CN112500320A - Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate - Google Patents
Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate Download PDFInfo
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- CN112500320A CN112500320A CN202011485470.3A CN202011485470A CN112500320A CN 112500320 A CN112500320 A CN 112500320A CN 202011485470 A CN202011485470 A CN 202011485470A CN 112500320 A CN112500320 A CN 112500320A
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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
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric 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 invention discloses a preparation device and a preparation method of pharmaceutical adjuvant sodium dodecyl sulfate3A sulfonating agent feed port and a dodecanol feed port, wherein the bottom of the sulfonating agent feed port is provided with an acid ester discharge port; the acid ester discharge port is connected with the feed port of the neutralizer; an alkali feeding hole is formed in the neutralizer; the outlet of the neutralizer is connected with the inlet of the homogenizing tank, the bottom discharge port of the homogenizing tank is connected with the feeder, and the feeder is connected with the dryer; the outlet of the dryer, the discharge hole of the quantitative feeder and the air purifier are connected to the cyclone filter through an air supply pipeline; the upper end of the cyclone filter is connected with a first induced draft fan, and the bottom of the cyclone filter is connected with a grinding system; the milling system is connected with a secondary dryer, and the secondary dryer is respectively connected with a second draught fan and a powder homogenizer(ii) a And the second induced draft fan is connected with a fatty alcohol recovery system. The drying process is safe and stable, the content of inorganic salt is low, and the product is not easy to precipitate.
Description
Technical Field
The invention relates to a device and a method for preparing pharmaceutical adjuvant sodium dodecyl sulfate, which are particularly suitable for preparing pharmaceutical powdery sodium dodecyl sulfate with low inorganic salt and low pH value.
Background
Sodium dodecyl sulfate is often used as a pharmaceutical adjuvant such as an emulsifier, a dispersant and the like in pharmacy, the alkalinity is less than 0.6ml (0.1N hydrochloric acid solution), and the pH value is not too high. In addition, sodium dodecyl sulfate belongs to a thermosensitive and acid-unstable surfactant, is easy to rancidity and decompose in a drying process, so that the product quality is reduced, and particularly, in a film scraping and drying process by using a viscous material with the concentration of 70%, the material is unevenly heated, and is easy to rancidity and decompose when being stuck on equipment. When 30% of liquid material is used for spray drying, the powder is easy to stick to the tower, and black spots in the product are caused by long-time high temperature. Therefore, it is common to add a proportion of a stabilizer to the material before drying to stabilize the pH between 7.5 and 9.5. At present, the stabilizers with good pH value of 7.5-9.5 effects include phosphates (including phosphates, polymeric phosphates, etc.), carbonate series, etc., while the sulfates, citrates, EDTA salts have poor pH value stabilizing effects. However, the addition of these inorganic salts can cause the reaction of calcium, aluminum and magnesium ions in the pharmaceutical production process to generate precipitates, which affect the stability of the product.
Disclosure of Invention
The invention aims to overcome the defects that the existing product is easy to precipitate and has high pH value requirement, and provides a device and a method for preparing pharmaceutical adjuvant sodium dodecyl sulfate with low inorganic salt and low pH value.
A preparation device of pharmaceutical adjuvant sodium dodecyl sulfate comprises a sulfonation reactor, a neutralizer, a homogenizing tank, a feeder, a quantitative feeder, a dryer, a cyclone filter, a milling system, a secondary dryer and a powder homogenizer;
the top of the sulfonation reactor is provided with SO3A sulfonating agent feed port and a dodecanol feed port, wherein the bottom of the sulfonating agent feed port is provided with an acid ester discharge port; the acid ester discharge port is connected with the feed port of the neutralizer;
the neutralizer is provided with an alkali feeding hole, and a liquid alkali neutralizer is introduced into the alkali feeding hole;
the outlet of the neutralizer is connected with the inlet of the homogenizing tank, the bottom discharge port of the homogenizing tank is connected with the feeder, and the feeder is connected with the dryer;
the outlet of the dryer, the discharge hole of the quantitative feeder and the air purifier are connected to the cyclone filter through an air supply pipeline;
the upper end of the cyclone filter is connected with a first induced draft fan, and the bottom of the cyclone filter is connected with a grinding system; the induced draft fan is connected with the waste gas treatment system;
the powder grinding system is connected with a secondary dryer, and the secondary dryer is respectively connected with a second induced draft fan and a powder homogenizer; and the second induced draft fan is connected with a fatty alcohol recovery system.
In the invention, a densimeter is arranged between the feed inlets of the sulfonation reactor and the neutralizer.
In the invention, the neutralizer is provided with a pH meter for adjusting the pH value of the neutralized slurry.
In the invention, a powder pH detector is arranged on the powder homogenizer.
The invention also discloses a preparation method of the pharmaceutical adjuvant sodium dodecyl sulfate, which comprises the following steps:
(1) controlling the sulfonation reaction degree: dodecanol and SO3The sulfonation reaction generates lauryl sulfate with the conversion rate of 90-99 percent and the density of the corresponding acid ester of 0.95-1.01 g/cm3The content of the inorganic acid can be obviously reduced by controlling the reaction degree.
(2) And (3) neutralization high pH control: the sulfonated lauryl sulfate reacts with liquid alkali to generate sodium dodecyl sulfate with the pH value of 9.5-11.5, and the aim of controlling the pH value at a high level is to reduce H in the material+And inorganic salt is prevented from being generated by rancidity in the processes of neutralization, drying and the like.
(3) Drying and adjusting the pH value of the powder: and (4) dehydrating and drying the neutralized materials, adding a solid organic acid regulator, and feeding the materials together to a milling system for milling and homogenizing. The addition of solid organic acid will not cause inorganic salt to rise, and the pH value of the powder is 4.5-9.5.
(4) Dealcoholizing: the milled material is heated by hot air to reduce the partial pressure of fatty alcohol to remove most of volatile dodecanol, and the fat removing and recovering system has the removal rate related to temperature and air quantity and hot air temperature of 65-145 ℃.
(5) Mixing and homogenizing: homogenizing the sodium dodecyl sulfate subjected to dealcoholization treatment, detecting the pH value, and packaging after the sodium dodecyl sulfate is qualified.
After the technical scheme is adopted, the invention has the beneficial effects that:
1. the inorganic salt content of the product is obviously reduced, the normal product is more than 1.0 percent, and the content of the product is less than 0.5 percent.
2. The product has low pH value of 4.5-9.5, good stability and no decomposition.
Drawings
FIG. 1 is a schematic diagram of the connection of the system of the present invention.
In the figure: 1. SO (SO)3A sulfonating agent feed port; 2. a dodecanol feed port; 3. an alkali feed port; 4. a solid organic acid modifier; 5. a sulfonation reactor; 5-1, a densimeter; 6. a neutralizer; 6-1, pH meter; 7. a homogenization tank; 8. a feeder; 9. a doser; 10. a dryer; 11. a cyclone filter; 12. a first induced draft fan; 12-1, an air purifier; 12-2, an exhaust gas treatment system; 13. a milling system; 14. a secondary dryer; 14-1 and a second induced draft fan; 14-2, a fatty alcohol recovery system; 15. a powder homogenizer; 15-1, powder pH detector.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
As shown in fig. 1, a device for preparing pharmaceutical excipient sodium dodecyl sulfate: comprises a sulfonation reactor 5, a neutralizer 6, a homogenizing tank 7, a feeder 8, a quantitative feeder 9, a dryer 10, a cyclone filter 11, a milling system 13, a secondary dryer 14 and a powder homogenizer 15;
SO is arranged at the top of the sulfonation reactor 53A sulfonating agent feed port 1 and a dodecanol feed port 2, and an acid ester discharge port is arranged at the bottom of the sulfonating agent feed port and the dodecanol feed port; the acid ester discharge hole is connected with the feed inlet of the neutralizer 6;
the neutralizer 6 is provided with an alkali feed port 3, wherein a liquid alkali neutralizer is introduced;
the outlet of the neutralizer 6 is connected with the inlet of a homogenizing tank 7, the bottom discharge port of the homogenizing tank is connected with a feeder 8, and the feeder 8 is connected with a dryer 10;
the outlet of the dryer 10 and the outlet of the quantitative feeder 9 and the air purifier 12-1 are connected to the cyclone filter 11 through an air supply pipeline;
the upper end of the cyclone filter 11 is connected with a first induced draft fan 12, and the bottom of the cyclone filter is connected with a grinding system 13; the induced draft fan I12 is connected with the waste gas treatment system 12-2;
the grinding system 13 is connected with a secondary dryer 14, and the secondary dryer 14 is respectively connected with a second induced draft fan 14-1 and a powder homogenizer 15; and the second induced draft fan 14-1 is connected with the fatty alcohol recovery system 14-2.
The material outlet at the bottom of the homogenizing tank 7 is fed to a dryer 10 through a feeder 8, the dried material, the solid organic acid regulator 4 from a quantitative feeder 9 and the air purified by an air purifier 12-1 are conveyed to a cyclone filter 11 through an air conveying pipe, and the waste gas is discharged to a waste gas treatment system 12-2 through a first induced draft fan 12. And a solid material milling system 13 at the bottom of the cyclone filter 11 mixes and mills dried lauryl sodium sulfate and solid organic acid into powder, conveys the powder to a secondary dryer 14 to remove unreacted alcohol, and conveys the powder to a fatty alcohol recovery system 14-2 through a second induced draft fan 14-1 to recover fatty alcohol. The dealcoholized sodium dodecyl sulfate is conveyed to a powder homogenizer 15 for homogenization, the pH value is detected by a powder pH detector 15-1, the feeding speed of a quantitative feeder 9 is adjusted according to the pH value, and the pH value is kept in a qualified range.
A densimeter 5-1 is arranged between the feed inlets of the sulfonation reactor 5 and the neutralizer 6, the conversion rate of the sulfonation reaction is mainly controlled, the appropriate conversion rate is kept at 80-99%, and the lower content of inorganic acid in the intermediate sulfonated monomer acid ester is reduced.
The neutralizer 6 is provided with a pH meter 6-1 for adjusting the pH value of the neutralized slurry. Because of the acid instability of the sodium dodecyl sulfate, the pH value is controlled to be relatively higher and is generally controlled to be 9.5-11.5, and H is reduced+Concentration, and prevents the inorganic salt from rising due to rancidity in the processes of material neutralization, storage, drying and the like.
The air supply pipeline is provided with a quantitative feeder 9 for conveying the solid organic acid regulator 4, and the solid organic acid and the material with high pH value are mixed and ground into powder to regulate the pH value to be in the range of 4.5-9.5. The anhydrous sodium dodecyl sulfate is difficult to be rancid, and the organic acid is added only by mixing a small amount of organic acid into the sodium dodecyl sulfate with high pH value, the pH value of the sodium dodecyl sulfate is not reduced, only the pH value of the mixture is 4.5-9.5 after the mixture is dissolved in water, and the inorganic salt is not increased when the mixture is detected.
The powder homogenizer 15 is provided with a powder pH detector 15-1, and the feeding speed of the quantitative feeder is controlled by detecting the pH value of the powder.
The milled powder is provided with a secondary drying dealcoholization system, and volatile matters in the powder are removed by increasing the temperature of hot air (65-145 ℃) to reduce the volatile partial pressure of the dodecanol.
Example 2
A preparation method of a pharmaceutic adjuvant sodium dodecyl sulfate is characterized by comprising the following steps:
(1) controlling the sulfonation reaction degree: 105g of dodecanol and 41.3g of SO3The sulfonation reaction generates 146.3g of lauryl sulfate, and the conversion rate is 95.0 percent;
(2) and (3) neutralization high pH control: the sulfonated lauryl sulfate reacts with 32 percent sodium hydroxide to generate 65.2g of lauryl sodium sulfate, and the pH value is controlled to be 10.5;
(3) drying and adjusting the pH value of the powder: dehydrating and drying the neutralized materials to obtain 162.4g, adding 1.1g of a solid organic acid regulator, and feeding the materials to a powder grinding system to grind and homogenize the materials, wherein the pH value of the powder is 7.6;
(4) dealcoholizing: reducing the partial pressure of fatty alcohol by using hot air to remove most of volatile dodecanol from the milled material, and recovering 4.3g of alcohol by using a de-fatting and recovering system;
(5) mixing and homogenizing: after the lauryl sodium sulfate after dealcoholization is subjected to powder homogenization, 154.5g of powder is subjected to pH value detection of 7.6, and the powder is packaged qualified.
Example 3
A preparation method of a pharmaceutic adjuvant sodium dodecyl sulfate is characterized by comprising the following steps:
(1) controlling the sulfonation reaction degree: 103g of dodecanol and 41.3g of SO3144.3g of lauryl sulfate is generated by sulfonation reaction, and the conversion rate is 97.0 percent;
(2) and (3) neutralization high pH control: the sulfonated lauryl sulfate reacts with 32 percent sodium hydroxide to generate 65.2g of lauryl sodium sulfate, and the pH value is controlled to be 10.3;
(3) drying and adjusting the pH value of the powder: dehydrating and drying the neutralized materials to obtain 160.4g of the neutralized materials, adding 1.0g of a solid organic acid regulator, and feeding the materials to a powder grinding system for grinding and homogenizing to obtain powder with the pH value of 7.9;
(4) dealcoholizing: reducing partial pressure of fatty alcohol by hot air to remove most volatile dodecanol from the milled material, and recovering 2.5g of alcohol by a de-fatting recovery system;
(5) mixing and homogenizing: after the lauryl sodium sulfate subjected to dealcoholization is subjected to powder homogenization, 154g of powder is subjected to pH value detection of 7.9, and the powder is packaged qualified.
Example 4
A preparation method of a pharmaceutic adjuvant sodium dodecyl sulfate is characterized by comprising the following steps:
(1) controlling the sulfonation reaction degree: 103g of dodecanol and 41.3g of SO3144.3g of lauryl sulfate is generated by sulfonation reaction, and the conversion rate is 97.0 percent;
(2) and (3) neutralization high pH control: the sulfonated lauryl sulfate reacts with 32 percent sodium hydroxide to generate 67.8g of lauryl sodium sulfate, and the pH value is controlled to be 10.9;
(3) drying and adjusting the pH value of the powder: dehydrating and drying the neutralized materials to obtain 160.4g of the neutralized materials, adding 5.5g of a solid organic acid regulator, and feeding the materials to a powder grinding system for grinding and homogenizing to obtain powder with the pH value of 8.2;
(4) dealcoholizing: reducing the partial pressure of fatty alcohol by using hot air to remove most of volatile dodecanol from the milled material, and recovering 2.2g of alcohol by using a de-fatting and recovering system;
(5) mixing and homogenizing: after the lauryl sodium sulfate subjected to dealcoholization is subjected to powder homogenization, 154g of powder is subjected to pH value detection of 8.2, and the powder is packaged qualified.
The above description is directed to specific embodiments of the present invention, but the present invention is not limited to the above description. Any equivalent modifications and alterations to this technical solution would be considered within the scope of this invention by those skilled in the art. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (5)
1. The utility model provides a preparation facilities of pharmaceutic adjuvant lauryl sodium sulfate which characterized in that: comprises a sulfonation reactor (5), a neutralizer (6), a homogenizing tank (7), a feeder (8), a quantitative feeder (9), a dryer (10), a cyclone filter (11), a milling system (13), a secondary dryer (14) and a powder homogenizer (15);
SO is arranged at the top of the sulfonation reactor (5)3A sulfonating agent feed port (1) and a dodecanol feed port (2), and an acid ester discharge port is arranged at the bottom of the sulfonating agent feed port and the dodecanol feed port; the discharge hole of the acid ester is connected with the feed hole of the neutralizer (6);
an alkali feeding hole (3) is formed in the neutralizer (6), and a liquid alkali neutralizer is introduced into the alkali feeding hole;
the outlet of the neutralizer (6) is connected with the inlet of a homogenizing tank (7), the bottom discharge port of the homogenizing tank is connected with a feeder (8), and the feeder (8) is connected with a dryer (10);
the outlet of the dryer (10), the discharge hole of the quantitative feeder (9) and the air purifier (12-1) are connected to the cyclone filter (11) through an air supply pipeline;
the upper end of the cyclone filter (11) is connected with a first induced draft fan (12), and the bottom of the cyclone filter is connected with a powder grinding system (13); the first induced draft fan (12) is connected with the waste gas treatment system (12-2);
the powder grinding system (13) is connected with a secondary dryer (14), and the secondary dryer (14) is respectively connected with a second induced draft fan (14-1) and a powder homogenizer (15); and the second induced draft fan (14-1) is connected with the fatty alcohol recovery system (14-2).
2. The device for preparing the pharmaceutical excipient sodium dodecyl sulfate according to claim 1, which is characterized in that: a densimeter (5-1) is arranged between the feed inlets of the sulfonation reactor and the neutralizer.
3. The device for preparing the pharmaceutical excipient sodium dodecyl sulfate according to claim 1, which is characterized in that: and a pH meter (6-1) is arranged on the neutralizer (6) to adjust the pH value of the neutralized slurry.
4. The device for preparing the pharmaceutical excipient sodium dodecyl sulfate according to claim 1, which is characterized in that: and a powder pH detector (15-1) is arranged on the powder homogenizer (15).
5. A preparation method of a pharmaceutic adjuvant sodium dodecyl sulfate is characterized by comprising the following steps:
(1) controlling the sulfonation reaction degree: dodecanol and SO3The sulfonation reaction generates lauryl sulfate with the conversion rate of 90-99 percent and the density of the corresponding acid ester of 0.95-1.01 g/cm3；
(2) And (3) neutralization high pH control: reacting sulfonated lauryl sulfate with liquid alkali to generate sodium dodecyl sulfate, and controlling the pH value to be 9.5-11.5;
(3) drying and adjusting the pH value of the powder: dehydrating and drying the neutralized materials, adding a solid organic acid regulator, and feeding the materials into a powder grinding system for grinding and homogenizing, wherein the pH value of the powder is 4.5-9.5;
(4) dealcoholizing: reducing the partial pressure of fatty alcohol by using hot air to remove most of volatile dodecanol from the milled material, and removing fat by using a fat recovery system, wherein the temperature of hot air is 65-145 ℃;
(5) mixing and homogenizing: homogenizing the sodium dodecyl sulfate subjected to dealcoholization treatment, detecting the pH value, and packaging after the sodium dodecyl sulfate is qualified.
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| CN202011485470.3A CN112500320A (en) | 2020-12-16 | 2020-12-16 | Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate |
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| CN202011485470.3A CN112500320A (en) | 2020-12-16 | 2020-12-16 | Preparation device and method of pharmaceutical adjuvant sodium dodecyl sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113028740A (en) * | 2021-04-29 | 2021-06-25 | 江苏优扬药业有限公司 | Low-temperature drying device and method for pharmaceutic adjuvant |
| CN113773236A (en) * | 2021-09-10 | 2021-12-10 | 上海奥威日化有限公司 | Precursor composition for preparing sodium alkyl sulfate dry product |
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