CN112521307A - Separation method of tetracycline hydrochloride - Google Patents
Separation method of tetracycline hydrochloride Download PDFInfo
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- CN112521307A CN112521307A CN202011501690.0A CN202011501690A CN112521307A CN 112521307 A CN112521307 A CN 112521307A CN 202011501690 A CN202011501690 A CN 202011501690A CN 112521307 A CN112521307 A CN 112521307A
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- tetracycline hydrochloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a separation method of tetracycline hydrochloride, which comprises the following process steps: slowly putting the tetracycline hydrochloride crystal liquid into a centrifuge which runs at a low speed, running at a high speed to spin-dry the material after discharging is finished, then adding acetone into the centrifuge to rinse the material, starting the centrifuge again to run at a high speed to spin-dry the material, putting the material into a material receiving vehicle, introducing clean air, and performing suction filtration. The separation and leaching process of the tetracycline hydrochloride crystal liquid is directly finished in the centrifugal machine, the whole process is closed, the volatilization of the organic solvent can be reduced, the production environment is effectively improved, the unit consumption of the solvent is greatly reduced, the production cost is reduced, and the physical and psychological health of personnel is guaranteed.
Description
Technical Field
The invention relates to an antibiotic refining technology, in particular to a separation method of tetracycline hydrochloride.
Background
The tetracycline hydrochloride is the hydrochloride of the tetracycline, has the same action and curative effect as the tetracycline, and is the first choice medicine for treating nonbacterial infections such as chlamydia infection, rickettsia disease, mycoplasma pneumonia, recurrent fever and the like; it can also be used for treating brucellosis, cholera, tularemia, rat bite, anthrax, tetanus, plague, actinomycosis, gas gangrene, and infection of respiratory system caused by sensitive bacteria, biliary tract infection, urinary tract infection, and skin soft tissue infection.
Chinese patent CN201510801097.0 provides a method for preparing tetracycline hydrochloride, wherein the separation of tetracycline hydrochloride crystal liquid is performed by vacuum filtration, when the temperature of the tetracycline hydrochloride crystal liquid is reduced to 22-30 ℃, the crystal liquid is placed into a filtration tank, vacuum filtration is opened, acetone is used for washing for many times, and finally air-pumping, drying and discharging are performed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the separation method of the tetracycline hydrochloride, which effectively improves the production environment, reduces the loss of the organic solvent, reduces the production cost, improves the working efficiency, reduces the labor intensity, shortens the working period and realizes the reduction of the number of workers and the improvement of the effect.
The technical scheme adopted for realizing the aim of the invention is as follows:
a separation method of tetracycline hydrochloride is characterized by comprising the following process steps: slowly putting the tetracycline hydrochloride crystal liquid into a centrifuge which runs at a low speed, running at a high speed to spin-dry the material after discharging is finished, then adding acetone into the centrifuge to rinse the material, starting the centrifuge again to run at a high speed to spin-dry the material, putting the material into a material receiving vehicle, introducing clean hot air, and performing suction filtration.
The high-speed rotation spin-drying time is controlled to be 10-90 min.
The dosage of the acetone is 0.075 to 0.15 times of the volume of the tetracycline hydrochloride crystal liquid.
And the acetone leaching time is controlled to be 10-15 min.
The temperature of the clean hot air is controlled to be 40-60 ℃.
And the suction filtration time is controlled to be 60-90 min.
The invention has the following technical advantages:
1. the separation and leaching process of the tetracycline hydrochloride crystal liquid is directly finished in the explosion-proof, corrosion-proof and closed centrifuge, and the whole process is closed, so that the safety coefficient is greatly improved, the volatilization of an organic solvent can be reduced, the production environment is improved, the unit consumption of the solvent is greatly reduced, the production cost is reduced, and the physical and psychological health of personnel is guaranteed.
2. The method adopts the centrifuge to separate the tetracycline hydrochloride crystal liquid, can ensure that the tetracycline hydrochloride and the organic solvent are separated more thoroughly because the centrifugal force generated by the high-speed rotation of the centrifuge is greater than vacuum, then adopts an acetone leaching mode to wash the materials, and adopts a method of introducing hot air and performing suction filtration to ensure that the solvent residue meets the standard requirement.
Drawings
FIG. 1 is a process flow diagram of the method for separating tetracycline hydrochloride of the present invention.
Detailed Description
The invention is illustrated below by way of examples, which are to be understood as being illustrative and not limiting. The scope and core content of the invention are to be determined by the claims.
The tetracycline hydrochloride crystal liquid in the following examples is obtained from the crystal liquid produced by the preparation method of tetracycline hydrochloride disclosed in the prior art, such as CN201510801097.0, CN201610413230.X, CN201210514795.9 and the like.
Example 1
And (3) taking 15L of tetracycline hydrochloride crystal liquid which is cooled to 25 ℃, slowly putting the tetracycline hydrochloride crystal liquid into a low-speed rotating centrifugal machine, rotating at a high speed for 15min after discharging, and spin-drying the butanol. And then slowly adding 1.12L of acetone into the centrifuge to carry out leaching on the material for 15min, and then rotating at a high speed for 60min to spin-dry the acetone. And (3) placing the wet tetracycline hydrochloride product obtained by leaching and spin-drying into a material receiving vehicle, introducing 50 ℃ clean air from the upper part of the material receiving vehicle, vacuumizing for 90min from the lower part, sampling and detecting 2420ppm of butanol residues and 57ppm of acetone residues, and pumping the material into a temporary storage tank.
Example 2
And (3) taking 20L of tetracycline hydrochloride crystal liquid, cooling to 24 ℃, slowly putting the tetracycline hydrochloride crystal liquid into a low-speed rotating centrifugal machine, rotating at a high speed for 25min after discharging, and spin-drying the butanol. And then slowly adding 2L of acetone into the centrifuge to carry out leaching on the material for 10min, and then rotating at a high speed for 70min to spin-dry the acetone. And (3) placing the wet tetracycline hydrochloride product obtained by leaching and spin-drying into a material receiving vehicle, introducing clean air at 55 ℃ from the upper part of the material receiving vehicle, vacuumizing for 90min from the lower part, sampling and detecting 2600ppm of residual butanol and 45ppm of residual acetone, and pumping the material into a temporary storage tank.
Example 3
And (3) cooling 25L of tetracycline hydrochloride crystal liquid to 25 ℃, slowly putting the tetracycline hydrochloride crystal liquid into a low-speed rotating centrifugal machine, rotating at a high speed for 20min after discharging, and spin-drying the butanol. Then 3.75L of acetone is slowly added into the centrifuge to carry out leaching on the material, the leaching time is 15min, then the material is rotated at a high speed for 90min, and the acetone is dried. And (3) placing the wet tetracycline hydrochloride product obtained by leaching and spin-drying into a material receiving vehicle, introducing clean air at 60 ℃ from the upper part of the material receiving vehicle, vacuumizing for 90min from the lower part, sampling and detecting 2230ppm of residual butanol and 69ppm of residual acetone, and pumping the material into a temporary storage tank.
Control group
And (3) taking 20L of tetracycline hydrochloride crystal liquid, cooling to 25 ℃, slowly putting into a suction filtration cylinder, discharging, and performing suction filtration for 60 min. Then adding 4L of acetone into the suction filtration cylinder for leaching the material twice, wherein the leaching time is 40min, and then carrying out suction filtration for 120 min. And sampling and detecting the tetracycline hydrochloride wet product subjected to suction filtration, wherein the butanol residue is 2496ppm, and the acetone residue is 70 ppm.
| Residual ppm of butanol | Acetone residual ppm | Unit consumption of acetone kg/kg | |
| Example 1 | 2420 | 57 | 0.1 |
| Example 2 | 2600 | 45 | 0.11 |
| Example 3 | 2230 | 69 | 0.1 |
| Sample controls | 2496 | 70 | 0.22 |
| Quality standard | ≤3000ppm | ≤100ppm | - |
Claims (6)
1. A separation method of tetracycline hydrochloride is characterized by comprising the following process steps: slowly putting the tetracycline hydrochloride crystal liquid into a centrifuge which runs at a low speed, running at a high speed to spin-dry the material after discharging is finished, then adding acetone into the centrifuge to rinse the material, starting the centrifuge again to run at a high speed to spin-dry the material, putting the material into a material receiving vehicle, introducing clean hot air, and performing suction filtration.
2. The method for separating tetracycline hydrochloride according to claim 1, wherein the spin-drying time in high-speed operation is controlled to 10 to 90 min.
3. A process for separating tetracycline hydrochloride according to claim 1, characterized in that the amount of acetone added is 0.075 to 0.15 times the volume of the tetracycline hydrochloride crystal.
4. The method for separating tetracycline hydrochloride according to claim 1 or 3, characterized in that the acetone elution time is controlled to 10 to 15 min.
5. The method for separating tetracycline hydrochloride according to claim 1, wherein the temperature of the clean hot air is controlled to 40 to 60 ℃.
6. The method for separating tetracycline hydrochloride according to claim 1, wherein the suction filtration time is controlled to 60-90 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011501690.0A CN112521307A (en) | 2020-12-17 | 2020-12-17 | Separation method of tetracycline hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011501690.0A CN112521307A (en) | 2020-12-17 | 2020-12-17 | Separation method of tetracycline hydrochloride |
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| CN112521307A true CN112521307A (en) | 2021-03-19 |
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| CN202011501690.0A Pending CN112521307A (en) | 2020-12-17 | 2020-12-17 | Separation method of tetracycline hydrochloride |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759584A (en) * | 2008-12-08 | 2010-06-30 | 河南新天地药业有限公司 | Technology for purifying DL-p-hydroxyphenylglycine |
| CN104513176A (en) * | 2015-01-08 | 2015-04-15 | 内蒙古格林特制药有限责任公司 | Preparation method for oxytetracycline hydrochloride |
| CN105294481A (en) * | 2015-11-19 | 2016-02-03 | 宁夏启元药业有限公司 | Preparation method of tetracycline hydrochloride |
| CN107954892A (en) * | 2017-12-22 | 2018-04-24 | 宁夏启元药业有限公司 | A kind of method of solvent residual amount in reduction quadracycline |
| CN110894521A (en) * | 2019-12-10 | 2020-03-20 | 金河生物科技股份有限公司 | Method for producing tetracycline |
| CN111302994A (en) * | 2020-04-14 | 2020-06-19 | 陶陈丁 | Novel preparation method of potassium thioacetate |
-
2020
- 2020-12-17 CN CN202011501690.0A patent/CN112521307A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759584A (en) * | 2008-12-08 | 2010-06-30 | 河南新天地药业有限公司 | Technology for purifying DL-p-hydroxyphenylglycine |
| CN104513176A (en) * | 2015-01-08 | 2015-04-15 | 内蒙古格林特制药有限责任公司 | Preparation method for oxytetracycline hydrochloride |
| CN105294481A (en) * | 2015-11-19 | 2016-02-03 | 宁夏启元药业有限公司 | Preparation method of tetracycline hydrochloride |
| CN107954892A (en) * | 2017-12-22 | 2018-04-24 | 宁夏启元药业有限公司 | A kind of method of solvent residual amount in reduction quadracycline |
| CN110894521A (en) * | 2019-12-10 | 2020-03-20 | 金河生物科技股份有限公司 | Method for producing tetracycline |
| CN111302994A (en) * | 2020-04-14 | 2020-06-19 | 陶陈丁 | Novel preparation method of potassium thioacetate |
Non-Patent Citations (1)
| Title |
|---|
| 罗茜: "《固液分离》", 31 March 1997, 冶金工业出版社 * |
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