CN107311127A - A kind of production method of salt-free nitrosyl sulfuric acid - Google Patents
A kind of production method of salt-free nitrosyl sulfuric acid Download PDFInfo
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- CN107311127A CN107311127A CN201710479188.6A CN201710479188A CN107311127A CN 107311127 A CN107311127 A CN 107311127A CN 201710479188 A CN201710479188 A CN 201710479188A CN 107311127 A CN107311127 A CN 107311127A
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- China
- Prior art keywords
- sulfuric acid
- salt
- production method
- nitrosyl sulfuric
- free
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
Abstract
The invention discloses a kind of production method of salt-free nitrosyl sulfuric acid, sulfuric acid and the nitration mixture of nitric acid formation are used for raw material, sulfur dioxide gas is passed through in the presence of initiator and carries out redox reaction, solution turned blue purple and pressure jump are the nitrosyl sulfuric acid solution that can obtain required mass fraction in reaction system.Reaction temperature control of the present invention is readily produced control in 25 DEG C~40 DEG C, and convenient operation reduces energy consumption；Reacted under the pressure no more than 0.25MPa, reaction speed can be improved, control the loss of sulfur dioxide gas, reduce environmental pollution.Reach the purpose for facilitating production operation, reducing production cost, making full use of resource.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of production method of salt-free nitrosyl sulfuric acid.
Background technology
Salt-free nitrosyl sulfuric acid solution has high concentration, good fluidity, low cost a little, is widely used in diazotising
Reaction is central, particularly the diazo-reaction of alkalescent arylamine and most of heterocyclic amino compounds, more shows the excellent of it
More performance.And the nitrosyl sulfuric acid solution for using sodium nitrite method to generate, because the niter cake of reaction generation is in sulfuric acid
Solubility is smaller, often forms crystallization, makes material retrogradation, is unfavorable for reaction.
In spite of the method that nitrosyl sulfuric acid solution is produced using various spent acid, but it is mingled with various impurity, it is impossible to wide
General application.When being particularly mingled with chloride ion impurities, nitrosyl chloride, rather than target substance are easily formed, the quality of product is influenceed
And the reliability of reaction.
Nitrogen oxides is changed under conditions of up to 800 DEG C or so with oxygen in air and nitrogen, with the concentrated sulfuric acid and hair
Cigarette sulfuric acid is in 50 DEG C~70 DEG C reaction production nitrosyl sulfuric acid solution, and reaction condition is harsher, and nitrosyl sulfuric acid is at 78 DEG C
Left and right is easily decomposed, and production process safety coefficient is low, security incident easily occurs, and cause environmental pollution.
Nitrosyl sulfuric acid is unstable material, exists only in sulfuric acid in finite concentration form, could preferably join
With reaction, storage and transport.
The content of the invention
Goal of the invention：In order to solve the deficiencies in the prior art, the invention provides a kind of production of salt-free nitrosyl sulfuric acid
Method, under the conditions of low temperature, low pressure reaction, carries out oxidation-reduction reaction and obtains nitrosyl sulfuric acid solution, realize convenient operation,
Raising reaction speed, reduction environmental pollution, drop can save consumption and make full use of resource and the purpose of safety in production.
Technical scheme：A kind of production method of salt-free nitrosyl sulfuric acid, uses sulfuric acid and the nitration mixture of nitric acid formation for raw material,
Initiator is added, sulfur dioxide gas is passed through and carries out oxidation-reduction reaction, when solution turned blue purple in reaction system and pressure are prominent
During change, reaction terminates, the nitrosyl sulfuric acid solution of mass fraction needed for obtaining.
Wherein, nitric acid stream is added to temperature control in sulfuric acid and is no more than 35 DEG C.
Wherein, the mass fraction of sulfuric acid is 90%~104.5%, and the mass fraction of nitric acid is 85%~98%, sulfuric acid with
The mass ratio of nitric acid is 1~4:1.
Wherein, initiator is water or salt-free nitrosyl sulfuric acid solution, and the consumption of water is 5%~10%, salt-free nitrosyl sulphur
The consumption of acid is 1%~5%.
Wherein, temperature control when being passed through sulfur dioxide gas is at 25 DEG C~40 DEG C.
Wherein, Stress control when being passed through sulfur dioxide gas is in 0.1MPa~0.25MPa.
Wherein, sulfur dioxide gas flow control is in 15~40m3/h。
Wherein, reaction reaches terminal when being changed into blue-violet solution by solution in observing response system, and is ventilating
Reaction reaches terminal during the state that stroke pressure is undergone mutation.
Wherein, the obtained nitrosyl sulfuric acid liquid quality fraction that reaction is obtained is 35%-65%.
Reaction equation is：
Beneficial effect：Reaction temperature control of the present invention is readily produced control in 25 DEG C~40 DEG C, and convenient operation reduces energy
Consumption；Reacted under the pressure no more than 0.25MPa, reaction speed can be improved, controlled the loss of sulfur dioxide gas, subtract
Few environmental pollution.Reach the purpose for facilitating production operation, reducing production cost, making full use of resource.
Embodiment
The present invention is described in further detail with reference to specific embodiment.It should be understood that these examples are intended merely to lift
The example explanation present invention, rather than the scope of the present invention is limited in any way, any technical staff for being familiar with this technology is not taking off
From the change and retouching made in the spirit and scope of the present invention, protection scope of the present invention all should be belonged to.
Embodiment 1
1630kg92% sulfuric acid is added in the reactor, adds 520kg90% nitric acid in 35 DEG C to flow down, and is added
50kg42.15% nitrosyl sulfuric acid solution, temperature stabilization starts to be passed through sulfur dioxide gas, flow control is 20 at 26 DEG C
~25m3/ h, venting process temperature stabilization is at 26 DEG C~30 DEG C, and after ventilating 4 hours, reaction solution is bluish violet, pressure jump point
For 0.12MPa, sulfur dioxide 480kg is consumed, the nitrosyl sulfuric acid solution that 2675kg contents are 35.79%, 100% nitrous is obtained
Acyl sulfate yield is 99.25%.
Embodiment 2
Add 1000kg98% sulfuric acid in the reactor, in 35 DEG C to flow down plus 520kg95% nitric acid, add 50kg water,
50kg42.15% nitrosyl sulfuric acid solution, temperature stabilization starts to be passed through sulfur dioxide gas, flow control is 30 at 30 DEG C
~35m3/ h, venting process temperature stabilization is at 30 DEG C~35 DEG C, and after ventilating 3.5 hours, reaction solution is bluish violet, pressure jump
Point is 0.2MPa, consumes sulfur dioxide 506kg, obtains the nitrosyl sulfuric acid solution that 2120kg contents are 47.52%, and 100% is sub-
Nitryl sulfuric acid yield is 99.05%.
Embodiment 3
600kg92% sulfuric acid is added in the reactor, adds 520kg95% nitric acid in 35 DEG C to flow down, and is added
50kg42.15% nitrosyl sulfuric acid solution, temperature stabilization starts to be passed through sulfur dioxide gas, flow control is 20 at 30 DEG C
~25m3/ h, venting process temperature stabilization is at 35 DEG C~40 DEG C, and after ventilating 4 hours, reaction solution is bluish violet, pressure jump point
For 0.13MPa, sulfur dioxide 505kg is consumed, the nitrosyl sulfuric acid solution that 1670kg contents are 60.75%, 100% nitrous is obtained
Acyl sulfate yield is 99.76%.
Embodiment 4
440kg92% sulfuric acid is added in the reactor, adds 520kg90% nitric acid in 35 DEG C to flow down, and is added
50kg42.15% nitrosyl sulfuric acid solution, temperature stabilization starts to be passed through sulfur dioxide gas, flow control is 25 at 30 DEG C
~30m3/ h, venting process temperature stabilization is at 30 DEG C~35 DEG C, and after ventilating 4.5 hours, reaction solution is bluish violet, pressure jump
Point is 0.12MPa, consumes sulfur dioxide 479.5kg, obtains the nitrosyl sulfuric acid solution that 1485kg contents are 64.46%, 100%
Nitrosyl sulfuric acid yield is 99.23%.
Claims (9)
1. a kind of production method of salt-free nitrosyl sulfuric acid, it is characterized in that：Sulfuric acid and the nitration mixture of nitric acid formation are used for raw material, plus
Enter initiator, be passed through sulfur dioxide gas and carry out oxidation-reduction reaction, when solution turned blue purple and pressure jump in reaction system
When, reaction terminates, the nitrosyl sulfuric acid solution of mass fraction needed for obtaining.
2. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：Nitric acid stream is added to the middle temperature of sulfuric acid
Degree control is no more than 35 DEG C.
3. the production method of the salt-free nitrosyl sulfuric acid according to claim 1,2, it is characterized in that：The mass fraction of sulfuric acid is
90%~104.5%, the mass fraction of nitric acid is 85%~98%, and the mass ratio of sulfuric acid and nitric acid is 1~4:1.
4. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：Initiator is water or salt-free Asia
Nitryl sulfuric acid solution, the consumption of water is 5%~10%, and the consumption of salt-free nitrosyl sulfuric acid is 1%~5%.
5. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：When being passed through sulfur dioxide gas
Temperature control at 25 DEG C~40 DEG C.
6. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：When being passed through sulfur dioxide gas
Stress control in 0.1MPa~0.25MPa.
7. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：Sulfur dioxide gas rate of flow of fluid control
System is in 15~40m3/h。
8. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：By in observing response system
Reaction reaches terminal when solution is changed into blue-violet solution, and reaction reaches end in the state that venting process pressure is undergone mutation
Point.
9. the production method of salt-free nitrosyl sulfuric acid according to claim 1, it is characterized in that：React obtained nitrosyl sulphur
Acid solution mass fraction is 35%~65%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710479188.6A CN107311127A (en) | 2017-06-22 | 2017-06-22 | A kind of production method of salt-free nitrosyl sulfuric acid |
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|---|---|---|---|
| CN201710479188.6A CN107311127A (en) | 2017-06-22 | 2017-06-22 | A kind of production method of salt-free nitrosyl sulfuric acid |
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| CN107311127A true CN107311127A (en) | 2017-11-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115092896A (en) * | 2022-06-09 | 2022-09-23 | 蓬莱嘉信染料化工股份有限公司 | Method for preparing nitrosyl sulfuric acid by using microchannel reactor and application of nitrosyl sulfuric acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2343782A1 (en) * | 1998-09-01 | 2000-03-09 | Metallgesellschaft Ag | Method for removing nitrogen oxides from nitrosyl sulphuric acid |
| CN103435018A (en) * | 2013-08-21 | 2013-12-11 | 江苏科圣化工机械有限公司 | Method and device for tower-type continuous production of nitrosyl sulfuric acid |
-
2017
- 2017-06-22 CN CN201710479188.6A patent/CN107311127A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2343782A1 (en) * | 1998-09-01 | 2000-03-09 | Metallgesellschaft Ag | Method for removing nitrogen oxides from nitrosyl sulphuric acid |
| CN103435018A (en) * | 2013-08-21 | 2013-12-11 | 江苏科圣化工机械有限公司 | Method and device for tower-type continuous production of nitrosyl sulfuric acid |
Non-Patent Citations (1)
| Title |
|---|
| 谭凤姣: "无盐亚硝酰硫酸合成工艺研究", 《湘潭师范学院学报(自然科学版)》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115092896A (en) * | 2022-06-09 | 2022-09-23 | 蓬莱嘉信染料化工股份有限公司 | Method for preparing nitrosyl sulfuric acid by using microchannel reactor and application of nitrosyl sulfuric acid |
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Application publication date: 20171103 |
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