CN108640860A - The preparation method and N-acetylsulfanilyl chloride of the N-acetylsulfanilyl chloride of green energy conservation - Google Patents
The preparation method and N-acetylsulfanilyl chloride of the N-acetylsulfanilyl chloride of green energy conservation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/01—Sulfonic acids
- C07C309/28—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
- C07C309/45—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
- C07C309/51—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton at least one of the nitrogen atoms being part of any of the groups, X being a hetero atom, Y being any atom
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/78—Halides of sulfonic acids
- C07C309/86—Halides of sulfonic acids having halosulfonyl groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
- C07C309/88—Halides of sulfonic acids having halosulfonyl groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
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Abstract
The preparation method and N-acetylsulfanilyl chloride of the N-acetylsulfanilyl chloride of green energy conservation, belong to chemical field.Method is included under the agitating and heating of 60 70 DEG C of temperature：Antifebrin is mixed to obtain to sulfonation stoste with glacial acetic acid.It is passed through 0.3 0.4Mpa of pressure in dry air to reaction vessel into sulfonation stoste, is passed through 0.6 0.8Mpa of pressure in sulfur trioxide gas to reaction vessel, and the inner air of reaction vessel is passed through sulfonation stoste and reacts 4 8h, glacial acetic acid is recovered under reduced pressure and obtains sulfonated liquid.It is passed through 0.3 0.4Mpa of pressure in dry air to reaction vessel to sulfonated liquid, the inner air of reaction vessel, which is passed through sulfonated liquid, while being passed through thionyl chloride into sulfonated liquid after stopping external aeration reacting 2 3h, and thionyl chloride is recovered under reduced pressure.To raw material availability height and avoid generating waste water and spent acid, energy conservation and environmental protection.N-acetylsulfanilyl chloride obtained is environmental friendly, at low cost, quality is high.
Description
Technical field
The present invention relates to chemical field fields, and more particularly to a kind of system of the N-acetylsulfanilyl chloride of green energy conservation
Preparation Method and N-acetylsulfanilyl chloride.
Background technology
N-acetylsulfanilyl chloride is to prepare sulfamido sterilization to press down the phonetic azoles of mould drug such as sulfanilamide (SN), sulfonamidoxazole, sulfanilamide (SN)
The intermediate of methyl-isoxazole, sulfapyrazole and domian etc., is also used for synthetic dyestuffs, is widely used in curing
The fields such as medicine, coating, plastics and pesticide.
Currently, N-acetylsulfanilyl chloride synthetic method generally use chlorosulfonic acid is sulfonating agent carries out chlorine to antifebrin
Sulfonation, chlorosulfonation is balanced reaction in this method, must just large excess of chlorosulfonic acid be used to participate in reaction to improve yield, caused
Chlorosulfonation dosage is big, generates the problems such as spent acid is more, processing cost is high.
In view of this, special propose the application.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of the N-acetylsulfanilyl chloride of green energy conservation, to raw material
Utilization rate is high and avoids generating waste water and spent acid, energy conservation and environmental protection.
Another object of the present invention is to provide a kind of N-acetylsulfanilyl chloride, environmental friendly, at low cost, quality
It is high.
The present invention solves its technical problem using following technical scheme to realize.
The present invention proposes a kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, including：
Under the conditions of the agitating and heating of 60-70 DEG C of temperature, antifebrin and glacial acetic acid are mixed to get sulfonation stoste, to sulphur
It is passed through pressure in dry air to reaction vessel in change stoste and reaches 0.3-0.4Mpa, sulfur trioxide gas is passed through into sulfonation stoste
Pressure reaches 0.6-0.8Mpa in body to reaction vessel, stops external aeration and the inner air of reaction vessel is passed through sulfonation original
Liquid reacts 4-8h, and glacial acetic acid is recovered under reduced pressure and obtains sulfonated liquid, pressure in dry air to reaction vessel is passed through into sulfonated liquid and is reached
To 0.3-0.4Mpa, stop leading to the inner air of reaction vessel while being passed through thionyl chloride into sulfonated liquid after external aeration
Enter sulfonated liquid reaction 2-3h, remaining thionyl chloride is recovered under reduced pressure.
The present invention proposes a kind of N-acetylsulfanilyl chloride, is made according to above-mentioned preparation method.
The advantageous effect of the embodiment of the present invention is：
The preparation method of the N-acetylsulfanilyl chloride of green energy conservation provided by the invention, using sulfur trioxide as sulfonating agent
Sulfonation is carried out to antifebrin in glacial acetic acid solvent, then chlorination is carried out by chlorinating agent of thionyl chloride, both can guarantee to second
The quality of acylamino- benzene sulfonyl chloride, and avoid generating waste water and spent acid.In sulfonation process：It is passed through sulfur trioxide into sulfonation stoste
Gas carries out sulfonation, since sulfur trioxide gas cannot be completely anti-with antifebrin in time during being passed through sulfonation stoste
It answers, the inner air of reaction vessel is passed through in stoste by sulfur trioxide gas after the completion of being passed through continues sulfonating reaction, is conducive to
The a large amount of sulfur trioxide gas lodged in reaction vessel is recycled in sulfonation stoste and is further carried out with antifebrin soon
Speed, adequately reaction, the cycle of the inner air of reaction vessel can also coordinate stirring action to be sufficiently mixed liquid material, accelerate
The progress of reaction, the utilization rate for improving raw material.In chlorination process：It is added into sulfonated liquid logical while thionyl chloride is reacted
Enter inner air, the cycle cooperation stirring action of inner air is sufficiently mixed liquid material, since thionyl chloride is with extremely strong
The cycle of smoking property inner air the thionyl chloride of smoke can also be passed through sulfonated liquid again and react, accelerate reaction
Carry out, improve the utilization rate of raw material.It is passed through outside dry air into sulfonation stoste and sulfonated liquid and forms a large amount of gas in liquid material
Bubble be conducive to fully be reacted, while to reaction vessel interior carry out supercharging to conducive to reaction later stage material content it is relatively low and
Reaction can be carried out fully when the extent of reaction is higher.
N-acetylsulfanilyl chloride provided by the invention is made according to above-mentioned preparation method, correspondingly has work
The advantages that skill is environmentally friendly, at low cost, quality is high.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Preparation method to the N-acetylsulfanilyl chloride of the green energy conservation of the embodiment of the present invention and to acetyl ammonia below
Base benzene sulfonyl chloride is specifically described.
The present invention provides a kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, is original with antifebrin
Material uses sulfur trioxide to carry out sulfonating reaction for sulfonating agent first, and thionyl chloride is then used to carry out chlorination reaction for chlorinating agent.
In sulfonating reaction, antifebrin is dissolved as solvent using glacial acetic acid, enable antifebrin fully with
Sulfonating agent simultaneously reacts；Antifebrin can be separated and recovered using vacuum distillation after the completion of reaction.In chlorination reaction, dichloro
The chance of Cl- attacks S-O keys is big in sulfoxide, and it is abundant to be conducive to reaction；It can be by unreacted using vacuum distillation after the completion of reaction
Thionyl chloride separation and recovery.
It is reacted using above-mentioned sulfonating agent, chlorinating agent and solvent, both can guarantee the product of N-acetylsulfanilyl chloride
Matter, and avoid generating waste water and spent acid.Can control simultaneously coordinates stirring operation to carry out under 60-70 DEG C of temperature condition, instead
The temperature that should be controlled is unified, and operation is more convenient.
Specifically, in entire reaction process control reaction kettle temperature be 60-70 DEG C, such as temperature be optionally 60 DEG C,
62 DEG C, 65 DEG C, 68 DEG C, 70 DEG C etc..Mechanical agitation is carried out with the rotating speed of 400-600r/min, such as mixing speed is optionally
400r/min, 450r/min, 500r/min, 550r/min, 600r/min etc..
(1) batch mixing operation is carried out first.
Glacial acetic acid is added in reaction kettle, the glacial acetic acid in reaction kettle is added in antifebrin, closes charge door, at this time
To sulfonation stoste.
Optionally, the mass ratio of antifebrin and glacial acetic acid is 1:3-4, such as can be 1:3、1：3.2、1:3.5、1：
3.8、1:4 etc..
It is passed through pressure in dry air to reaction vessel into sulfonation stoste and reaches 0.3-0.4Mpa, such as makes reaction vessel
Interior pressure reaches 0.3Mpa, 0.32Mpa, 0.34Mpa, 0.36Mpa, 0.38Mpa, 0.4Mpa etc..It is passed through the speed of dry air
It is 0.8-1.2 for the volume of the dry air per minute being passed through and the volume ratio of sulfonation stoste:1, such as 0.8:1、0.9:1、1:
1、1.1:1、1.2:1 etc..
The operation of dry air is passed through into sulfonation stoste, gas is to the disturbance cooperative mechanical stirring action of liquid material to sulfonation
Stoste is sufficiently mixed, and so that antifebrin is fully dissolved and is homogeneously dispersed in glacial acetic acid.Sulfonation during ventilation
Stoste gradually completes mixing and heats up, without individually carrying out.A large amount of bubbles are formed in liquid material by operation to be conducive to fully instead
It answers, while supercharging is carried out to reaction vessel interior to be conducive to react when reaction later stage material content is relatively low and the extent of reaction is higher
It can fully carry out.
(2) sulfonating reaction is secondly carried out.
It is passed through pressure in sulfur trioxide gas to reaction vessel into sulfonation stoste and reaches 0.6-0.8Mpa, such as makes reaction
Container inner pressure reaches 0.6Mpa, 0.65Mpa, 0.7Mpa, 0.75Mpa, 0.8Mpa etc..Then stop external aeration and will react
The inner air of container is passed through sulfonation stoste and carries out inner air cycle.
It is passed through sulfur trioxide gas into sulfonation stoste and carries out sulfonation, since sulfur trioxide gas is being passed through sulfonation stoste
Cannot be reacted completely with antifebrin in time in the process, sulfur trioxide gas be passed through after the completion of by the inner air of reaction vessel
It is passed through in stoste and continues sulfonating reaction, sulphur is recycled to conducive to by a large amount of sulfur trioxide gas lodged in reaction vessel
Change further is carried out with antifebrin in stoste it is quick, adequately react.The cycle of the inner air of reaction vessel can also coordinate
Stirring action is sufficiently mixed liquid material, accelerates the progress of reaction, improves the utilization rate of raw material.
Optionally, the speed for being passed through sulfur trioxide gas is the volume per minute for being passed through sulfur trioxide gas and sulfonation stoste
Volume ratio be 0.8-1.2:1, the speed for being passed through inner air is the volume per minute for being passed through inner air and sulfonation stoste
Volume ratio is 0.8-1.2:1.Such as 0.8:1、0.9:1、1:1、1.1:1、1.2:1 etc..
In reaction process, extent of reaction can determine whether by pressure change, such as the detection primary first-order equation kettle per half an hour
Internal pressure illustrates sulfur trioxide by the internal pressure substantially constant of reaction kettle the reaction was complete with antifebrin when detecting.This
Invent in some specific embodiments, pressure is constant refer to reaction kettle internal pressure in measuring twice in succession changing value it is equal
Less than 0.02Mpa.Through inventor the study found that after being passed through inner air reaction 4-8h in sulfonation stoste, the inside of reaction kettle is pressed
Power kept in balance.Therefore after being passed through inner air 4-8h in sulfonation stoste, reaction was completed, such as reaction 4h, 5h, 6h, 7h, 8h
Deng.
After sulfonating reaction, decompression operation is carried out to reaction kettle, glacial acetic acid is evaporated under reduced pressure, glacial acetic acid is carried out
Separation and recycling, obtain sulfonated liquid.
(3) chlorination reaction is finally carried out.
Into sulfonated liquid, pressure reaches 0.3-0.4Mpa in dry air to reaction vessel, such as makes pressure in reaction vessel
Reach 0.3Mpa, 0.32Mpa, 0.34Mpa, 0.36Mpa, 0.38Mpa, 0.4Mpa etc..The speed for being passed through dry air is every point
The volume for the dry air that clock is passed through and the volume ratio of sulfonated liquid are 0.8-1.2:1, such as 0.8:1、0.9:1、1:1、1.1:1、
1.2:1 etc..
The operation that dry air is passed through into sulfonated liquid forms a large amount of bubbles in liquid material, is conducive to further sub- with dichloro
Sulfone fully reacts, at the same to reaction vessel interior carry out supercharging to conducive to reaction later stage material content is relatively low and the extent of reaction compared with
Reaction can be carried out fully when high.
Stopping be passed through dry air from outside after, by thionyl chloride slowly, be continuously added in sulfonated liquid while, will be anti-
It answers the inner air of container to be passed through sulfonated liquid to be reacted.It is passed through the speed of inner air in reaction and is passed through internal sky to be per minute
The volume of gas and the volume ratio of sulfonated liquid are 0.8-1.2:1.Such as 0.8:1、0.9:1、1:1、1.1:1、1.2:1 etc..
The cycle cooperation stirring action of inner air is sufficiently mixed liquid material, may advantageously facilitate coming into full contact with for raw material
And reaction.Since there is thionyl chloride the cycle of extremely strong smoking property inner air can also lead to the thionyl chloride of smoke again
Enter sulfonated liquid to be reacted, accelerates the progress of reaction, improves the utilization rate of raw material.
Optionally, thionyl chloride is passed through sulfonated liquid by bundle pipes.It leads to thionyl chloride in the form of multigroup droplet
Enter in sulfonated liquid, efficient, thionyl chloride and the abundant chlorination of sulfonated liquid during charging of charging.
Since thionyl chloride and reacting for sulfonated liquid are thorough, the molar ratio of antifebrin and thionyl chloride is optionally 1:
1.0-1.1 such as 1:1、1:1.02、1:1.04、1:1.06、1:1.08、1:1.1 etc., that is, saving raw material can fully react again.
Further, the inner air of thionyl chloride and reaction vessel is passed through sulfonated liquid from the bottom of reaction vessel, and two
The circumferential direction that chlorine sulfoxide is passed through the gas outlet of sulfonated liquid along the inner air of reaction vessel is passed through sulfonated liquid.Make the gas for being passed through sulfonated liquid
Body dispels thionyl chloride, further promotes reaction.
In some preferable embodiments of the invention, the operation that thionyl chloride is passed through into sulfonated liquid includes the first charging
Stage, the second feeding stage and third feeding stage.The time of first feeding stage be 20-35min, such as 20min, 25min,
30min, 35min etc..The time of second feeding stage be 60-90min, such as 60min, 65min, 70min, 75min, 80min,
85min, 90min etc..The time of first feeding stage is 40-55min, such as 40min, 45min, 50min, 55min etc..Entirely
The time of charging reaction is 2-3h.
From the first feeding stage to the second feeding stage and third feeding stage, as reaction gradually carries out, material concentration
It is gradually reduced, reactivity continuously decreases, and the charging rate of thionyl chloride is gradually reduced, and is fully carried out convenient for reaction.Specifically
Ground, the mass ratio that the first feeding stage of control, the second feeding stage and third feeding stage are passed through thionyl chloride are 3-4:3-4:
1, such as mass ratio is followed successively by 3:3:1、3:3.5:1、3:4:1、3.5:3:1、3.5:3.5:1、3.5:4:1、4:3:1、4:3.5:
1、4:4:1 etc..
Between first feeding stage and the second feeding stage and between the second feeding stage and third feeding stage into
Row bleeding.It opens air bleeding valve and gas is passed through to the absorption for carrying out tail gas such as hydrogen chloride gas in lye, until reaction vessel
Interior pressure is reduced to 0.15-0.20Mpa, such as 0.15Mpa, 0.16Mpa, 0.17Mpa, 0.18Mpa, 0.19Mpa, 0.2Mpa
Deng closing air bleeding valve.Carry out the charging and reaction of next stage.Hydrogen chloride in the inner air of bleeding reduction reaction kettle
Content is conducive to the progress of reaction.
It keeps the inner air in reaction kettle to be passed through the operation of liquid material in bleeding, hydrogen chloride gas is enable fully to wave
It sends out and is discharged.
Further, bleeding carries out after the first feeding stage and the second feeding stage complete 5-10min, makes
The thionyl chloride that each feeding stage later stage is added can adequately be reacted.
Bleeding includes that exhaust for the first time and second are vented, and exhaust for the first time carries out second after completing 5-10min
Exhaust, the change value of pressure of exhaust and second of exhaust is roughly equal for the first time.In exhaust process not due to hydrogen chloride content
Disconnected to reduce, remaining a small amount of thionyl chloride further participates in reaction, exhaust for the first time and second of exhaust interval 5-10min, with
Remaining a small amount of thionyl chloride is set fully to be reacted.
After sulfonating reaction, decompression operation is carried out to reaction kettle, remaining unreacted thionyl chloride is depressurized
Distillation, thionyl chloride is detached and is recycled, cooling up to N-acetylsulfanilyl chloride.
The present invention provides a kind of N-acetylsulfanilyl chloride, is made according to above-mentioned preparation method, is correspondingly had
The advantages that environmental friendly, at low cost, quality is high.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, including：
Under conditions of 65 DEG C of temperature, mixing speed 500r/min：
S1, by mass ratio be 1:3.5 antifebrin mixes in a kettle with glacial acetic acid, obtains sulfonation stoste.To sulfonation
It is passed through dry air to reacting kettle inner pressure in stoste and reaches 0.35Mpa.
S2, it is passed through sulfur trioxide gas to reacting kettle inner pressure into sulfonation stoste reaches 0.7Mpa, stop external aeration
And the extraction of the inner air of reaction kettle is passed into sulfonation stoste and reacts 4h, glacial acetic acid is recovered under reduced pressure and obtains sulfonated liquid.
S3, it is passed through dry air to reacting kettle inner pressure into sulfonated liquid reaches 0.35Mpa.According to antifebrin and dichloro
The molar ratio of sulfoxide is 1:1 is on the waiting list thionyl chloride.The inner air extraction of reaction kettle is passed into sulfonated liquid：Pass through bundle pipes
3/7 thionyl chloride is passed through in 30min in sulfonated liquid by circumferential along gas outlet, and air bleeding valve is opened by tail gas after reacting 8min
It is passed through in lye and reaches 0.18Mpa to reacting kettle inner pressure and close air bleeding valve；Continue the thionyl chloride by 3/7 in 80min
It is passed through in sulfonated liquid, tail gas is passed through in lye to reacting kettle inner pressure by opening air bleeding valve after reaction 8min reaches 0.18Mpa simultaneously
Close air bleeding valve；The thionyl chloride of residue 1/7 is passed through in 50min in sulfonated liquid, is recovered under reduced pressure after reaction 8min remaining
Thionyl chloride, it is cooling up to N-acetylsulfanilyl chloride.
Wherein, the speed ventilated in S1, S2, S3 step is the volume ratio of the volume and liquid material of the gas per minute being passed through
It is 1:1.
Embodiment 2
A kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, difference from example 1 is that：
In S3 steps, in bleeding, pressure release carries out after closing air bleeding valve the reaction was continued 8min when half, opens air bleeding valve
Carry out the pressure discharge operations of remaining half.
Embodiment 3
A kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, difference from example 1 is that：
In S3 steps, between the first feeding stage and the second feeding stage and the second feeding stage and third feeding stage
Between without bleeding.
Embodiment 4
A kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, difference from example 1 is that：
In S3 steps, the charging rate of thionyl chloride remains unchanged and without bleeding.
Test example
The yield of N-acetylsulfanilyl chloride made from embodiment 1-4 according to mass balance calculate and to purity
It is measured, the results are shown in Table 1.
1 acetamidobenzenesulfonyl chloride yield of table and purity data table
| Project | Yield (%) | Purity (%) |
| Embodiment 1 | 93.8 | 95.7 |
| Embodiment 2 | 94.1 | 96.2 |
| Embodiment 3 | 91.8 | 93.6 |
| Embodiment 4 | 91.3 | 92.9 |
In conclusion the preparation method of the N-acetylsulfanilyl chloride of the green energy conservation of the offer of the embodiment of the present invention,
To raw material availability height and avoid generating waste water and spent acid, energy conservation and environmental protection.The N-acetylsulfanilyl chloride of preparation correspondingly has
The advantages that standby environmental friendly, at low cost, quality is high.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the N-acetylsulfanilyl chloride of green energy conservation, which is characterized in that including：
Under the conditions of the agitating and heating of 60-70 DEG C of temperature, antifebrin and glacial acetic acid are mixed to get sulfonation stoste, to the sulphur
It is passed through pressure in dry air to reaction vessel in change stoste and reaches 0.3-0.4Mpa, three oxidations are passed through into the sulfonation stoste
Pressure reaches 0.6-0.8Mpa in sulphur gas to reaction vessel, stops external aeration and leads to the inner air of the reaction vessel
Enter the sulfonation stoste reaction 4-8h, the glacial acetic acid is recovered under reduced pressure and obtains sulfonated liquid, is passed through into the sulfonated liquid described dry
Pressure reaches 0.3-0.4Mpa in dry air to the reaction vessel, and dichloro is passed through into the sulfonated liquid after stopping external aeration
The inner air of the reaction vessel is passed through the sulfonated liquid while sulfoxide and reacts 2-3h, is recovered under reduced pressure remaining described two
Chlorine sulfoxide.
2. preparation method according to claim 1, which is characterized in that the mass ratio of the antifebrin and the glacial acetic acid
It is 1:3-4；
And/or the molar ratio of the antifebrin and the thionyl chloride is 1:1.0-1.1.
3. preparation method according to claim 1, which is characterized in that per minute to be passed through described three into the sulfonation stoste
The volume ratio of the volume of sulfur oxide gas and the sulfonation stoste is 0.8-1.2:1；
And/or the volume of the inner air per minute that the reaction vessel is passed through into the sulfonation stoste with it is described with it is described
The volume ratio of sulfonation stoste is 0.8-1.2:1；
And/or the volume of the inner air per minute that the reaction vessel is passed through into the sulfonated liquid with described with the sulphur
The volume ratio for changing liquid is 0.8-1.2:1.
4. preparation method according to claim 1, which is characterized in that the thionyl chloride is passed through the sulphur by bundle pipes
Change liquid；
Preferably, the inner air of the thionyl chloride and the reaction vessel is passed through from the bottom of the reaction vessel described
Sulfonated liquid；
It is highly preferred that the thionyl chloride is passed through the circumferential direction of the gas outlet of the sulfonated liquid along the inner air of the reaction vessel
It is passed through the sulfonated liquid.
5. preparation method according to claim 1 or 4, which is characterized in that it is sub- to be passed through the dichloro into the sulfonated liquid
The operation of sulfone includes the first feeding stage, the second feeding stage and third feeding stage, the first feeding stage and the second charging rank
Between section and operation, which is exhausted, between the second feeding stage and third feeding stage makes pressure in the reaction vessel reach
To 0.15-0.20Mpa.
6. preparation method according to claim 5, which is characterized in that bleeding is respectively at the first feeding stage and second
Feeding stage carries out after completing 5-10min.
7. preparation method according to claim 5, which is characterized in that bleeding includes that exhaust for the first time and second are arranged
Gas, for the first time exhaust after completing 5-10min be vented for the second time.
8. preparation method according to claim 5, which is characterized in that the first feeding stage, the second feeding stage and third
The mass ratio that feeding stage is passed through the thionyl chloride is 3-4:3-4:1.
9. preparation method according to claim 8, which is characterized in that the time of the first feeding stage is 20-35min, the
The time of two feeding stages is 60-90min, and the time of third feeding stage is 40-55min.
10. a kind of N-acetylsulfanilyl chloride as made from claim 1-9 any one of them preparation methods.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111718286A (en) * | 2020-07-23 | 2020-09-29 | 邓博天 | Industrial production method of aromatic hydrocarbon sulfonyl chloride with power supply group |
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