CN109574047B - Method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid - Google Patents
Method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid Download PDFInfo
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- C07D265/04—1,3-Oxazines; Hydrogenated 1,3-oxazines
- C07D265/12—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems
- C07D265/14—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems condensed with one six-membered ring
- C07D265/18—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems condensed with one six-membered ring with hetero atoms directly attached in position 2
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid is characterized by comprising the following steps of: adding an extracting agent into the medical lithium-containing waste liquid, and collecting a water phase and an organic phase; heating and concentrating the water phase; adding an extracting agent for extracting and separating liquid, and collecting a water phase and an organic phase; adding resin, and collecting a water phase as a mother solution; adding alkali and Na into mother liquor2CO3Adjusting the pH value, and performing solid-liquid separation to obtain a clear solution; adjusting the pH of the clear liquid back by using hydrochloric acid, and boiling; adjusting the pH of the clear liquid to 6.0-8.0 by LiOH to obtain a purified liquid; evaporating and concentrating the purified solution to obtain a LiCl saturated solution, adding an organic solvent, and separating out crystals to obtain a LiCl crude product; dissolving the crude product with an organic solvent, carrying out solid-liquid separation, and carrying out spray drying to obtain a LiCl product; mixing the organic phases, evaporating to dryness, and separating various organic matters by thin-layer chromatography to obtain efavirenz. The invention realizes the recovery of high-purity lithium chloride and efavirenz by a multi-step impurity removal and recovery process, and the method is simple and feasible.
Description
Technical Field
The invention relates to recycling of lithium-containing waste liquid, in particular to a method for recycling high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid.
Background
Lithium, silver metal, the symbol of the element Li, atomic number 3, atomic weight 6.941. The density was 0.534 g/cm3, which is the lowest density metal. Melting point 180 ℃ and boiling point 1340 ℃. The color of the air is gradually changed into yellow or black. Reacts violently with water to generate lithium hydroxide and hydrogen, reacts rapidly with dilute hydrochloric acid and dilute sulfuric acid to release hydrogen, reacts slowly with cold sulfuric acid, and reacts violently with nitric acid. Does not react with oxygen at normal temperature, and reacts with nitrogen to generate a protective lithium nitride layer. When heated to over 100 deg.C, lithium oxide is formed, and when red hot, it can react with hydrogen. Can be directly combined with halogen and sulfur under certain conditions.
The lithium compound has the functions of tranquilizing, relieving pain, inducing diuresis, etc., and has been used in medicine for many years for treating psychosis, rheumatic arthritis, etc. In the process of producing lithium-containing medical intermediate, a large amount of lithium-containing waste liquid is generated. The prior art mainly comprises the following steps:
patent CN1072190C mainly provides a method for recovering lithium from waste liquid of lithium alkyl production. Hydrolyzing the waste liquid under the protection of nitrogen, adjusting the pH value with HCl, and then using Na2CO3Precipitating to obtain a lithium carbonate product, and centrifuging the mother solution to obtain lithium chloride. WO2017181759A1 mainly uses H2O2Oxidizing and removing the color of organic matters in the waste liquid, removing inorganic impurities, adding a sodium refining agent, and spray drying to obtain a lithium chloride product. Patent CN102815680A mainly relates to the addition of phosphoric acid to lithium-containing waste liquid to prepare lithium phosphate. Patent CN105129826B mainly relates to the recovery of lithium from waste liquid of medicine and synthetic plastics, and its main mode is evaporation concentration, roasting to obtain crude product, carbonization, impurity removal and thermal decomposition to obtain the product. The main process of patent CN1781847A is to adjust the alkali with hydrochloric acid, at the same time, add BaCl2 and oxalic acid into the alkali, filter, add hydrochloric acid to adjust the neutrality, and spray-dry to obtain LiCl product.
Most of the prior art does not relate to the removal of organic matters in the waste liquid, even if patents relating to the removal of the organic matters exist, the removal rate of the organic matters is not high, the liquid after impurity removal still has residual organic matters, the color of the solution is yellow, the color of the solution needs to be removed by using hydrogen peroxide, but the organic matters are not completely removed fundamentally, the process is longer, the recovery rate is low, and the quality of products is poor due to the introduction of other impurities; if the organic matters in the waste liquid are not completely removed, the quality of the product is seriously influenced, and the whiteness and the purity of the product are difficult to control.
On the other hand, the prior art does not relate to a method for recovering and extracting a certain medicine from the lithium-containing waste liquid of the medicine.
Disclosure of Invention
The invention provides a method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid, aiming at overcoming the defects of low recovery rate, secondary pollution, high recovery cost, complex process and incomplete removal of organic matters in the conventional process of recovering lithium from the medical lithium-containing waste liquid and filling the technical blank that the medical components are not collected from the waste liquid.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid sequentially comprises the following steps:
step (1), extraction and liquid separation: adding an extracting agent into the medical lithium-containing waste liquid, extracting at least once, and collecting a water phase and an organic phase;
and (2) evaporating and concentrating: heating and concentrating the water phase extracted in the step (1), and cooling until a near saturated state is achieved without salt precipitation;
and (3) extracting and separating liquid: adding the extracting agent into the concentrated aqueous phase obtained in the step (2) for extraction and liquid separation, extracting at least once, and collecting the aqueous phase and the organic phase;
step (4), adsorption: adding resin into the water phase obtained in the step (4), stirring, filtering, and collecting the water phase as mother liquor;
and (5) removing impurities: adding alkali and Na into the mother liquor obtained in the step (4)2CO3Adjusting the pH value to 6-12, and performing solid-liquid separation to obtain a clear liquid; adjusting the pH value of the clear liquid to 3-8 by using hydrochloric acid, and boiling; adjusting the pH of the boiled clear liquid to 6.0-8.0 by using lithium hydroxide to obtain purified liquid;
and (6) purifying by a solvent-out crystallization method: evaporating and concentrating the purified solution obtained in the step (5) until an LiCl saturated solution is obtained, adding a first organic solvent into the LiCl saturated solution, and crystallizing and separating out LiCl crystals to obtain a LiCl crude product;
and (7) dissolving, spray drying: dissolving the LiCl crude product obtained in the step (6) by using a second organic solvent, carrying out solid-liquid separation to obtain a solution, and carrying out spray drying on the solution to obtain high-purity industrial first-grade LiCl;
and (8) evaporating to dryness: and (3) mixing the organic phases obtained in the step (1) and the step (3), evaporating to dryness by using a rotary evaporator to obtain a brown viscous mixture, dissolving the brown viscous mixture in an extracting agent, separating various organic matters by adopting a thin layer chromatography, dissolving the various organic matters in absolute ethyl alcohol in a container, sealing, standing and volatilizing to obtain the efavirenz crystal.
The relevant content in the above technical solution is explained as follows:
1. in the scheme, the medical lithium-containing waste liquid contains lithium ions, sulfate ions, chloride ions, calcium ions, iron ions, magnesium ions, sodium ions, potassium ions and efavirenz.
2. In the above scheme, in the step (1), the volume ratio of the medical lithium-containing waste liquid to the extracting agent is 1: 10-10: 1.
3. In the above scheme, in the step (1), the step (3) and the step (8), all the extracting agents are ethyl acetate.
4. In the scheme, in the step (2), the heating concentration temperature is 80-120 ℃.
5. In the above scheme, in the step (4), the alkali is NaOH.
6. In the above scheme, in the step (6), the first organic solvent is any one or a mixture of several of ethanol, methanol, diethyl ether, ethylene glycol and tetrahydrofuran.
7. In the above scheme, in the step (7), the second organic solvent is any one of ethanol, methanol, ether and ethylene glycol.
8. In the scheme, the resin is macroporous ion exchange resin with any one of the trademarks of D231, DK251, 731 and 290.
The design concept of the invention is as follows: the method comprises a complete separation process, an impurity removal process and a recovery process of organic matters, and the industrial first-grade lithium chloride product and the efavirenz single crystal are obtained by extraction, concentration, re-extraction, resin exchange, impurity removal, evaporation, elution, absolute ethyl alcohol dissolution, spray drying and rotary evaporation to dryness. That is, the invention can fully recover and utilize medical lithium-containing waste liquid, can recover high-purity lithium chloride from a water phase, can also recover high-purity efavirenz from an organic phase, has simple recovery process, and can ensure that the content of impurities in the recovered product is very low on the basis. The method comprises the following specific steps:
the step (1) is to primarily remove organic matters in the waste liquid, and simultaneously, the efavirenz is kept in an organic phase.
Step (2) is a preparation for step (3) and the aqueous phase obtained in step (1) is concentrated by evaporation.
And (3) removing organic matters contained in the water phase for the second time, wherein the water phase contains lithium chloride, the organic phase contains efavirenz, and the organic phase is collected to the maximum extent for recycling the efavirenz.
And (4) purifying the water sample from which the organic matters are removed by resin, wherein most of metal cation impurities such as iron ions, calcium ions, magnesium ions, potassium ions and the like can be removed.
And (5) removing metal ions such as iron ions and calcium ions further for deep impurity removal.
And (6) crystallizing and precipitating LiCl crystals by utilizing a dissolution crystallization principle to obtain a LiCl crude product, wherein most impurities in the lithium chloride are removed.
The lithium chloride obtained in the step (7) has high quality, reaches the industrial first-grade standard, and has the purity of over 99 percent.
And (8) separating the efavirenz from various organic matters. Evaporating the organic phase obtained in the step (1) and the organic phase obtained in the step (3) by using a rotary evaporator to obtain a brown viscous mixture, separating various organic matters by adopting a thin layer chromatography, dissolving the various organic matters in absolute ethyl alcohol in a container, sealing, standing and volatilizing for a period of time to obtain the efavirenz crystal.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention has simple recovery process and simple operation, and can simultaneously recover industrial first-grade lithium chloride and efavirenz.
(2) The method can recover lithium from the medical waste liquid containing a large amount of organic matters, has high recovery rate which reaches over 96 percent, is thorough in separation, does not introduce other impurities, can control the whiteness and the purity of the lithium chloride product without adding hydrogen peroxide, and ensures that the recovered lithium chloride reaches the industrial first-level standard and has qualified whiteness and the purity of over 99 percent.
(3) The invention fully recycles the organic phase, extracts the efavirenz single crystal from the organic phase, does not add other precipitating agents, does not influence the product quality, and has high purity of the efavirenz.
In a word, the waste liquid generated in the pharmaceutical industry is taken as a raw material source, the recovery of lithium chloride and the recovery of efavirenz are realized through a multi-step impurity removal and recovery process, the purity of two products is very high, the effective treatment of the waste liquid is realized, the method is simple and feasible, the energy consumption is low, and no other precipitator is added.
Drawings
Figure 1 is a nuclear magnetic spectrum of efavirenz.
Detailed Description
The invention is further described below with reference to the following examples:
the raw materials of examples 1 to 3 are liquids such as intermediate waste liquid generated in the process of pharmaceutical production, and the main compositions thereof are shown in the following table:
example 1: method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid
Sequentially comprises the following steps:
and (1) pouring 500mL of wastewater into a 1L separating funnel by using a measuring cylinder, adding 100mL of ethyl acetate for extraction and separation, and extracting for three times respectively. 500mL of the aqueous phase and 260mL of the organic phase were collected.
And (2) evaporating and concentrating: and (3) putting 500mL of the extracted water sample into a 500mL beaker, heating to 100 ℃, concentrating to about 220mL, stopping heating, and cooling until the water sample reaches a near saturation state without separating out salt.
And (3) extracting and separating liquid: adding 40mL of ethyl acetate into the concentrated aqueous phase obtained in the step (2) for extraction and liquid separation, extracting for three times, and collecting the aqueous phase and the organic phase;
step (4), adsorption: adding 30g of resin into the water phase obtained in the step (4), stirring, reacting for 3 hours, filtering, and collecting the water phase as mother liquor;
and (5) removing impurities: adjusting the pH of the mother liquor obtained in the step (4) to 12 by using about 10 mol/L NaOH solution, and simultaneously adding Na2CO3Stirring for 30min, and performing solid-liquid separation; adjusting pH of the obtained clear solution to 2.0 with industrial HCl, and boiling for 30 min; regulating the pH of the boiled clear liquid to 7.0 by using a saturated LiOH solution to obtain a purified liquid;
and (6) purifying by a solvent-out crystallization method: evaporating and concentrating the purified solution obtained in the step (5) until an LiCl saturated solution is obtained, and then adding absolute ethyl alcohol into the LiCl saturated solution until LiCl crystals are crystallized and separated out to obtain a LiCl crude product;
and (7) dissolving, spray drying: adding absolute ethanol into the LiCl crude product obtained in the step (6) according to the proportion that 170 g LiCl is dissolved in 1L of absolute ethanol, stirring and dissolving for about 30min, carrying out solid-liquid separation to obtain an ethanol solution of LiCl, and directly carrying out spray drying to obtain an industrial first-grade lithium chloride product;
and (8) evaporating to dryness: and (3) mixing the organic phases obtained in the step (1) and the step (3), evaporating to dryness by using a rotary evaporator to obtain a brown viscous mixture, dissolving the brown viscous mixture in ethyl acetate, separating various organic matters by adopting a thin layer chromatography, dissolving the various organic matters in absolute ethyl alcohol in a container, sealing, standing and volatilizing for a period of time to obtain the efavirenz crystal.
The recovery rate of lithium was 97% and the purity was 99.2%. The HPLC purity of efavirenz was 99.8%. The resulting crystals were efavirenz as evidenced by the nuclear magnetic spectrum of figure 1.
Example 2: method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid
Sequentially comprises the following steps:
and (1) pouring 500mL of wastewater into a 10L separating funnel by using a measuring cylinder, adding 5000mL of ethyl acetate for extraction and separation, and extracting for three times respectively. 500mL of aqueous phase and 1300mL of organic phase were collected.
And (2) evaporating and concentrating: and (3) putting 500mL of the extracted water sample into a 500mL beaker, heating to 90 ℃, concentrating to about 220mL, stopping heating, and cooling until the water sample reaches a near saturation state without separating out salt.
And (3) extracting and separating liquid: adding 40mL of ethyl acetate into the concentrated aqueous phase obtained in the step (2) for extraction and liquid separation, extracting for three times, and collecting the aqueous phase and the organic phase;
step (4), adsorption: adding 30g of resin into the water phase obtained in the step (4), stirring, reacting for 3 hours, filtering, and collecting the water phase as mother liquor;
and (5) removing impurities: adjusting the pH of the mother liquor obtained in the step (4) to 12 by using about 10 mol/L NaOH solution, and simultaneously adding Na2CO3Stirring for 30min, and performing solid-liquid separation; adjusting pH of the obtained clear solution to 2.0 with industrial HCl, and boiling for 30 min; regulating the pH of the boiled clear liquid to 7.0 by using a saturated LiOH solution to obtain a purified liquid;
and (6) purifying by a solvent-out crystallization method: evaporating and concentrating the purified solution obtained in the step (5) until an LiCl saturated solution is obtained, and then adding ethylene glycol into the LiCl saturated solution until LiCl crystals are crystallized and separated out to obtain a LiCl crude product;
and (7) dissolving, spray drying: adding absolute ethanol into the LiCl crude product obtained in the step (6) according to the proportion that 170 g LiCl is dissolved in 1L of absolute ethanol, stirring and dissolving for about 30min, carrying out solid-liquid separation to obtain an ethanol solution of LiCl, and directly carrying out spray drying to obtain an industrial first-grade lithium chloride product;
and (8) evaporating to dryness: and (3) mixing the organic phases obtained in the step (1) and the step (3), evaporating to dryness by using a rotary evaporator to obtain a brown viscous mixture, dissolving the brown viscous mixture in ethyl acetate, separating various organic matters by adopting a thin layer chromatography, dissolving the various organic matters in absolute ethyl alcohol in a container, sealing, standing and volatilizing for a period of time to obtain the efavirenz crystal.
The recovery rate of lithium was 97.5% and the purity was 99.4%. The HPLC purity of efavirenz was 99.7%.
Example 3: method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid
Sequentially comprises the following steps:
and (1) pouring 500mL of wastewater into a 1L separating funnel by using a measuring cylinder, adding 50mL of ethyl acetate for extraction and separation, and extracting for three times respectively. 500mL of aqueous phase and 130mL of organic phase were collected.
And (2) evaporating and concentrating: and (3) putting 500mL of the extracted water sample into a 500mL beaker, heating the water sample to 110 ℃, concentrating the water sample to about 220mL, stopping heating, and cooling the water sample until the water sample reaches a near saturation state without separating out salt.
And (3) extracting and separating liquid: adding 40mL of ethyl acetate into the concentrated aqueous phase obtained in the step (2) for extraction and liquid separation, extracting for three times, and collecting the aqueous phase and the organic phase;
step (4), adsorption: adding 30g of resin into the water phase obtained in the step (4), stirring, reacting for 3 hours, filtering, and collecting the water phase as mother liquor;
and (5) removing impurities: adjusting the pH of the mother liquor obtained in the step (4) to 12 by using about 10 mol/L NaOH solution, adding Na2CO3, stirring for 30min, and carrying out solid-liquid separation; adjusting pH of the obtained clear solution to 2.0 with industrial HCl, and boiling for 30 min; regulating the pH of the boiled clear liquid to 7.0 by using a saturated LiOH solution to obtain a purified liquid;
and (6) purifying by a solvent-out crystallization method: evaporating and concentrating the purified solution obtained in the step (5) until an LiCl saturated solution is obtained, and then adding ether into the LiCl saturated solution until LiCl crystals are crystallized and separated out to obtain a LiCl crude product;
and (7) dissolving, spray drying: adding absolute ethanol into the LiCl crude product obtained in the step (6) according to the proportion that 170 g LiCl is dissolved in 1L of absolute ethanol, stirring and dissolving for about 30min, carrying out solid-liquid separation to obtain an ethanol solution of LiCl, and directly carrying out spray drying to obtain an industrial first-grade lithium chloride product;
and (8) evaporating to dryness: and (3) mixing the organic phases obtained in the step (1) and the step (3), evaporating to dryness by using a rotary evaporator to obtain a brown viscous mixture, dissolving the brown viscous mixture in ethyl acetate, separating various organic matters by adopting a thin layer chromatography, dissolving the various organic matters in absolute ethyl alcohol in a container, sealing, standing and volatilizing for a period of time to obtain the efavirenz crystal.
The recovery rate of lithium was 98% and the purity was 99.5%. The HPLC purity of efavirenz was 99.6%.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. A method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid is characterized by comprising the following steps: sequentially comprises the following steps:
step (1), extraction and liquid separation: adding an extracting agent into the medical lithium-containing waste liquid, and collecting a water phase and an organic phase; the medical lithium-containing waste liquid contains lithium ions, sulfate ions, chloride ions, calcium ions, iron ions, magnesium ions, sodium ions and efavirenz;
and (2) evaporating and concentrating: heating and concentrating the water phase extracted in the step (1), and cooling until a near saturated state is achieved without salt precipitation;
and (3) extracting and separating liquid: adding the extracting agent into the concentrated aqueous phase obtained in the step (2) for extraction and liquid separation, and collecting the aqueous phase and the organic phase;
step (4), adsorption: adding resin into the water phase obtained in the step (4), stirring, filtering, and collecting the water phase as mother liquor;
and (5) removing impurities: adding alkali and Na into the mother liquor obtained in the step (4)2CO3Adjusting the pH value to 6-12, and performing solid-liquid separation to obtain a clear liquid; adjusting the pH value of the clear liquid to 3-8 by using hydrochloric acid, and boiling; adjusting the pH of the boiled clear liquid to 6.0-8.0 by using lithium hydroxide to obtain purified liquid;
and (6) purifying by a solvent-out crystallization method: evaporating and concentrating the purified solution obtained in the step (5) until an LiCl saturated solution is obtained, adding a first organic solvent into the LiCl saturated solution to reduce the solubility of LiCl in the solution so as to rapidly crystallize and precipitate, and obtaining a LiCl crude product after LiCl crystals are crystallized and precipitated;
and (7) dissolving, spray drying: dissolving the LiCl crude product obtained in the step (6) by using a second organic solvent, carrying out solid-liquid separation to obtain a solution, and carrying out spray drying on the solution to obtain high-purity LiCl;
and (8) evaporating to dryness: mixing the organic phases obtained in the step (1) and the step (3), evaporating to obtain a brown viscous mixture, dissolving the brown viscous mixture in an extracting agent, separating various organic matters by adopting a thin layer chromatography, sealing, standing and volatilizing to obtain an efavirenz crystal;
in the step (1), the step (3) and the step (8), all the extracting agents are ethyl acetate.
2. The method for recovering high-purity efavirenz and lithium chloride from the lithium-containing medical waste liquid according to claim 1, characterized in that: in the step (1), the volume ratio of the medical lithium-containing waste liquid to the extracting agent is 1: 10-10: 1.
3. The method for recovering high-purity efavirenz and lithium chloride from the lithium-containing medical waste liquid according to claim 1, characterized in that: in the step (2), the heating concentration temperature is 80-120 ℃.
4. The method for recovering high-purity efavirenz and lithium chloride from the lithium-containing medical waste liquid according to claim 1, characterized in that: in the step (5), the base is NaOH.
5. The method for recovering high-purity efavirenz and lithium chloride from the lithium-containing medical waste liquid according to claim 1, characterized in that: in the step (6), the first organic solvent is any one or a mixture of ethanol, methanol, diethyl ether, ethylene glycol and tetrahydrofuran.
6. The method for recovering high-purity efavirenz and lithium chloride from the lithium-containing medical waste liquid according to claim 1, characterized in that: in the step (7), the second organic solvent is any one of ethanol, methanol, diethyl ether and ethylene glycol.
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