CN110452135A - A kind of N-acetylsulfanilyl chloride novel crystallization method - Google Patents
A kind of N-acetylsulfanilyl chloride novel crystallization method Download PDFInfo
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- CN110452135A CN110452135A CN201910912852.0A CN201910912852A CN110452135A CN 110452135 A CN110452135 A CN 110452135A CN 201910912852 A CN201910912852 A CN 201910912852A CN 110452135 A CN110452135 A CN 110452135A
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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
- C07C303/08—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 halogenosulfonic acids
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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
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
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Abstract
The present invention relates to chemical industry purification technique fields, disclose a kind of N-acetylsulfanilyl chloride novel crystallization method, antifebrin, chlorosulfonic acid are added in reaction kettle, level-one slurry is formed after stirring, continues to form second level slurry after insulated and stirred, ice water is added in second level slurry and forms three-level slurry, three-level slurry is passed into level-one vacuum crystallizer, three-level slurry is gradually concentrated, and ultimately forms level-one magma, crystal grain is gradually precipitated in level-one magma.The present invention passes through setting level-one vacuum crystallizer and secondary vacuum crystallizer, three-level slurry cools down automatically with acid solution, no setting is required heat-transfer surface, it avoids crystal and generates a large amount of brilliant dirt on heat-transfer area, quantity and the growth rate for controlling nucleus are more convenient, and by setting level-one ultrasonic wave assisting crystallisation device and second level ultrasonic wave assisting crystallisation device, nucleation rate is fast, crystallization time shortens, homogeneous grain size obtained.
Description
Technical field
The present invention relates to chemical industry purification technique field, specially a kind of N-acetylsulfanilyl chloride novel crystallization method.
Background technique
N-acetylsulfanilyl chloride is a kind of important chemical intermediate, is to prepare the mould drug of sulfamido sterilization suppression to commonly use
Pharmaceutical intermediate, synthetic dyestuffs can be used directly to, can be used for synthesis para-ester and in the dyestuffs such as bit amino oil
Mesosome is widely used in the fields such as medicine, coating, plastics and pesticide, currently, N-acetylsulfanilyl chloride production mostly uses greatly
The traditional handicraft of excessive chlorosulfonic acid method, synthesis intermediate product hydrolyzation material need to be diluted with water so that acetylaminobenzene sulphur is precipitated
Acyl chlorides crystal, common method is the dilution device that interval is formed with the dilution kettle with stirring and storage tank and discharging pump, used
Dilution equipment quantity is more, takes up a large area, and causes inconvenience to workshop appliance arrangement, and equipment cost is high, utilization rate is low.
Acetylaminobenzene is used for disclosed in Chinese utility model patent ublic specification of application CN208995421U
The serial dilution device of sulfonic acid chloride cooling Crystallization Process, in crystallization process, partial crystals fouling on container reduces and is made
The efficiency of yield afterwards, crystallization is lower, and brilliant dirt also will affect whole crystal quality after falling off, and is not easy to the item of control crystallization
Part and rate of crystalline growth, grain size is uneven, and the quality of crystal grain is lower.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of N-acetylsulfanilyl chloride novel crystallization method, tools
The advantages that standby homogeneous grain size, crystallization rate are fast and are not easy fouling, solve solution influenced vulnerable to coolant temperature and
Easy fouling, grain size is uneven and crystallizes time used longer problem.
(2) technical solution
To realize that above-mentioned preparation homogeneous grain size, crystallization rate are fast and being not easy the purpose of fouling, the present invention is provided
Following technical solution:
Preferably, the ratio of the antifebrin and chlorosulfonic acid is 1:5~1:6, and the whipping temp of the level-one slurry is
11 DEG C~65 DEG C.
Preferably, the temperature of the reacting kettle jacketing steam is 63 ± 2 DEG C, and the temperature of the ice water is 7 DEG C~9 DEG C.
Preferably, 5 DEG C~10 DEG C of the temperature of the three-level slurry, the temperature of the level-one magma are 3 DEG C~4 DEG C.
Preferably, the absolute pressure in the level-one vacuum crystallizer is 4000Pa~4500Pa, the secondary vacuum knot
Absolute pressure in brilliant device is 6000Pa~6500Pa.
Preferably, it is 30KHz~40KHz that the level-one ultrasonic wave assisting crystallisation device, which issues the frequency of ultrasonic wave, described two
The frequency that grade ultrasonic wave assisting crystallisation device issues ultrasonic wave is 35KHz~45KHz.
Preferably, the sieve is 32 mesh~35 mesh, and the temperature of the second level magma is 1 DEG C~2 DEG C.
Preferably, the temperature in the level-one vacuum crystallizer is 4 DEG C~5 DEG C, the temperature in the secondary vacuum crystallizer
Degree is 2 DEG C~3 DEG C.
Preferably, the mixing speed of the level-one slurry is 190 revs/min~360 revs/min, and the ice water is distilled water.
The present invention provides a kind of N-acetylsulfanilyl chloride novel crystallization method, comprising the following steps:
1) antifebrin, chlorosulfonic acid are added in reaction kettle, stirring mixes them thoroughly, and forms level-one slurry.
2) be passed through steam in reacting kettle jacketing, level-one slurry made to be warming up to 60 DEG C~65 DEG C, and continue insulated and stirred 2~
Second level slurry is formed after 3 hours, reaction 2~3 hours, ice water dilution is gradually added into second level slurry, forms three-level slurry.
3) three-level slurry being passed into level-one vacuum crystallizer, level-one vacuum crystallizer keeps certain vacuum degree, and three
Grade slurry flashes in level-one vacuum crystallizer, and subsequent three-level slurry is gradually concentrated, and temperature reduces, and ultimately forms level-one crystalline substance
Slurry.
4) level-one ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into level-one vacuum crystallizer, in level-one magma gradually
Crystal grain is precipitated, is continually fed into ice water and level-one magma is rinsed with crystal grain, until the ice water after rinsing is in neutrality, qualified crystalline substance
Grain is sifted out by sieve, is subsequently passed strong wind and is dried.
5) by flowing into secondary vacuum crystallizer after sieve, second level is true for the acid solution in level-one magma and lesser crystal grain
Empty crystallizer keeps higher vacuum degree, and acid solution flashes in secondary vacuum crystallizer, and subsequent acid solution is gradually concentrated, and temperature drops
It is low, ultimately form second level magma.
6) second level ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into secondary vacuum crystallizer, in second level magma gradually
Crystal grain is precipitated, is continually fed into ice water and second level magma is rinsed with crystal grain, until the ice water after rinsing is in neutrality, qualified crystalline substance
Grain is sifted out by sieve, is subsequently passed strong wind and is dried, remaining liquid is recycled.
(3) beneficial effect
Compared with prior art, the present invention provides a kind of N-acetylsulfanilyl chloride novel crystallization method, have with
It is lower the utility model has the advantages that
1, the N-acetylsulfanilyl chloride novel crystallization method passes through setting level-one vacuum crystallizer and secondary vacuum knot
Brilliant device, three-level slurry cool down automatically with acid solution, no setting is required heat-transfer surface, avoid crystal and generate a large amount of crystalline substance on heat-transfer area
Dirt, without clearing up thicker brilliant dirt, high production efficiency controls the quantity of nucleus convenient for maintaining advantageous crystallization condition
It is more convenient with growth rate, in addition, qualified crystal grain is screened with underproof crystal grain, is convenient for by setting sieve
Improve the quality of crystal grain.
2, the N-acetylsulfanilyl chloride novel crystallization method passes through setting level-one ultrasonic wave assisting crystallisation device and second level
Ultrasonic wave assisting crystallisation device, nucleation rate is fast, and crystallization time shortens, and Growing Process of Crystal Particles is steady, and crystalline form is good, crystal grain obtained
Uniform in size, crystal growth generates brilliant dirt later on inner wall, and brilliant dirty by ultrasonic oscillation, constantly falling off, it is brilliant then to be formed
Body increases the yield and purity of crystal.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1:
Antifebrin, chlorosulfonic acid are added in reaction kettle, the ratio of antifebrin and chlorosulfonic acid is 1:5.26, stirs second
Anilide is allowed to be sufficiently mixed with chlorosulfonic acid, forms level-one slurry, and the whipping temp of level-one slurry is 15 DEG C, and level-one slurry stirs
Mixing speed is 200 revs/min, and steam is passed through in reacting kettle jacketing, and the temperature of reacting kettle jacketing steam is 61 DEG C, makes level-one slurry
60 DEG C are warming up to, and continues insulated and stirred 2 hours, second level slurry is formed after reaction 2 hours, is gradually added into second level slurry
Ice water dilution, the temperature of ice water are 9 DEG C, and ice water is distilled water, form three-level slurry later, and the temperature of three-level slurry is 10 DEG C,
Three-level slurry is passed into level-one vacuum crystallizer, level-one vacuum crystallizer keeps certain vacuum degree, level-one vacuum crystallization
Absolute pressure in device is 4000Pa, and the temperature in level-one vacuum crystallizer is 5 DEG C, and three-level slurry is in level-one vacuum crystallizer
Flash distillation, subsequent three-level slurry are gradually concentrated, and temperature reduces, and ultimately form level-one magma, and the temperature of level-one magma is 4 DEG C, will
Level-one ultrasonic wave assisting crystallisation device issues ultrasonic wave and is introduced into level-one vacuum crystallizer, and level-one ultrasonic wave assisting crystallisation device issues super
The frequency of sound wave is 30KHz, and crystal grain is gradually precipitated in level-one magma, is continually fed into ice water and floats to level-one magma with crystal grain
It washes, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, it is subsequently passed strong wind and is dried, sieve 32
Mesh, the acid solution and lesser crystal grain in level-one magma after sieve by flowing into secondary vacuum crystallizer, secondary vacuum crystallization
Device keeps higher vacuum degree, and the absolute pressure in secondary vacuum crystallizer is 6000Pa, the temperature in secondary vacuum crystallizer
It is 3 DEG C, acid solution flashes in secondary vacuum crystallizer, and subsequent acid solution is gradually concentrated, and temperature reduces, and ultimately forms second level crystalline substance
Slurry, the temperature of second level magma are 2 DEG C, and second level ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into secondary vacuum crystallizer,
The frequency that second level ultrasonic wave assisting crystallisation device issues ultrasonic wave is 35KHz, and crystal grain is gradually precipitated in second level magma, is continually fed into ice
Water rinses second level magma with crystal grain, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, then logical
Enter strong wind to be dried, remaining liquid is recycled.
The yield of crystal is higher in the present embodiment 1, and Growing Process of Crystal Particles is steady, and crystalline form is good, and lopsided crystal grain is less, crystal grain
Purity is high, the raw material availability for preparing N-acetylsulfanilyl chloride crystal is high, and production waste liquid is less.
Embodiment 2:
Antifebrin, chlorosulfonic acid are added in reaction kettle, the ratio of antifebrin and chlorosulfonic acid is 1:5.26, stirs second
Anilide is allowed to be sufficiently mixed with chlorosulfonic acid, forms level-one slurry, and the whipping temp of level-one slurry is 15 DEG C, and level-one slurry stirs
Mixing speed is 200 revs/min, and steam is passed through in reacting kettle jacketing, and the temperature of reacting kettle jacketing steam is 61 DEG C, makes level-one slurry
60 DEG C are warming up to, and continues insulated and stirred 2 hours, second level slurry is formed after reaction 2 hours, is gradually added into second level slurry
Ice water dilution, the temperature of ice water are 9 DEG C, and ice water is distilled water, form three-level slurry later, and the temperature of three-level slurry is 10 DEG C,
Three-level slurry is passed into level-one vacuum crystallizer, level-one vacuum crystallizer keeps higher vacuum degree, level-one vacuum crystallization
Absolute pressure in device is 4500Pa, and the temperature in level-one vacuum crystallizer is 5 DEG C, and three-level slurry is in level-one vacuum crystallizer
Flash distillation, subsequent three-level slurry are gradually concentrated, and temperature reduces, and ultimately form level-one magma, and the temperature of level-one magma is 4 DEG C, will
Level-one ultrasonic wave assisting crystallisation device issues ultrasonic wave and is introduced into level-one vacuum crystallizer, and level-one ultrasonic wave assisting crystallisation device issues super
The frequency of sound wave is 30KHz, and crystal grain is gradually precipitated in level-one magma, is continually fed into ice water and floats to level-one magma with crystal grain
It washes, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, it is subsequently passed strong wind and is dried, sieve 35
Mesh, the acid solution and lesser crystal grain in level-one magma after sieve by flowing into secondary vacuum crystallizer, secondary vacuum crystallization
Device keeps higher vacuum degree, and the absolute pressure in secondary vacuum crystallizer is 6500Pa, the temperature in secondary vacuum crystallizer
It is 3 DEG C, acid solution flashes in secondary vacuum crystallizer, and subsequent acid solution is gradually concentrated, and temperature reduces, and ultimately forms second level crystalline substance
Slurry, the constant temperature of second level magma are 2 DEG C, and second level ultrasonic wave assisting crystallisation device is issued ultrasonic wave and introduces secondary vacuum crystallizer
In, the frequency that second level ultrasonic wave assisting crystallisation device issues ultrasonic wave is 35KHz, and crystal grain is gradually precipitated in second level magma, persistently leads to
Enter ice water and second level magma is rinsed with crystal grain, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, with
After be passed through strong wind and be dried, remaining liquid is recycled.
The present embodiment difference from example 1 is that: absolute pressure and secondary vacuum in level-one vacuum crystallizer
Absolute pressure in crystallizer is higher, and crystallization rate is fast, optimizes the pressure condition of crystallization, facilitates the quality for promoting crystal grain.
Embodiment 3:
Antifebrin, chlorosulfonic acid are added in reaction kettle, the ratio of antifebrin and chlorosulfonic acid is 1:5.26, stirs second
Anilide is allowed to be sufficiently mixed with chlorosulfonic acid, forms level-one slurry, and the whipping temp of level-one slurry is 15 DEG C, and level-one slurry stirs
Mixing speed is 200 revs/min, and steam is passed through in reacting kettle jacketing, and the temperature of reacting kettle jacketing steam is 61 DEG C, makes level-one slurry
60 DEG C are warming up to, and continues insulated and stirred 2 hours, second level slurry is formed after reaction 2 hours, is gradually added into second level slurry
Ice water dilution, the temperature of ice water are 9 DEG C, and ice water is distilled water, form three-level slurry later, and the temperature of three-level slurry is 10 DEG C,
Three-level slurry is passed into level-one vacuum crystallizer, level-one vacuum crystallizer keeps certain vacuum degree, level-one vacuum crystallization
Absolute pressure in device is 4000Pa, and the temperature in level-one vacuum crystallizer is 5 DEG C, and three-level slurry is in level-one vacuum crystallizer
Flash distillation, subsequent three-level slurry are gradually concentrated, and temperature reduces, and ultimately form level-one magma, and the temperature of level-one magma is 4 DEG C, will
Level-one ultrasonic wave assisting crystallisation device issues ultrasonic wave and is introduced into level-one vacuum crystallizer, and level-one ultrasonic wave assisting crystallisation device issues super
The frequency of sound wave is 40KHz, and crystal grain is gradually precipitated in level-one magma, is continually fed into ice water and floats to level-one magma with crystal grain
It washes, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, it is subsequently passed strong wind and is dried, sieve 35
Mesh, the acid solution and lesser crystal grain in level-one magma after sieve by flowing into secondary vacuum crystallizer, secondary vacuum crystallization
Device keeps higher vacuum degree, and the absolute pressure in secondary vacuum crystallizer is 6000Pa, the temperature in secondary vacuum crystallizer
It is 2 DEG C, acid solution flashes in secondary vacuum crystallizer, and subsequent acid solution is gradually concentrated, and temperature reduces, and ultimately forms second level crystalline substance
Slurry, the temperature of second level magma are 1 DEG C, and second level ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into secondary vacuum crystallizer,
The frequency that second level ultrasonic wave assisting crystallisation device issues ultrasonic wave is 45KHz, and crystal grain is gradually precipitated in second level magma, is continually fed into ice
Water rinses second level magma with crystal grain, until the ice water after rinsing is in neutrality, qualified crystal grain is sifted out by sieve, then logical
Enter strong wind to be dried, remaining liquid is recycled.
The present embodiment difference from example 1 is that: level-one ultrasonic wave assisting crystallisation device and second level ultrasonic wave assist
The frequency that crystallizer issues ultrasonic wave is higher, and higher ultrasonic frequency helps to refine crystal grain, and the speed of crystal nucleation becomes
Fastly, crystal is reduced there is a situation where fouling, and crystal size is uniform.
The beneficial effects of the present invention are: by setting level-one vacuum crystallizer and secondary vacuum crystallizer, three-level slurry with
Acid solution cools down automatically, no setting is required heat-transfer surface, avoids crystal and generates a large amount of brilliant dirt on heat-transfer area, without to thicker crystalline substance
Dirt is cleared up, high production efficiency, and convenient for maintaining advantageous crystallization condition, the quantity and growth rate for controlling nucleus are more just
Victory is screened qualified crystal grain with underproof crystal grain by the way that sieve is arranged, convenient for improving the quality of crystal grain, by setting
Level-one ultrasonic wave assisting crystallisation device and second level ultrasonic wave assisting crystallisation device are set, nucleation rate is fast, and crystallization time shortens, grain growth
Process is steady, and crystalline form is good, homogeneous grain size obtained, and crystal growth generates brilliant dirt later on inner wall, brilliant dirty ultrasonic
Wave concussion, constantly falls off and then forms crystal, increase the yield and purity of crystal.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (9)
1. a kind of N-acetylsulfanilyl chloride novel crystallization method, which comprises the following steps:
1) antifebrin, chlorosulfonic acid are added in reaction kettle, stirring mixes them thoroughly, and forms level-one slurry.
2) it is passed through steam in reacting kettle jacketing, so that level-one slurry is warming up to 60 DEG C~65 DEG C, and it is small to continue insulated and stirred 2~3
When, second level slurry is formed after reaction 2~3 hours, ice water dilution is gradually added into second level slurry, forms three-level slurry.
3) three-level slurry is passed into level-one vacuum crystallizer, level-one vacuum crystallizer keeps certain vacuum degree, three-level material
Slurry flashes in level-one vacuum crystallizer, and subsequent three-level slurry is gradually concentrated, and temperature reduces, and ultimately forms level-one magma.
4) level-one ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into level-one vacuum crystallizer, is gradually precipitated in level-one magma
Crystal grain is continually fed into ice water and rinses to level-one magma with crystal grain, until the ice water after rinsing is in neutrality, qualified crystal grain quilt
Sieve sifts out, and is subsequently passed strong wind and is dried.
5) acid solution in level-one magma and lesser crystal grain after sieve by flowing into secondary vacuum crystallizer, secondary vacuum knot
Brilliant device keeps higher vacuum degree, and acid solution flashes in secondary vacuum crystallizer, and subsequent acid solution is gradually concentrated, and temperature reduces,
Ultimately form second level magma.
6) second level ultrasonic wave assisting crystallisation device sending ultrasonic wave is introduced into secondary vacuum crystallizer, is gradually precipitated in second level magma
Crystal grain is continually fed into ice water and rinses to second level magma with crystal grain, until the ice water after rinsing is in neutrality, qualified crystal grain quilt
Sieve sifts out, and is subsequently passed strong wind and is dried, and remaining liquid is recycled.
2. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that the second
The ratio of anilide and chlorosulfonic acid is 1:5~1:6, and the whipping temp of the level-one slurry is 11 DEG C~65 DEG C.
3. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described anti-
The temperature for answering kettle jacket steam is 63 ± 2 DEG C, and the temperature of the ice water is 7 DEG C~9 DEG C.
4. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described three
The temperature of grade slurry is 5 DEG C~10 DEG C, and the temperature of the level-one magma is 3 DEG C~4 DEG C.
5. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described one
Absolute pressure in grade vacuum crystallizer is 4000Pa~4500Pa, and the absolute pressure in the secondary vacuum crystallizer is
6000Pa~6500Pa.
6. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described one
The frequency that grade ultrasonic wave assisting crystallisation device issues ultrasonic wave is 30KHz~40KHz, and the second level ultrasonic wave assisting crystallisation device issues
The frequency of ultrasonic wave is 35KHz~45KHz.
7. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that the sieve
Net is 32 mesh~35 mesh, and the temperature of the second level magma is 1 DEG C~2 DEG C.
8. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described one
Temperature in grade vacuum crystallizer is 4 DEG C~5 DEG C, and the temperature in the secondary vacuum crystallizer is 2 DEG C~3 DEG C.
9. a kind of N-acetylsulfanilyl chloride novel crystallization method according to claim 1, which is characterized in that described one
The mixing speed of grade slurry is 190 revs/min~360 revs/min, and the ice water is distilled water.
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| CN112225635A (en) * | 2020-11-03 | 2021-01-15 | 中国石油化工股份有限公司 | Device, method and application for crystallization and separation of paraxylene |
| CN115259988A (en) * | 2022-08-08 | 2022-11-01 | 中国石油化工股份有限公司 | Separation method and separation system for double-reinforced p-xylene crystallization |
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Application publication date: 20191115 |