CN112209889A - Method for preparing sulfaquinoxaline without solvent - Google Patents
Method for preparing sulfaquinoxaline without solvent Download PDFInfo
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- CN112209889A CN112209889A CN202010348345.1A CN202010348345A CN112209889A CN 112209889 A CN112209889 A CN 112209889A CN 202010348345 A CN202010348345 A CN 202010348345A CN 112209889 A CN112209889 A CN 112209889A
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- reaction kettle
- sulfaquinoxaline
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D241/00—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings
- C07D241/36—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems
- C07D241/38—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems with only hydrogen or carbon atoms directly attached to the ring nitrogen atoms
- C07D241/40—Benzopyrazines
- C07D241/44—Benzopyrazines with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
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Abstract
The invention discloses a method for preparing sulfaquinoxaline without solvent, which comprises the following steps: adding industrial sulfanilamide, chloride and potassium carbonate into a condensation reaction kettle at room temperature, and uniformly stirring; heating the materials in the condensation reaction kettle to 195-200 ℃, and reacting for 8-9 hours; adding drinking water into the condensation reaction kettle, and stirring until the materials are completely dissolved; pressing to a decoloring reaction kettle; adding active carbon, and stirring and decoloring for 8-15 minutes; filter pressing, namely pressing the filter liquid into a neutralization crystallization reaction kettle; controlling the temperature of the material at 80-85 ℃, dropwise adding a hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8; slowly stirring for growing the crystals for 30 minutes; controlling the temperature of the materials at 80-85 ℃, and continuously dropwise adding a hydrochloric acid solution to adjust the pH value to 1.0; slowly stirring to grow the crystal for 60 minutes; discharging, separating crystal and mother liquor, and drying; washing, spin-drying, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%; collecting powder to obtain the sulfaquinoxaline dry product.
Description
Technical Field
The invention relates to the technical field of pharmaceutical technology, in particular to a method for preparing sulfaquinoxaline without solvent.
Background
The sulfaquinoxaline is a bulk drug for veterinary use. The conventional preparation method of sulfaquinoxaline needs to use an organic solvent, and the subsequent process operation of production has the working procedures of solvent recovery, purification and the like, so that the solvent volatilization can be caused, the environment is polluted, and the production cost is increased.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a solvent-free method for preparing sulfaquinoxaline, which has novel technology, is not applicable to an organic solvent in the process of preparing sulfaquinoxaline, reduces the volatilization pollution of the solvent and reduces the production cost.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing sulfaquinoxaline without solvent comprises the following steps:
s1, adding industrial sulfanilamide, chloride and potassium carbonate into the condensation reaction kettle at room temperature, and uniformly stirring;
s2, heating the materials in the condensation reaction kettle to 195-200 ℃, keeping the temperature of the system at 195-200 ℃, and reacting for 8-9 hours;
s3, after the reaction is finished, adding drinking water into the condensation reaction kettle, and stirring until the materials are completely dissolved;
s4, pressing the material liquid in the condensation reaction kettle to a decoloring reaction kettle;
s5, adding activated carbon into the decoloring reaction kettle, and stirring and decoloring for 8-15 minutes;
s6, performing filter pressing on the materials in the decoloring reaction kettle, and pressing the filter liquid into the neutralization crystallization reaction kettle;
s7, controlling the temperature of the materials in the neutralization crystallization reaction kettle to be 80-85 ℃, dropwise adding a hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8;
s8, stopping dripping the hydrochloric acid, and slowly stirring for growing the crystals for 30 minutes;
s9, controlling the temperature of the material to be 80-85 ℃, and continuously dropwise adding a hydrochloric acid solution to adjust the pH value to 1.0;
s10, stopping dripping the hydrochloric acid, and slowly stirring for growing the crystal for 60 minutes;
s11, discharging, separating crystals and mother liquor, and drying the mother liquor in the crystals;
s12, washing the crystal with water and then drying the crystal;
s13, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%;
and S14, collecting powder to obtain the sulfaquinoxaline dry product.
Preferably, in step S6, the activated carbon in the decoloring reactor is simultaneously washed with drinking water, and the washing liquid is collectively pressed into the neutralization crystallization reactor.
Preferably, in the step S1, the weight parts of the raw materials are: 220-230 parts of industrial sulfanilamide, 190-210 parts of chloride and 200-220 parts of potassium carbonate.
Preferably, in the step S3, the ratio of the sum of the mass of the industrial sulfanilamide, the chloride and the potassium carbonate to the volume of the drinking water is 0.5-1 kg/L.
Preferably, in the step S5, the ratio of the mass of the activated carbon to the volume of the drinking water in the step S3 is 0.01-0.02 kg/L.
Preferably, in the step S6, the ratio of the mass of the activated carbon to the volume of the drinking water subjected to water washing is 0.05 to 0.07 kg/L.
Preferably, in the steps S8 and S10, the hydrochloric acid solution is a 1:1 hydrochloric acid solution by volume ratio.
The invention has the beneficial effects that: the invention provides a process method for synthesizing sulfaquinoxaline without solvent, which does not use organic solvent in the process of preparing the sulfaquinoxaline. The preparation method reduces the operation procedures of solvent recovery and purification and the like, avoids the harm of solvent volatilization to pollute the environment, reduces the production cost, improves the production yield of the sulfaquinoxaline and improves the quality of the sulfaquinoxaline.
Detailed Description
The claimed solution of the present invention will now be described in further detail with reference to examples.
Example one
The method for preparing sulfaquinoxaline without solvent in the embodiment comprises the following steps:
s1, adding 220kg of industrial sulfanilamide, 190kg of chloride and 200kg of potassium carbonate into a condensation reaction kettle at room temperature, and uniformly stirring.
S2, heating the materials in the condensation reaction kettle to 195-200 ℃, keeping the temperature of the system at 195-200 ℃, and reacting for 8-9 hours.
S3, after the reaction is finished, 1200L of drinking water is added into the condensation reaction kettle, and the mixture is stirred until the materials are completely dissolved.
S4, pressing the materials in the condensation reaction kettle to a decoloring reaction kettle.
S5, adding 20kg of activated carbon into the decoloring reaction kettle, and stirring and decoloring for 8-15 minutes.
And S6, performing filter pressing on the materials in the decoloring reaction kettle, simultaneously washing the activated carbon in the decoloring reaction kettle by using 300L of drinking water, and pressing the filtrate and the washing liquid into the neutralization crystallization reaction kettle.
And S7, controlling the temperature of the materials in the neutralization crystallization reaction kettle to be 80-85 ℃, dropwise adding 1:1 hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8.
And S8, stopping dripping the hydrochloric acid solution, and slowly stirring for growing the crystal for 30 minutes.
S9, controlling the temperature of the materials to be 80-85 ℃, and continuously dropwise adding a 1:1 hydrochloric acid solution to adjust the pH value to 1.0.
And S10, stopping dripping the hydrochloric acid solution, and slowly stirring for crystal growth for 60 minutes.
S11, discharging, separating crystals and mother liquor, and drying the mother liquor in the crystals.
And S12, washing the crystal with water and then drying the crystal.
S13, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%.
S14, collecting powder to obtain 290-293 kg of sulfaquinoxaline dry product.
Example two
The method for preparing sulfaquinoxaline without solvent in the embodiment comprises the following steps:
s1, adding 230kg of industrial sulfanilamide, 210kg of chloride and 220kg of potassium carbonate into a condensation reaction kettle at room temperature, and uniformly stirring.
S2, heating the materials in the condensation reaction kettle to 195-200 ℃, keeping the temperature of the system at 195-200 ℃, and reacting for 8-9 hours.
S3, after the reaction is finished, 1200L of drinking water is added into the condensation reaction kettle, and the mixture is stirred until the materials are completely dissolved.
S4, pressing the materials in the condensation reaction kettle to a decoloring reaction kettle.
S5, adding 20kg of activated carbon into the decoloring reaction kettle, and stirring and decoloring for 8-15 minutes.
And S6, performing filter pressing on the materials in the decoloring reaction kettle, simultaneously washing the activated carbon in the decoloring reaction kettle by using 300L of drinking water, and pressing the filtrate and the washing liquid into the neutralization crystallization reaction kettle.
And S7, controlling the temperature of the materials in the neutralization crystallization reaction kettle to be 80-85 ℃, dropwise adding 1:1 hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8.
And S8, stopping dripping the hydrochloric acid solution, and slowly stirring for growing the crystal for 30 minutes.
S9, controlling the temperature of the materials to be 80-85 ℃, and continuously dropwise adding a 1:1 hydrochloric acid solution to adjust the pH value to 1.0.
And S10, stopping dripping the hydrochloric acid solution, and slowly stirring for crystal growth for 60 minutes.
S11, discharging, separating crystals and mother liquor, and drying the mother liquor in the crystals.
And S12, washing the crystal with water and then drying the crystal.
S13, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%.
S14, collecting powder to obtain 305-310 kg of sulfaquinoxaline dry product.
EXAMPLE III
The method for preparing sulfaquinoxaline without solvent in the embodiment comprises the following steps:
s1, adding 228kg of industrial sulfanilamide, 200kg of chloride and 210kg of potassium carbonate into a condensation reaction kettle at room temperature, and uniformly stirring.
S2, heating the materials in the condensation reaction kettle to 195-200 ℃, keeping the temperature of the system at 195-200 ℃, and reacting for 8-9 hours.
S3, after the reaction is finished, 1200L of drinking water is added into the condensation reaction kettle, and the mixture is stirred until the materials are completely dissolved.
S4, pressing the materials in the condensation reaction kettle to a decoloring reaction kettle.
S5, adding 20kg of activated carbon into the decoloring reaction kettle, and stirring and decoloring for 8-15 minutes.
And S6, performing filter pressing on the materials in the decoloring reaction kettle, simultaneously washing the activated carbon in the decoloring reaction kettle by using 300L of drinking water, and pressing the filtrate and the washing liquid into the neutralization crystallization reaction kettle.
And S7, controlling the temperature of the materials in the neutralization crystallization reaction kettle to be 80-85 ℃, dropwise adding 1:1 hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8.
And S8, stopping dripping the hydrochloric acid solution, and slowly stirring for growing the crystal for 30 minutes.
S9, controlling the temperature of the materials to be 80-85 ℃, and continuously dropwise adding a 1:1 hydrochloric acid solution to adjust the pH value to 1.0.
And S10, stopping dripping the hydrochloric acid solution, and slowly stirring for crystal growth for 60 minutes.
S11, discharging, separating crystals and mother liquor, and drying the mother liquor in the crystals.
And S12, washing the crystal with water and then drying the crystal.
S13, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%.
S14, collecting powder to obtain 302-308 kg of sulfaquinoxaline dry products.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to limit the present invention in any way. Those skilled in the art can make many changes and modifications to the disclosed embodiments, or modify equivalent embodiments to practice the disclosed embodiments, without departing from the scope of the disclosed embodiments. Therefore, equivalent variations made according to the idea of the present invention should be covered within the protection scope of the present invention without departing from the contents of the technical solution of the present invention.
Claims (7)
1. A method for preparing sulfaquinoxaline without solvent is characterized by comprising the following steps:
s1, adding industrial sulfanilamide, chloride and potassium carbonate into the condensation reaction kettle at room temperature, and uniformly stirring;
s2, heating the materials in the condensation reaction kettle to 195-200 ℃, keeping the temperature of the system at 195-200 ℃, and reacting for 8-9 hours;
s3, after the reaction is finished, adding drinking water into the condensation reaction kettle, and stirring until the materials are completely dissolved;
s4, pressing the material liquid in the condensation reaction kettle to a decoloring reaction kettle;
s5, adding activated carbon into the decoloring reaction kettle, and stirring and decoloring for 8-15 minutes;
s6, performing filter pressing on the materials in the decoloring reaction kettle, and pressing the filter liquid into the neutralization crystallization reaction kettle;
s7, controlling the temperature of the materials in the neutralization crystallization reaction kettle to be 80-85 ℃, dropwise adding a hydrochloric acid solution within 45-60 minutes, and adjusting the pH value to 1.8;
s8, stopping dripping the hydrochloric acid, and slowly stirring for growing the crystals for 30 minutes;
s9, controlling the temperature of the material to be 80-85 ℃, and continuously dropwise adding a hydrochloric acid solution to adjust the pH value to 1.0;
s10, stopping dripping the hydrochloric acid, and slowly stirring for growing the crystal for 60 minutes;
s11, discharging, separating crystals and mother liquor, and drying the mother liquor in the crystals;
s12, washing the crystal with water and then drying the crystal;
s13, discharging, crushing, and drying at 110-120 ℃ until the water content is less than or equal to 1.0%;
and S14, collecting powder to obtain the sulfaquinoxaline dry product.
2. The solventless process for preparing sulfaquinoxaline according to claim 1, wherein: in the step S6, the activated carbon in the decoloring reactor is washed with drinking water, and the washing liquid is pressed into the neutralization crystallization reactor.
3. The solventless process for preparing sulfaquinoxaline according to claim 1, wherein: in the step S1, the raw materials are in parts by weight: 220-230 parts of industrial sulfanilamide, 190-210 parts of chloride and 200-220 parts of potassium carbonate.
4. The solventless process for preparing sulfaquinoxaline according to claim 1, wherein: in the step S3, the ratio of the sum of the mass of the industrial sulfanilamide, the chloride and the potassium carbonate to the volume of the drinking water is 0.5-1 kg/L.
5. The solventless process for preparing sulfaquinoxaline according to claim 1, wherein: in the step S5, the ratio of the mass of the activated carbon to the volume of the drinking water in the step S3 is 0.01-0.02 kg/L.
6. The solventless process for preparing sulfaquinoxaline according to claim 2, wherein: in the step S6, the ratio of the mass of the activated carbon to the volume of the drinking water subjected to water washing is 0.05-0.07 kg/L.
7. The solventless process for preparing sulfaquinoxaline according to claim 1, wherein: in the step S8 and the step S10, the hydrochloric acid solution is a hydrochloric acid solution with a volume ratio of 1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010348345.1A CN112209889A (en) | 2020-04-28 | 2020-04-28 | Method for preparing sulfaquinoxaline without solvent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010348345.1A CN112209889A (en) | 2020-04-28 | 2020-04-28 | Method for preparing sulfaquinoxaline without solvent |
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| CN112209889A true CN112209889A (en) | 2021-01-12 |
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| CN202010348345.1A Pending CN112209889A (en) | 2020-04-28 | 2020-04-28 | Method for preparing sulfaquinoxaline without solvent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539172A (en) * | 2022-03-25 | 2022-05-27 | 浙江工业大学 | Method for continuously preparing sulfaquinoxaline without solvent |
| CN114735872A (en) * | 2022-03-17 | 2022-07-12 | 佛山市南海北沙制药有限公司 | Method for recycling and reusing sulfanilamide quinoxaline process wastewater |
-
2020
- 2020-04-28 CN CN202010348345.1A patent/CN112209889A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李俊飞 等: "磺胺喹噁啉合成工艺研究", 《山西大学学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114735872A (en) * | 2022-03-17 | 2022-07-12 | 佛山市南海北沙制药有限公司 | Method for recycling and reusing sulfanilamide quinoxaline process wastewater |
| CN114539172A (en) * | 2022-03-25 | 2022-05-27 | 浙江工业大学 | Method for continuously preparing sulfaquinoxaline without solvent |
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