.9%.Emission-free generation.Thus
As it can be seen that the exhaust gas that 2- amino-6-nitrobenzothiazole production workshop section generates includes the active component for being conducive to reaction and carrying out, to anti-
Catalytic action should be played, is not only had instead after replacing a part of raw material sulfur dioxide using exhaust gas without reducing yield and content
Conducive to the progress of reaction.
Comparative example 1
(1) being continuously passed through mass fraction according to the speed of 990kg/h and 152.5kg/h in sulfuric acid configuration pot is 98%
The concentrated sulfuric acid and water, the sulfuric acid solution that configuration concentration is 85%, sulfuric acid configure pot outlet sulfuric acid concentration control 85%, are subsequently passed mixed
Acid configuration pot, and the concentrated nitric acid that mass fraction is 98% is added with the speed of 257.5kg/h and is made into nitration mixture, nitration mixture configures pot outlet
Nitric acid mass fraction is controlled 18%；
(2) nitration mixture, sulfur dioxide gas enter reaction tower by continuous feed and are reacted, nitration mixture charging rate and dioxy
Change sulphur gas feed speed and carry out continuous and automatic chain control, reaction tower temperature controls 55~65 DEG C, the charging of reaction tower nitration mixture
Speed control is in 1.4t/h, SO2Speed is passed through for 270kg/h, after successive reaction 4h, to product quality and corresponding consumption of raw materials
It is analyzed.Final nitrosyl sulfuric acid finished product 6585kg, content 30.32% convert yield 98.2%, tail gas by liquid alkaline into
Row absorbs.
Production method and system of the embodiment of the present invention to provided nitrosyl sulfuric acid are described above, for
Those of ordinary skill in the art, thought according to an embodiment of the present invention, have in specific embodiments and applications
Change place, in conclusion the contents of this specification are not to be construed as limiting the invention.
Claims (7)
1. a kind of production method of nitrosyl sulfuric acid, which is characterized in that its production system utilized 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；
Specifically includes 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 generated during nitrosyl sulfuric acid production or waste acid concentration
Enter after gas and absorb sulfuric acid storage tank, be absorbed sulfuric acid；
(3) it absorbs sulfuric acid and water and/or the concentrated sulfuric acid from sulfuric acid storage tank is added in sulfuric acid configuration pot, be configured to demand concentration
Sulfuric acid solution enters nitration mixture configuration pot, and the concentrated nitric acid from nitric acid storage tank is added, is configured to nitration mixture；
(4) nitration mixture, the gas containing sulfur dioxide enter reaction tower by continuous feed and are reacted, and are continuously available nitrosyl sulfuric acid
Finished product enters pan tank；
In the absorption 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
The gas composition mixed tail gas of generation is passed through in absorption tower；
In step (1), the spent acid is chlorobenzene, among nitro-chlorobenzene, 2- amino -4- acetyl-anisidine, disperse blue 284#
The spent acid generated in the spent acid or azo dyes coupled processes that body nitrifying process generates；
In step (4), the gas containing sulfur dioxide is 2- amino-6-nitrobenzothiazole or 2- amino -5,6- dichloro
Benzothiazole produces the exhaust gas that workshop section generates.
2. the production method of nitrosyl sulfuric acid according to claim 1, which is characterized 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, which is characterized in that in step (3), according to sulfuric acid need
The amount of asking, by automation 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, which is characterized 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, which is characterized in that in step (4), reaction tower is to connect
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, which is characterized in that in step (4), use disperse red
145, form waste gas of sulfur dioxide caused by cyclization 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, which is characterized in that the reaction temperature of the reaction tower
Degree automate with external refrigerant temperature chain, 45~70 DEG C of temperature of control.
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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 |
| 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 |
| 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 |
| CN112456450B (en) * | 2020-10-15 | 2022-02-18 | 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 |
| CN114163057B (en) * | 2021-12-23 | 2023-04-18 | 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 |
| CN114314532B (en) * | 2022-01-11 | 2022-08-09 | 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 |
| CN115463519B (en) * | 2022-10-14 | 2023-06-20 | 安徽省海徽化工有限公司 | Method and system for producing nitrososulfuric acid with high efficiency |
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