CN109400506A - A kind of synthetic method of high-purity chlorosulphonyl isocyanate - Google Patents
A kind of synthetic method of high-purity chlorosulphonyl isocyanate Download PDFInfo
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- CN109400506A CN109400506A CN201811353003.8A CN201811353003A CN109400506A CN 109400506 A CN109400506 A CN 109400506A CN 201811353003 A CN201811353003 A CN 201811353003A CN 109400506 A CN109400506 A CN 109400506A
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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
- C07C303/36—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of amides of sulfonic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
- C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
- C07D291/06—Six-membered rings
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Abstract
The present invention provides a kind of synthetic methods of high-purity chlorosulphonyl isocyanate, comprising: A) under diluent existence condition, sulfur trioxide and chlorine cyanogen are subjected to sulfonating reaction, obtain reaction solution；B the reaction solution) is subjected to pyrolysis, the reaction solution after being thermally decomposed；C the reaction solution after the thermal decomposition) is subjected to positive pressure continuous still, obtains high-purity chlorosulphonyl isocyanate and distillation front-end volatiles；The diluent is selected from chlorosulphonyl isocyanate or the distillation front-end volatiles.Synthetic method provided by the invention improves process overall yields；This method, as reaction dissolvent, is avoided high boiling solvent and used using distillation front-end volatiles, and pyrolytic process, recovery section chlorine cyanogen and sulfur trioxide, is improved the utilization rate of raw material, is reduced production cost.The technique distillation process is distilled using positive pressure and is carried out by the way of continuous feed simultaneously, is substantially increased the yield of product, is shortened distillation time, reduces energy consumption and cost of labor, and industrialization large-scale production is suitble to.
Description
Technical field
The invention belongs to chemosynthesis technical fields, and in particular to a kind of synthetic method of high-purity chlorosulphonyl isocyanate.
Background technique
Chlorosulphonyl isocyanate is a very active intermediate.The substance is reacted with hydroxyl, amino, carboxyl generates N
~chlorine sulfonamido formic acid esters, urea, amide.It can add with water, reactive hydrogen, alcohol, phenol, amine, amide, carboxylic acid, alkene, aldehyde, ketone, ester
At, obtain various new compounds, can make dehydrating agent, oxidant use.Chlorosulphonyl isocyanate is mainly for the production of cephalo furan
The drugs such as pungent, Cefoxitin, carumonan.
Chlorosulphonyl isocyanate manufacturing process and uncomplicated in industrial production, generally mostly uses chlorine cyanogen and sulfur trioxide anti-
It answers, then obtains product chlorosulphonyl isocyanate to resulting crude product chlorosulphonyl isocyanate progress purification & isolation is reacted.?
Though there is production method more mature, technical level is not high.Such as patent JP77855 and EP294613, severe reaction conditions, discomfort
Close industrialized production；CN101891657 has used atent solvent, and directly distills, and does not carry out to the impurity that side reaction generates
Processing, be easy to cause product purity lower, is unable to longtime running.Therefore it provides a kind of synthesis that can be improved yield and purity
Method, and can be used for industrialized production is the current technical issues that need to address.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of synthesis side of high-purity chlorosulphonyl isocyanate
Method, the synthetic method product yield and purity is high of chlorosulphonyl isocyanate provided by the invention, and reaction condition is mild, is easy to real
Now industrialize.
The present invention provides a kind of synthetic methods of high-purity chlorosulphonyl isocyanate, comprising the following steps:
A) under diluent existence condition, sulfur trioxide and chlorine cyanogen is subjected to sulfonating reaction, obtain reaction solution；
B the reaction solution) is subjected to pyrolysis, the reaction solution after being thermally decomposed；
C the reaction solution after the thermal decomposition) is subjected to positive pressure continuous still, obtains high-purity chlorosulphonyl isocyanate and distillation
Front-end volatiles；
The diluent is selected from chlorosulphonyl isocyanate or step C) obtained distillation front-end volatiles.
Sulfur trioxide and chlorine cyanogen are carried out sulfonating reaction first by the present invention, specifically, diluent is added into reaction unit,
Then sulfur trioxide and chlorine cyanogen are added in reaction unit, carry out sulfonating reaction and obtains reaction solution after reaction.
Wherein, the diluent is selected from chlorosulphonyl isocyanate or step C) obtained distillation front-end volatiles.In this hair
In bright, chlorosulphonyl isocyanate can be used as diluent when first prepares chlorosulphonyl isocyanate, then later
Batch use the distillation front-end volatiles obtained after positive pressure continuous still.
Wherein, the usage amount of the diluent is the 1%~5% of inventory total amount.
Wherein, the temperature of the sulfonating reaction is 28~43 DEG C, preferably 30~40 DEG C, more preferably 32~38 DEG C.
The molar ratio of the sulfur trioxide and chlorine cyanogen is 1:(0.8~1.2), preferably 1:(0.9~11).
In the present invention, the chlorine cyanogen is prepared according to following reaction equation:
Cl2+NaCN→ClCN
Specifically, liquid chlorine and sodium cyanide solution are carried out chlorination reaction in chlorination reactor simultaneously, then through cooling dry
It is dry that pure liquid cyanogen chloride is made.
Then by reaction solution heat temperature raising carry out pyrolysis, wherein the temperature of the pyrolysis be 100~
120 DEG C, preferably 105~115 DEG C.Wherein, the pyrolysis carries out preferably in thermal decomposer, and the present invention is to described
The specific source of thermal decomposer is there is no specifically limited, and well known to a person skilled in the art thermal decomposers.Thermal decomposition
In the process, the sulfur trioxide and chlorine cyanogen in reaction process are collected.Reaction solution after thermal decomposition, after being thermally decomposed.
Then, by after the thermal decomposition reaction solution carry out positive pressure continuous still, obtain high-purity chlorosulphonyl isocyanate and
Distill front-end volatiles.
Wherein, the positive pressure continuous still carries out in continuous still system, and referring to Fig. 1, Fig. 1 is company provided by the invention
The schematic diagram of continuous Distallation systm.The continuous still system includes:
De- light upper tower, Tuo Qingzhong tower and the de- gently lower tower being sequentially connected from top to bottom, described take off are opened in the middle part of gently upper tower
Equipped with feed liquid port；
The weight-removing column that liquid inlet is connected with the liquid outlet of the de- light lower tower, the weight-removing column top is provided with distillation
Front-end volatiles outlet, the weight-removing column middle part are provided with product outlet, and the weight-removing column lower part is provided with recombination sub-export.
In certain specific embodiments of the invention, the de- gently upper tower, Tuo Qingzhong tower, de- gently lower tower and weight-removing column
For packed tower.For the present invention to the type of the filler there is no specifically limited, well known to a person skilled in the art can be used for chlorine sulphur
The filler of acyl isocyanates distillation.
Wherein, the filler in the de- light upper tower is subsection setup, and the filler in the de- light upper tower is divided into upper section filler
With lower section filler, the feed liquid port is opened in de- gently upper tower tower wall and the position between upper section filler and lower section filler
It sets.
The filler of the de- light middle tower and de- light lower tower is without subsection setup.
The liquid outlet of the de- light upper tower is connected with the liquid inlet for taking off tower in light, the liquid of the de- light above tower
Outlet is set to the bottom end of the de- light upper tower, and the liquid inlet for taking off tower in light is set to the top of the de- light middle tower,
And it is located at the position of the filler in de- light middle tower or more.
The liquid outlet of the de- light middle tower is connected with the liquid inlet for taking off light lower tower, the liquid of the de- gently middle tower
Outlet is set to the bottom end of the de- light middle tower, and the liquid inlet of the de- light lower tower is set to the top of the de- gently lower tower,
And it is located at the position of the filler of de- light lower tower tower wall or more.
Filler in the weight-removing column is subsection setup, in the weight-removing column filler be divided into upper section filler, middle section filler with
And lower section filler；
The liquid outlet of the de- light lower tower is connected with the liquid inlet of the weight-removing column, and the liquid of the de- light lower tower enters
Mouth is set to the de- gently lower tower bottom end, during the liquid inlet of the weight-removing column is opened in the weight-removing column tower wall and is located at
Position between section filler and lower section filler.
The weight-removing column top is provided with the outlet of distillation front-end volatiles, described in certain specific embodiments of the invention
Front-end volatiles outlet is opened in the weight-removing column tower wall and is located at the position of the upper section filler or more；
It is provided with product outlet in the middle part of the weight-removing column, in certain specific embodiments of the invention, the finished product goes out
Mouth is opened in the weight-removing column tower wall, and the position between middle section filler and lower section filler；
The weight-removing column lower part is provided with recombination sub-export, in certain specific embodiments of the invention, the recombination
Sub-export is opened in weight-removing column bottom.
Pressure in the continuous still system is 1.5MPa.
When carrying out positive pressure continuous still, the reaction solution after thermal decomposition is passed through continuous still by feed liquid port duration
In system, and in continuous still system, the boiling point of the reaction solution after the thermal decomposition reaches 130 DEG C or more, then thermally decomposes
Reaction solution afterwards is taking off light upper tower and de- light middle tower decomposition completely, obtains approaching the production of qualification after the de- light lower tower stage separates
Product, then, the product enter weight-removing column rectifying after the side outlet extraction of de- light lower tower again, obtain qualified product.To
Reduce the process of current 3~4 times rectifying repeatedly, and then improves the yield and yield of product.Product is by one-time continuous essence
The chlorosulphonyl isocyanate to conform to quality requirements is made after evaporating, obtained distillation front-end volatiles give over to next reaction diluent.
When carrying out positive pressure continuous still, the tower top temperature of the de- light upper tower, Tuo Qingzhong tower, de- light lower tower and weight-removing column
It is 93~100 DEG C.The pressure of the positive pressure continuous still is 1.5~2.0MPa.
Batch distillation in the prior art must slightly be evaporated twice, qualified products can be obtained in a rectifying, distill total recovery
For 65%-70%, kettle residual is big, and energy consumption is big, and product purity is 99% or more.
And continuous still provided by the invention can once obtain qualified products, distillation total recovery is 90%, and kettle residual is small, section
The about energy, product purity are 99.5% or more.
Referring to fig. 2, Fig. 2 is the flow diagram of the synthetic method of high-purity chlorosulphonyl isocyanate provided by the invention.That is,
Sulfur trioxide and chlorine cyanogen carry out sulfonating reaction first, after pyrolysis and distillation, obtain chlorosulphonyl isocyanate, and
Distillation front-end volatiles therein can be used for the solvent of sulfonating reaction, and the sulfur trioxide collected in pyrolytic process can be used for making with chlorine cyanogen
For the raw material of sulfonating reaction.
Reaction equation is as follows:
Compared with prior art, the present invention provides a kind of synthetic method of high-purity chlorosulphonyl isocyanate, including it is following
Step: A) under diluent existence condition, sulfur trioxide and chlorine cyanogen are subjected to sulfonating reaction, obtain reaction solution；It B) will be described anti-
Liquid is answered to carry out pyrolysis, the reaction solution after being thermally decomposed；C) that the reaction solution progress positive pressure after the thermal decomposition is continuous
Distillation obtains high-purity chlorosulphonyl isocyanate and distillation front-end volatiles；The diluent is selected from chlorosulphonyl isocyanate or step C)
The obtained distillation front-end volatiles.Synthetic method provided by the invention improves process overall yields；This method evaporates before using distillation
It is allocated as reaction dissolvent, avoids high boiling solvent use, and pyrolytic process, recovery section chlorine cyanogen and sulfur trioxide, it improves
The utilization rate of raw material, reduces production cost.Simultaneously the technique distillation process using positive pressure distillation and continuous feed by the way of into
Row, substantially increases the yield of product, shortens distillation time, reduce energy consumption and cost of labor, is suitble to industrialization extensive
Production.This method is easy to operate, reduces production cost, and production process is safe and reliable.
Detailed description of the invention
Fig. 1 is the schematic diagram of continuous still system provided by the invention；
Fig. 2 is the flow diagram of the synthetic method of high-purity chlorosulphonyl isocyanate provided by the invention.
Specific embodiment
For a further understanding of the present invention, below with reference to embodiment to high-purity chlorosulphonyl isocyanate provided by the invention
Synthetic method is illustrated, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
Present embodiments providing a kind of continuous still system includes:
De- light upper tower, Tuo Qingzhong tower and the de- gently lower tower being sequentially connected from top to bottom, described take off are opened in the middle part of gently upper tower
Equipped with feed liquid port；
The weight-removing column that liquid inlet is connected with the liquid outlet of the de- light lower tower, the weight-removing column top is provided with distillation
Front-end volatiles outlet, the weight-removing column middle part are provided with product outlet, and the weight-removing column lower part is provided with recombination sub-export.
The de- gently upper tower, Tuo Qingzhong tower, de- gently lower tower and weight-removing column are packed tower, and filler is selected from 700Y screen waviness
Filler.
Wherein, the filler in the de- light upper tower is subsection setup, and the filler in the de- light upper tower is divided into upper section filler
With lower section filler, the feed liquid port is opened in de- gently upper tower tower wall and the position between upper section filler and lower section filler
It sets.
The filler of the de- light middle tower and de- light lower tower is without subsection setup.
The liquid outlet of the de- light upper tower is connected with the liquid inlet for taking off tower in light, the liquid of the de- light above tower
Outlet is set to the bottom end of the de- light upper tower, and the liquid inlet for taking off tower in light is set to the top of the de- light middle tower,
And it is located at the position of the filler in de- light middle tower or more.
The liquid outlet of the de- light middle tower is connected with the liquid inlet for taking off light lower tower, the liquid of the de- gently middle tower
Outlet is set to the bottom end of the de- light middle tower, and the liquid inlet of the de- light lower tower is set to the top of the de- gently lower tower,
And it is located at the position of the filler of de- light lower tower tower wall or more.
Filler in the weight-removing column is subsection setup, in the weight-removing column filler be divided into upper section filler, middle section filler with
And lower section filler；
The liquid outlet of the de- light lower tower is connected with the liquid inlet of the weight-removing column, and the liquid of the de- light lower tower enters
Mouth is set to the de- gently lower tower bottom end, during the liquid inlet of the weight-removing column is opened in the weight-removing column tower wall and is located at
Position between section filler and lower section filler.
The weight-removing column top is provided with the outlet of distillation front-end volatiles, and the front-end volatiles outlet is opened in the weight-removing column tower
Wall and the position for being located at the upper section filler or more；
It is provided with product outlet in the middle part of the weight-removing column, the product outlet is opened in the weight-removing column tower wall, and is located at
Position between middle section filler and lower section filler；
The weight-removing column lower part is provided with recombination sub-export, and the recombination sub-export is opened in weight-removing column bottom.
Pressure in the continuous still system is 1.5~2.0MPa.
When carrying out positive pressure continuous still, the tower top of the de- light upper tower, Tuo Qingzhong tower, de- light lower tower and weight-removing column is controlled
Temperature is 93~100 DEG C.
When following example 2~4 carry out continuous still, continuous still system provided by embodiment 1 is selected.
Embodiment 2
20mL chlorosulfonic acid isocyanate is added into reaction unit as reaction dissolvent, then by a certain amount of while being passed through three
Sulfur oxide 80.06g and chlorine cyanogen 61.47g keeps 30 DEG C of temperature reactions.Reaction solution is warming up to 120 DEG C to thermally decompose, is recycled
Sulfur trioxide is passed through in next sulfonating reaction.Reaction solution after thermal decomposition is subjected to rectifying, reaction solution uses the side of continuous still
Formula carries out.Gently lower tower reactor bottom heating is taken off while charging to open, and tower and de- gently upper tower heating in light is absolved again later, when the pressure in kettle
Power reaches 1.7Mpa, and tower top temperature reaches 95 DEG C, infinite reflux 2 hours, guarantees continuously to feed again after the completion of thermal decomposition sufficiently, simultaneously
Foreshot and finished product continuously produce, and obtaining purity is 99.5% chlorosulphonyl isocyanate 118.9g, and yield of product reaches
84% or more.
Embodiment 3
Batch front-end volatiles on 20mL are added into reaction unit and are then passed through three oxidations simultaneously by certain as reaction dissolvent
Sulphur 80.06g, chlorine cyanogen 61.47g and gas recovery keep 34 DEG C of temperature reactions.Reaction solution is warming up to 100 DEG C to thermally decompose,
Recycle sulfur trioxide.Reaction solution after thermal decomposition is subjected to rectifying, reaction solution is carried out by the way of continuous still.What is fed is same
When de- gently lower tower reactor bottom heating open, absolve tower and de- gently upper tower heating in light again later, when the pressure in kettle reaches 1.5Mpa, tower
Top temperature reaches 93 DEG C, infinite reflux 2 hours, guarantees continuously to feed again after the completion of thermal decomposition sufficiently, at the same before evaporate it is continuous with finished product
Extraction, obtaining purity is 99.5% chlorosulphonyl isocyanate 121.6g, and yield of product reaches 86% or more.
Embodiment 4
Batch front-end volatiles on 20mL are added into reaction unit and are then passed through three oxidations simultaneously by certain as reaction dissolvent
Sulphur 80.06g, chlorine cyanogen 61.47g and gas recovery keep 36 DEG C of temperature reactions.Reaction solution is warming up to 110 DEG C to thermally decompose,
Recycle sulfur trioxide.Reaction solution after thermal decomposition is subjected to rectifying, reaction solution is carried out by the way of continuous still.What is fed is same
When de- gently lower tower reactor bottom heating open, absolve tower and de- gently upper tower heating in light again later, when the pressure in kettle reaches 2.0Mpa, tower
Top temperature reaches 100 DEG C, infinite reflux 2 hours, guarantees continuously to feed again after the completion of thermal decomposition sufficiently, at the same before evaporate it is continuous with finished product
Extraction, obtaining purity is 99.5% chlorosulphonyl isocyanate 120.9g, and yield of product reaches 85% or more.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of synthetic method of high-purity chlorosulphonyl isocyanate, which comprises the following steps:
A) under diluent existence condition, sulfur trioxide and chlorine cyanogen is subjected to sulfonating reaction, obtain reaction solution；
B the reaction solution) is subjected to pyrolysis, the reaction solution after being thermally decomposed；
C the reaction solution after the thermal decomposition) is subjected to positive pressure continuous still, is evaporated before obtaining high-purity chlorosulphonyl isocyanate and distillation
Point；
The diluent is selected from chlorosulphonyl isocyanate or step C) obtained distillation front-end volatiles.
2. synthetic method according to claim 1, which is characterized in that the temperature of the sulfonating reaction is 28~43 DEG C.
3. synthetic method according to claim 1, which is characterized in that the molar ratio of the sulfur trioxide and chlorine cyanogen is 1:
(0.8~1.2).
4. synthetic method according to claim 1, which is characterized in that the temperature of the pyrolysis is 100~120
℃。
5. synthetic method according to claim 1, which is characterized in that the positive pressure continuous still is in continuous still system
It carries out, the continuous still system, comprising:
De- light upper tower, Tuo Qingzhong tower and the de- gently lower tower being sequentially connected from top to bottom, described take off offer in the middle part of gently upper tower
Feed liquid port；
The weight-removing column that liquid inlet is connected with the liquid outlet of the de- light lower tower, the weight-removing column top evaporates before being provided with distillation
Sub-export, the weight-removing column middle part are provided with product outlet, and the weight-removing column lower part is provided with recombination sub-export.
6. synthetic method according to claim 5, which is characterized in that the de- gently upper tower, Tuo Qingzhong tower, de- gently lower tower with
And the tower top temperature of weight-removing column is 93~100 DEG C.
7. synthetic method according to claim 1, which is characterized in that the pressure of the positive pressure continuous still be 1.5~
2.0MPa。
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| CN201811353003.8A CN109400506B (en) | 2018-11-14 | 2018-11-14 | Synthesis method of high-purity chlorosulfonyl isocyanate |
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| CN201811353003.8A CN109400506B (en) | 2018-11-14 | 2018-11-14 | Synthesis method of high-purity chlorosulfonyl isocyanate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174860A (en) * | 2020-10-09 | 2021-01-05 | 天津昊然分离科技有限公司 | Process method for preparing chlorosulfonyl isocyanate by continuous reactive distillation |
| CN112321462A (en) * | 2020-11-02 | 2021-02-05 | 四平市精细化学品有限公司 | Method for synthesizing chlorosulfonyl isocyanate by continuous method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174860A (en) * | 2020-10-09 | 2021-01-05 | 天津昊然分离科技有限公司 | Process method for preparing chlorosulfonyl isocyanate by continuous reactive distillation |
| CN112174860B (en) * | 2020-10-09 | 2023-10-13 | 天津昊然分离科技有限公司 | Process method for preparing chlorosulfonyl isocyanate through continuous reactive distillation |
| CN112321462A (en) * | 2020-11-02 | 2021-02-05 | 四平市精细化学品有限公司 | Method for synthesizing chlorosulfonyl isocyanate by continuous method |
| CN112321462B (en) * | 2020-11-02 | 2023-02-24 | 四平市精细化学品有限公司 | Method for synthesizing chlorosulfonyl isocyanate by continuous method |
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