A purification process system and method for glycerol for injection

Abstract

The application discloses a kind of purification process systems and methods of glycerin for injection, system includes ion exchange unit, oxidation unit, water removal unit, decolorization unit, purification unit in turn fluid communication, ion exchange unit receives upstream industrial glycerol raw material, the glycerol product that the purification unit exports meets the standard for injection.Industrial glycerol is treated in ion exchange unit in turn, and the treatment of removing aldehydes and reducing substance is carried out in oxidation unit, water removal unit is handled in water removal unit, decolorization unit is handled in decolorization unit, and after the deep purification treatment of purification unit, industrial glycerol can be purified to glycerol product meeting each index requirement of glycerol (for injection) in Chinese Pharmacopoeia (2025 edition).

Description

Technical Field

[0001] This invention relates to the field of purification technology for injectable glycerin, and more particularly to a purification process system and method for injectable glycerin. Background Technology

[0002] Glycerin (chemical name: glycerol) is a viscous liquid with three hydroxyl groups, and it has extremely wide and crucial applications in the pharmaceutical field.

[0003] As a crucial pharmaceutical raw material, the quality of injectable glycerin directly impacts the safety and efficacy of drugs. In pharmaceutical preparations, glycerin primarily plays the following roles: First, as a solvent, its excellent solubility allows for the uniform dispersion of water-insoluble drug components, facilitating the preparation of solutions and injections, ensuring stable drug distribution, and laying the foundation for precise drug delivery and effective treatment. Second, as a suspending agent, it regulates the flexibility and viscosity of formulations, improving user comfort and promoting drug penetration, thus enhancing local therapeutic effects. Furthermore, glycerin-containing enemas can be used for bowel preparation, stimulating intestinal peristalsis and softening stool, providing a clean environment for procedures such as colonoscopy. Therefore, high-purity injectable glycerin is essential for ensuring the quality of pharmaceutical products and medical efficacy.

[0004] Currently, the main industrial production methods for glycerin include natural oil hydrolysis and chemical synthesis. Natural oil hydrolysis uses natural oils as raw materials, and the resulting product is commonly known as natural glycerin. Chemical synthesis uses propylene as a raw material, and the resulting product is commonly known as synthetic glycerin. However, both methods struggle to produce glycerin products that meet the purity requirements for injection.

[0005] Specifically, the glycerol water or soap-making waste liquid obtained by the hydrolysis of natural oils has a low glycerol content and contains a large number of impurities, including: organic substances such as alcohols and esters, which are similar in structure and properties to glycerol and are difficult to separate effectively by conventional methods; inorganic salt impurities, which may affect the physical properties of glycerol such as conductivity, thereby impairing its stability in injections; sugar impurities, which can provide nutrients for microbial growth and increase the risk of product contamination; and fatty acid and lipid impurities, which may affect the appearance and odor of the product and cause adverse reactions such as local irritation after injection.

[0006] Glycerol produced by chemical synthesis also has impurity problems. Catalysts, solvents and other substances used in the synthesis process may remain in the product. These impurities are often toxic or irritating, seriously threatening the safety of injectable glycerol.

[0007] In summary, neither existing natural oil hydrolysis nor chemical synthesis methods can efficiently obtain high-purity glycerol for injection. Therefore, developing a continuous, stable, efficient, energy-saving, and environmentally friendly glycerol purification process system for injection is of significant practical importance and urgency for improving glycerol product quality, meeting the needs of the pharmaceutical industry, and promoting the high-quality development of the pharmaceutical industry. Summary of the Invention

[0008] The technical problem to be solved by the present invention is to provide a purification process system and method for injectable glycerin, so as to reduce the content of various impurities in industrial glycerin, improve the quality of glycerin products, and meet the needs of the pharmaceutical industry.

[0009] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is as follows: A purification process system for injectable glycerin includes an ion exchange unit, an oxidation unit, a dehydration unit, a decolorization unit, and a purification unit that are sequentially fluidly connected. The ion exchange unit receives industrial glycerol raw material transported upstream, and the purification unit outputs glycerol product.

[0010] A further technical solution is that the ion exchange unit includes ion exchange column A and ion exchange column B arranged in series; The ion exchange column A is filled with cation exchange resin, and the ion exchange column B is filled with anion exchange resin.

[0011] A further technical solution is that the cation exchange resin is Na. + Type or H + Type; and / or The anion exchange resin is CO3²⁺. - Type or HCO3 - Type; and / or The stacking height of the cation exchange resins is 6 to 12 times the inner diameter of ion exchange column A; and / or The stacking height of the anion exchange resins is 6 to 12 times the inner diameter of ion exchange column B; and / or Industrial glycerin enters the ion exchange unit at a flow rate of 30-4000 L / h.

[0012] A further technical solution is that the oxidation unit includes: The reaction column has an input end at the top and an output end at the bottom, and the reaction column is filled with a first packing material to increase the gas-liquid contact area. The first column vessel has its input end connected to the output end of the reaction column and its output end connected to the input end of the dehydration unit; and An ozone generator is connected to the bottom of the reaction column and / or the first column bottom.

[0013] A further technical solution is that the theoretical number of plates in the design of the reaction column is 5-10; and / or Industrial glycerin is introduced into the oxidation unit at a flow rate of 30-1400 L / h; and / or The inner diameter of the reaction column is 10-50 cm; and / or The ozone generator produces an ozone flow rate of 0.5-1 L / min.

[0014] A further technical solution is that the water removal unit includes: The water removal tower column has an input end at the upper end and an output end at the lower end. The water removal tower column is filled with a second packing material for gas replenishment and dehydration. The second tower has its input end connected to the output end of the dewatering tower column and its output end connected to the input end of the decolorization unit. A nitrogen generator is connected to the bottom of the dehydration tower column and / or the second tower bottom; and The first heating device is used to regulate the temperature of the dewatering column and / or the second reboiler.

[0015] A further technical solution lies in, The heating temperature of the first heating device is 50-70℃; and / or The theoretical design number of the dewatering tower column is 10-30; and / or The inner diameter of the water removal tower column is 10-50cm; and / or The nitrogen generator produces nitrogen at a flow rate of 0.5-1 L / min; and / or Industrial glycerin enters the dehydration unit at a flow rate of 30-1400 L / h.

[0016] A further technical solution is that the decolorization unit includes: An adsorption column, which may be one or multiple columns arranged in series, has an input end at the upper end and an output end at the lower end, and is filled with a third packing material for decolorization treatment. Preferably, industrial glycerin enters the decolorization unit at a flow rate of 30-4000 L / h; and / or The inner diameter of the adsorption column is 10-50 cm; and / or The height of the third packing material stack is 4-15 times the inner diameter of the adsorption column; More preferably, the height of the third packing stack is 9-12 times the inner diameter of the adsorption column.

[0017] A further technical solution is that the purification unit includes: The third tower is connected to the output of the decolorization unit at its input end; The control switch is located on the pipeline between the third tower reactor and the decolorization unit; The second heating device is used to heat the third tower vessel; The second tower head cooler is connected to the third tower vessel; and A finished product storage tank is connected to the coolant output end of the second tower head cooler, and a vacuum pump is connected to the finished product storage tank. Preferably, industrial glycerol is introduced into the purification unit at a flow rate of 30-1400 L / h; and / or The vacuum pump has a pumping speed of 10-30 m / s. 3 / h.

[0018] A purification process for injectable glycerol, comprising using the purification process system described in any one of the above claims to sequentially perform ion exchange, oxidation, dehydration, decolorization and purification treatments on industrial glycerol raw materials to obtain a standard glycerol product for injection.

[0019] The beneficial effects of adopting the above technical solution are as follows: The purification process system for injectable glycerol connects various units in series via pipelines to form a continuous purification line, enabling continuous and stable processing of industrial glycerol and gradual removal of impurities. The industrial glycerol undergoes sequential purification via an ion exchange unit, an oxidation unit for aldehyde and reducing agent removal, a dehydration unit for dehydration, a decolorization unit for decolorization, and a purification unit for deep purification. This process purifies the industrial glycerol to meet the requirements of the Pharmacopoeia of the People's Republic of China (2025 edition) for glycerol (for injection), ultimately yielding high-purity injectable glycerol. Attached Figure Description

[0020] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0021] Figure 1 This is a schematic diagram of the purification process system for injectable glycerol in this invention.

[0022] In the attached diagram: 10 - Raw material storage tank; 11-Ion exchange column A, 12-Ion exchange column B; 21 - Reaction column, 22 - First column kettle, 23 - Ozone generator; 31-Water removal tower column, 32-Second tower kettle, 33-Nitrogen generator, 34-First water bath heater, 35-Circulating pump, 36-First tower head cooler, 37-First storage tank; 41 - Adsorption column; 42 - Second storage tank; 51-Third tower kettle, 52-Second water bath heater, 53-Second tower head cooler, 54-Control switch, 55-Finished product storage tank, 56-Vacuum pump; 1-Raw material supply pump, 2-First water pump, 3-Second water pump, 4-Third water pump, 5-Fourth water pump. Detailed Implementation

[0023] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art can make similar extensions without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0024] In the description of this invention, unless otherwise stated, the terms "upper," "lower," "left," "right," "inner," "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0025] like Figure 1 As shown, a purification process system for injectable glycerol includes an ion exchange unit, an oxidation unit, a dehydration unit, a decolorization unit, and a purification unit, which are sequentially fluidly connected. These units are connected in series via pipelines to form a continuous purification line, enabling continuous and stable processing of industrial glycerol, gradual removal of impurities, and ultimately obtaining high-purity injectable glycerol. The ion exchange unit, as the front-end processing unit of the entire purification system, has its inlet connected to an upstream industrial glycerol raw material storage device to receive the industrial glycerol raw material transported upstream. The purification unit, as the end-end processing unit of the entire purification system, has its outlet connected to a finished product collection device to output glycerol products that meet injectable standards.

[0026] Through the system, industrial glycerin is sequentially processed through an ion exchange unit for impurity removal, an oxidation unit for aldehyde and reducing substance removal, a dehydration unit for dehydration, a decolorization unit for decolorization, and a purification unit for deep purification. This process purifies the industrial glycerin to meet the requirements of the Pharmacopoeia of the People's Republic of China (2025 edition) for glycerin (for injection).

[0027] In the purification process system, a raw material supply unit can be set up at the front end of the ion exchange unit according to the process requirements. The raw material supply unit includes a raw material storage tank 10, which is connected to the input end of the ion exchange unit through a supply pipeline. A raw material supply pump 1 is provided on the supply pipeline.

[0028] The viscosity of industrial glycerin is determined by its moisture content; different moisture contents result in different viscosity. If it is necessary to reduce the viscosity of industrial glycerin during production, an appropriate amount of water (e.g., 10% water) can be added to the industrial glycerin at the front end of the ion exchange unit. This significantly reduces the viscosity, facilitating the transport, metering, and feeding of the industrial glycerin into subsequent purification processes, while also reducing equipment operating resistance and energy consumption. The purification process system disclosed in this invention includes a dehydration unit that effectively removes water from the industrial glycerin after the addition of water, ensuring the smooth progress of subsequent purification processes and meeting the final product quality standards.

[0029] The purification process system for injectable glycerol utilizes an ion exchange unit to remove inorganic and organic ionic impurities from industrial glycerol, aiming to reduce the content of fatty acids, lipids, chlorides, and chlorinated compounds in glycerol. The ion exchange unit includes ion exchange columns A11 and B12 connected in series. There can be one or more A11 columns, arranged sequentially in series when multiple A11 columns are used. Similarly, there can be one or more B12 columns, arranged sequentially in series when multiple B12 columns are used. The specific number of ion exchange columns can be flexibly selected based on the impurity content of the industrial glycerol raw material. When the impurity content in the industrial glycerol raw material is low, one A11 and one B12 ion exchange column can be used, which can meet the impurity removal requirements while reducing equipment investment and operating costs. When the impurity content in the industrial glycerol raw material is high, multiple ion exchange columns of the same type connected in series can further improve the impurity removal effect through multi-stage adsorption, preventing impurities from entering subsequent units and affecting the quality of the final product.

[0030] The ion exchange columns A11 and B12 in the ion exchange unit adopt a series structure to achieve the stepwise removal of cationic and anionic impurities, avoiding the problem of decreased resin adsorption capacity and poor impurity removal effect caused by the simultaneous adsorption of the two types of ions.

[0031] The ion exchange column A11 is filled with cation exchange resin, which adsorbs cationic impurities contained in industrial glycerin, including inorganic cations such as sodium, calcium, and magnesium ions, as well as a small amount of organic cationic impurities. If these cationic impurities remain in glycerin, they will affect the conductivity of glycerin, thereby affecting the stability of the injection, and may even react with drug components, reducing the efficacy of the drug. Through the adsorption of the ion exchange column A11, the above-mentioned cationic impurities can be completely removed.

[0032] Specifically, the cation exchange resin is Na + Type or H +Types of cation exchange resins are available, allowing for flexible selection based on the acidity or alkalinity of the industrial glycerol: when the industrial glycerol raw material is acidic, Na+ cation exchange resins are selected. + Type cation exchange resin, Na + Type H cation exchange resin exhibits stable adsorption capacity under acidic conditions, effectively adsorbing cationic impurities in industrial glycerol without altering the pH value of the glycerol, thus preventing further increases in glycerol acid value. When the industrial glycerol raw material is neutral or alkaline, H type H cation exchange resin is selected. + Type H cation exchange resin + Both types of cation exchange resins exhibit excellent adsorption performance under neutral and alkaline conditions. They not only adsorb cationic impurities but also slightly adjust the pH of glycerol, bringing it closer to neutral and creating suitable reaction conditions for subsequent oxidation processes. Both types of cation exchange resins can achieve highly efficient adsorption of cationic impurities, ensuring stable and reliable impurity removal.

[0033] The ion exchange column B12 is filled with anion exchange resin, which adsorbs anionic impurities in industrial glycerol, including inorganic anions such as chloride ions and carbonate ions, as well as a small amount of organic anionic impurities. These anionic impurities can cause the acid value of glycerol to increase, affecting the stability and safety of glycerol. Through the adsorption of the ion exchange column B12, the above-mentioned anionic impurities can be effectively removed, ensuring that the acid and base properties of glycerol after treatment by the ion exchange unit are stable and the impurity content is significantly reduced, providing qualified raw materials for subsequent oxidation, dehydration and other processes.

[0034] Specifically, the anion exchange resin is CO3²⁻. - Type or HCO3 - Two types of anion exchange resins can be flexibly selected based on the type of anionic impurities in industrial glycerol: when the industrial glycerol contains a high content of strongly acidic anions (such as chloride ions), CO3²⁺ is selected. - Type anion exchange resin, CO3² - Type II anion exchange resins have a stronger adsorption capacity for strongly acidic anions, which can be quickly adsorbed and removed while generating harmless carbonic acid without introducing new impurities. When industrial glycerol contains a high content of weakly acidic anions (such as acetate ions), HCO3- is selected. - Type anion exchange resin, HCO3 - The type of anion exchange resin exhibits higher adsorption selectivity for weakly acidic anions, enabling precise removal of these anions and ensuring thorough removal of anionic impurities. Both types of anion exchange resins achieve highly efficient adsorption of anionic impurities, ensuring stable and reliable impurity removal performance.

[0035] The ion exchange unit can effectively reduce the content of fatty acids, lipids, chlorides, and chloroforms in glycerol. Chlorides and chloroforms are removed by CO3²⁻.- Type or HCO3 - This type of anion exchange resin achieves removal; its essence is that protonated tertiary amine groups bind CO3²⁻. - or HCO3 - (Among them, the weak base resin has no free CO3²) - Active group, CO3² - As an exchangeable anion, its core adsorbs Cl through protonation-activated isocharged anion exchange. - This process removes chlorides and chlorinated compounds; fatty acids and lipids in Na... + Type or H + Under the action of a cation exchange resin, the fatty acid is converted into fatty acid, which then reacts with CO3²⁻. - Type or HCO3 - The anion exchange resin reacts to form fatty acid salts that are insoluble in glycerol. These fatty acid salts have a high boiling point and, after being processed by the subsequent purification unit, can be retained in the third column reactor 51, thereby achieving effective separation from glycerol and removing fatty acids and lipids.

[0036] The stacking height of the cation exchange resin is 6-12 times the inner diameter of the ion exchange column A. This ensures sufficient contact between the industrial glycerol and the cation exchange resin, thereby achieving full adsorption of cationic impurities, while also controlling flow resistance to achieve a balance between energy saving and impurity removal.

[0037] The stacking height of the anion exchange resin is 6-12 times the inner diameter of the ion exchange column B. Its design principle is the same as that of the cation exchange resin. If the stacking height is too low, the anion impurities cannot fully contact the resin, resulting in incomplete impurity removal. If the stacking height is too high, it will increase the flow resistance, increase energy consumption, and even lead to blockage.

[0038] Industrial glycerol enters the ion exchange unit at a flow rate of 30-4000 L / h. Controlling the flow rate of the industrial glycerol directly affects the impurity removal effect and production efficiency of the ion exchange. If the flow rate is too low, the production efficiency is low, failing to meet the needs of large-scale production, and may also lead to excessively rapid resin saturation, shortening the resin's lifespan. If the flow rate is too high, the contact time between the industrial glycerol and the resin is too short, impurities cannot be fully adsorbed, the impurity removal effect deteriorates, and the feed requirements of subsequent processes cannot be met. The specific flow rate can be flexibly adjusted according to the number of ion exchange columns and the resin packing volume, ensuring impurity removal while improving production efficiency to meet the needs of large-scale continuous production.

[0039] The purification process system for injectable glycerin utilizes an oxidation unit to remove reducing impurities and oxidizable nitrogenous impurities from industrial glycerin, aiming to reduce aldehydes and reducing substances in glycerin. The oxidation unit includes a reaction column 21, a first reboiler 22, and an ozone generator 23. The reaction column 21 and the first reboiler 22 can be made of one of the following materials: stainless steel, glass, quartz glass, or polytetrafluoroethylene.

[0040] The upper part of the reaction column 21 is the input end and the lower part is the output end. The reaction column 21 is filled with a first packing material to increase the gas-liquid contact area. The input end of the reaction column 21 is connected to the output end of the ion exchange unit through a first pipeline equipped with a first water pump 2. The first water pump 2 provides power for the delivery of industrial glycerin, ensuring that the glycerin treated by the ion exchange unit can enter the reaction column 21 stably and uniformly, avoiding flow rate fluctuations from affecting the oxidation reaction effect. A flow regulating valve can also be installed in the first pipeline to precisely control the flow rate of glycerin entering the reaction column 21 to adapt to different oxidation reaction requirements.

[0041] The first packing material can be selected from one or a combination of Raschig rings, Pall rings, θ rings, arc saddle rings, rectangular saddle rings, and stainless steel corrugated wire mesh. By filling with the first packing material, industrial glycerin can be dispersed into fine droplets, increasing the contact area between glycerin and ozone gas, prolonging the contact time, and allowing ozone to fully react with reducing impurities and oxidizable nitrogen-containing impurities in glycerin. This avoids incomplete oxidation caused by insufficient gas-liquid contact and improves the oxidation and impurity removal effect.

[0042] The first reactor vessel 22 is located at the bottom of the reaction column 21, with its input end connected to the output end of the reaction column 21 and its output end connected to the input end of the dewatering unit. The ozone generator 23 is connected to the bottom of the first reactor vessel 22 and / or the reaction column 21.

[0043] The function of the first reactor 22 is to collect the glycerol after the oxidation reaction and to buffer and store the glycerol to prevent the oxidized glycerol from directly entering the dehydration unit and causing flow fluctuations, thus ensuring the stable operation of the subsequent dehydration process. In addition, the first reactor 22 can also conduct a secondary contact reaction with the incompletely reacted ozone, so that the residual ozone can react further with the impurities in the glycerol, improve the thoroughness of oxidation and impurity removal, reduce ozone waste, and lower production costs.

[0044] Ozone generator 23 is used to generate high-concentration ozone. As a strong oxidant, ozone oxidizes aldehydes and reducing substances through two pathways: direct ozone molecular addition and hydrogen extraction, and indirect oxidation by hydroxyl radicals. This oxidizes them into substances insoluble in glycerol. These substances have high boiling points and, after being processed by the subsequent purification unit, can be retained in the third column reactor 51, thus achieving effective separation from glycerol and achieving the removal effect. At the same time, ozone decomposes into oxygen after the reaction and will not remain in glycerol, avoiding any impact on subsequent processes and the quality of the final product. When the ozone generator 23 is connected only to the bottom of the reaction column 21, ozone is introduced from the bottom of the reaction column 21 and comes into countercurrent contact with the glycerol flowing from top to bottom, achieving efficient oxidation. When the ozone generator 23 is connected only to the first column 22, ozone is introduced into the first column 22 and comes into full contact with the collected glycerol, completing secondary oxidation. When the ozone generator 23 is connected to both the bottom of the reaction column 21 and the first column 22, the synergistic effect of primary and secondary oxidation can be achieved, further improving the oxidation and impurity removal effect and ensuring the effective removal of reducing impurities and aldehydes.

[0045] In the purification process system, the reaction column 21 is designed with a theoretical number of 5-10 plates. This ensures sufficient reaction between ozone and impurities, guaranteeing effective impurity removal, while also controlling equipment costs and energy consumption, maximizing cost-effectiveness. The inner diameter of the reaction column 21 is 10-50 cm. The ozone generator 23 produces ozone at a flow rate of 0.5-1 L / min. Industrial glycerol enters the oxidation unit at a flow rate of 30-1400 L / h. The various technical parameters are mutually compatible, ensuring sufficient oxidation of impurities while avoiding ozone waste and side reactions, thus guaranteeing a stable and efficient oxidation reaction.

[0046] The purification process system for injectable glycerin utilizes a dehydration unit to remove moisture from industrial glycerin, achieving a moisture removal rate of over 95%, reducing the moisture content in the glycerin to below 0.5%, ensuring stable operation of subsequent processes. The dehydration unit includes a dehydration column 31, a second column 32, a nitrogen generator 33, a first heating device, and a condensation recovery device. These components work synergistically to achieve efficient moisture removal from the glycerin, while simultaneously enabling moisture recovery and reuse, thus achieving energy conservation and environmental protection.

[0047] The upper part of the dehydration tower column 31 is the input end, and the lower part is the output end. The dehydration tower column 31 is filled with a second packing material for gas replenishment and dehydration. The input end of the dehydration tower column 31 is connected to the output end of the oxidation unit through a second pipeline equipped with a second water pump 3. The second water pump 3 provides power for the delivery of oxidized glycerol, ensuring that the glycerol enters the dehydration tower column 31 stably. A flow regulating valve and a temperature sensor can be installed on the second pipeline to accurately control the flow rate of glycerol and the temperature when it enters the dehydration tower column 31, adapting to the dehydration process requirements.

[0048] The second packing material can be selected from one or a combination of Raschig rings, Pall rings, θ rings, arc saddle rings, rectangular saddle rings, and stainless steel corrugated wire mesh. By filling with the second packing material, glycerol can be dispersed into fine droplets, increasing the contact area between glycerol and nitrogen gas, and simultaneously increasing the evaporation surface area of ​​glycerol, thus promoting the evaporation of water in glycerol. In addition, the second packing material can also support and distribute the gas and liquid, ensuring that nitrogen and glycerol are evenly distributed within the dehydration column 31, avoiding insufficient evaporation of water in local areas, and improving the dehydration effect.

[0049] The second column 32 is located at the bottom of the dehydration column 31, with its input end connected to the output end of the dehydration column 31 and its output end connected to the input end of the decolorization unit. The second column 32 is used to collect the glycerol after dehydration treatment and to buffer and store the glycerol to prevent flow fluctuations caused by the dehydrated glycerol directly entering the decolorization unit. In addition, the second column 32 can also perform secondary separation of incompletely separated water to ensure that the water in the glycerol is completely removed. At the same time, it can keep the glycerol warm to prevent the water from re-condensing due to the decrease in glycerol temperature.

[0050] Nitrogen generator 33 is connected to the bottom of the second column 32 and / or the dehydration column 31. Nitrogen generator 33 produces high-purity nitrogen. As an inert gas, nitrogen does not react with glycerol and does not introduce new impurities. Nitrogen is introduced from the bottom of the dehydration column 31 or the second column 32, contacting the glycerol counter-currently. This removes evaporated moisture from the glycerol and reduces the partial pressure of water vapor within the dehydration column 31, promoting further evaporation of moisture and improving dehydration efficiency. Simultaneously, the introduction of nitrogen prevents oxidation of the glycerol during heating, avoiding the formation of new impurities and ensuring the quality of the glycerol. When nitrogen generator 33 is only connected to the bottom of the dehydration column 31, nitrogen contacts the downward-flowing glycerol counter-currently, efficiently removing moisture. When nitrogen generator 33 is only connected to the second column 32, nitrogen is introduced into the second column 32, removing residual moisture from the glycerol. When nitrogen generator 33 is connected to both, multi-stage dehydration can be achieved, further improving the dehydration effect.

[0051] The first heating device is used to regulate the temperature of the dehydration column 31 and / or the second reboiler 32. Heating increases the temperature of the glycerol, reduces the solubility of water in the glycerol, promotes water evaporation, and improves dehydration efficiency. The heating temperature of the first heating device is 50-70℃. Excessive heating temperature will cause the glycerol to discolor, while insufficient temperature will result in poor heating performance. The temperature regulation of the first heating device can be flexibly adjusted according to the moisture content and throughput of the glycerol, ensuring effective dehydration while avoiding excessive temperature that could lead to glycerol decomposition or oxidation.

[0052] The first heating device includes two configuration methods, which can be used individually or both simultaneously: The first heating method is a heating jacket, which surrounds the outer wall of the dehydration tower column 31, forming a heating cavity between the heating jacket and the outer wall of the dehydration tower column 31. A heating medium, such as hot water or heat transfer oil, circulates within the heating cavity. The heating medium is circulated by a circulation pump 35 to ensure a uniform and stable temperature of the dehydration tower column 31. The heating jacket allows for overall heating of the dehydration tower column 31, ensuring that the glycerol is at a suitable evaporation temperature throughout the entire column, promoting thorough evaporation of moisture. Preferably, the heating temperature of the heating jacket is 50-70℃. This temperature range ensures rapid evaporation of moisture while preventing excessively high temperatures from causing glycerol decomposition, oxidation, or side reactions that could affect the quality of the glycerol.

[0053] The second heating method is a first water bath heater 34, which is connected to the second reboiler 32 and used to heat the second reboiler 32. Specifically, the second reboiler 32 is placed inside the first water bath heater 34. Water bath heating is gentle and uniform, allowing for precise temperature control of the second reboiler 32 and preventing localized overheating that could lead to glycerol deterioration. Preferably, the heating temperature of the first water bath heater 34 is 50-70℃, consistent with the heating temperature of the heating jacket, ensuring that the glycerol is within a suitable temperature range in both the dehydration column 31 and the second reboiler 32, thus improving the stability of the dehydration effect.

[0054] A condensation recovery device is connected to the top of the dehydration tower column 31 to condense and recover the water discharged from the dehydration tower column 31. The condensation recovery device includes a first tower head cooler 36 connected to the top of the dehydration tower column 31 and a first storage tank 37 connected to the coolant output end of the first tower head cooler 36. When nitrogen gas containing moisture is discharged from the top of the dehydration tower column 31, it enters the condensation recovery device. Under the action of the cooling medium, the moisture in the nitrogen gas is condensed into liquid water, realizing the separation of moisture and nitrogen gas. The separated liquid water enters the first storage tank 37 for collection and recovery, and can be used for industrial production or domestic water use, realizing the recycling of water resources and achieving the purpose of energy conservation and environmental protection. The separated nitrogen gas can be dried and recycled, further reducing production costs.

[0055] The water removal tower column 31, the first tower head cooler 36, and the second tower bottom 32 in the system can be made of one of the following materials: stainless steel, glass, quartz glass, and polytetrafluoroethylene.

[0056] In the system, the theoretical number of trays in the dewatering tower column 31 is designed to be 10-30, which ensures sufficient water separation while controlling equipment costs and energy consumption, achieving a balance between dewatering efficiency and cost. The inner diameter of the dewatering tower column 31 is 10-50 cm. The nitrogen generator 33 produces nitrogen at a flow rate of 0.5-1 L / min. Industrial glycerol enters the dewatering unit at a flow rate of 30-1400 L / h. At this point, the nitrogen flow rate, glycerol flow rate, dewatering temperature, and dewatering tower column 31 are matched, achieving efficient water removal while avoiding nitrogen waste and raw material losses.

[0057] The purification process system for injectable glycerin utilizes a decolorization unit to remove pigments from industrial glycerin. The decolorization unit includes an adsorption column 41 and a second storage tank 42.

[0058] The number of adsorption columns 41 can be one or multiple columns arranged in series, which can be flexibly selected according to the content of pigment impurities in glycerol. The adsorption column 41 is filled with a third packing material for decolorization treatment. The upper end of the adsorption column 41 is the input end and the lower end is the output end. The input end of the adsorption column 41 is connected to the output end of the dehydration unit through a third pipeline equipped with a third water pump 4. The third water pump 4 provides power for the dehydrated glycerol to be transported, ensuring that the glycerol enters the adsorption column 41 stably and at a uniform speed. A flow regulating valve and a filter can also be installed on the third pipeline. The filter is used to remove any solid impurities that may be present in the glycerol, to prevent solid impurities from clogging the adsorption column 41 and affecting the adsorption effect and production continuity. The flow regulating valve is used to precisely control the flow rate of glycerol to adapt to the adsorption process requirements.

[0059] The input end of the second storage tank 42 is connected to the output end of the adsorption column 41 at the end, and the output end of the second storage tank 42 is connected to the input end of the purification unit. The function of the second storage tank 42 is to collect the glycerol after decolorization treatment and to buffer and store the glycerol to avoid flow fluctuations caused by the decolorized glycerol directly entering the purification unit, thus ensuring the stable operation of subsequent purification processes. In addition, the second storage tank 42 can also perform a settling treatment on the glycerol to allow a small amount of unadsorbed fine impurities to precipitate, further improving the purity of the glycerol.

[0060] The third filler is activated carbon that has been boiled and washed with pure water, dried, and then activated by heating. The specific operation steps are as follows: S1. Boiling and washing with pure water is used to remove ash, soluble impurities, and residual chemicals from activated carbon. Use ultrapure water with a resistivity ≥18.2 MΩ·cm (free from ions and organic contaminants). The ratio of activated carbon to pure water is controlled at 1:5~1:10 (g / mL) to ensure complete immersion of the activated carbon. Boil at 100℃ under normal pressure for 30~60 min / cycle, repeating 2~3 times. After each boiling, discard the supernatant and add fresh ultrapure water. The endpoint is determined by the conductivity ≤10 μS / cm or the pH stabilizing at 6.5~7.5 (neutral) after the last wash water cools to room temperature.

[0061] S2. Drying is used to remove free water from activated carbon and prevent boiling and bed disturbance during subsequent heating and activation. Gradient drying is carried out using a forced-air drying oven (atmospheric pressure, circulating air). The parameters can be selected as drying at 80℃ for 2 h, followed by drying at 105℃ for 4~6 h.

[0062] S3. Heating activation aims to rebuild and expand the pores of activated carbon, thereby restoring and enhancing its adsorption performance. The temperature is maintained at 400–500℃ for 1–2 h, while strictly controlling the air flow rate to <10 mL / (min·g).

[0063] Activated carbon has a huge specific surface area and extremely strong adsorption capacity, which can efficiently adsorb various pigment impurities and organic impurities in glycerol. Boiling and washing with pure water can remove dust, impurities and soluble harmful substances from activated carbon, preventing the introduction of new impurities. Drying can remove moisture from activated carbon and increase adsorption capacity. Heating activation can enhance the adsorption activity of activated carbon, extend its service life, and ensure stable decolorization effect.

[0064] Preferably, the inner cavity of the adsorption column 41 is provided with a sieve plate, and the third packing is stacked on the sieve plate. The function of the sieve plate is to support the third packing and prevent it from flowing out from the bottom of the adsorption column 41. At the same time, the sieve plate is provided with uniformly distributed through holes, the diameter of which is smaller than the particle size of the third packing, to ensure that glycerol passes through smoothly and to prevent the third packing from being lost. The sieve plate also serves to distribute the glycerol, so that the glycerol flows evenly through the third packing layer, ensuring that the third packing fully exerts its adsorption effect and avoiding the problem of incomplete decolorization caused by local adsorption saturation.

[0065] Preferably, the inlet section, outlet section, and intermediate section of the adsorption column 41 are all equipped with guide plates. Multiple vertically arranged guide plates are provided at the same height, and the guide plates are parallel to each other, with a spacing of 300-800mm between adjacent guide plates. The function of the guide plates is to guide the glycerol entering the adsorption column 41 to be evenly distributed, avoiding direct impact of glycerol on the third packing layer, which could cause the third packing layer to loosen or clump, affecting the adsorption effect. At the same time, the guide plates can slow down the flow rate of glycerol, prolong the contact time between glycerol and the third packing, and improve the adsorption effect.

[0066] In the system, industrial glycerin enters the decolorization unit at a flow rate of 30-4000 L / h. The inner diameter of the adsorption column 41 is 10-50 cm. The height of the third packing stack is 4-15 times the inner diameter of the adsorption column 41, and more preferably, the height of the third packing stack is 9-12 times the inner diameter of the adsorption column 41. This ensures decolorization effect while controlling flow resistance, extending the service life of activated carbon, and achieving a balance between decolorization effect and cost.

[0067] The purification system for injectable glycerin utilizes a purification unit to remove high-boiling-point impurities, pyrogens, and non-volatile impurities from industrial glycerin. This aims to reduce the levels of easily carbonizable substances, metallic impurities, sugars, microorganisms, and bacterial endotoxins in the industrial glycerin. Through the purification unit, deep removal of impurities is achieved, ultimately producing glycerin that meets injectable standards. The purification unit includes a third column reactor 51, a second heating device, a second column head cooler 53, and a finished product storage tank 55. These components work synergistically, using vacuum distillation to achieve deep removal of high-boiling-point impurities, pyrogens, and non-volatile impurities, ensuring that the glycerin purity meets injectable standards.

[0068] The input end of the third column reactor 51 is connected to the output end of the decolorization unit via a fourth pipeline equipped with a fourth water pump 5. The fourth water pump 5 provides power for the delivery of decolorized glycerol, ensuring a stable flow of glycerol into the third column reactor 51. A control switch 54 is installed on the pipeline between the third column reactor 51 and the decolorization unit (i.e., the fourth pipeline) to control the flow of glycerol into the third column reactor 51, isolating the purification unit from other units in the system when vacuuming is required. Closing the control switch 54 ensures a stable vacuum environment in the purification unit, while preventing vacuuming from affecting the normal operation of other units. A flow regulating valve and a temperature sensor can also be installed on the fourth pipeline to precisely control the flow rate of glycerol and its temperature upon entering the third column reactor 51, adapting to the requirements of the distillation purification process.

[0069] The second heating device is used to heat the third column reactor 51. The second heating device can be electric heating, heat transfer oil heating, etc., but preferably a second water bath heater 52. Through heating by the second heating device, the temperature of the glycerol in the third column reactor 51 is raised above its boiling point, achieving glycerol evaporation. High-boiling-point impurities, pyrogenic substances, and non-volatile impurities, whose boiling points are higher than glycerol, cannot evaporate and remain in the third column reactor 51, thus achieving separation of glycerol from impurities and achieving deep purification.

[0070] The second column head cooler 53 is connected to the third column reboiler 51, and the finished product storage tank 55 is connected to the coolant output end of the second column head cooler 53. A vacuum pump 56 is connected to the finished product storage tank 55. The finished product storage tank 55 can be made of stainless steel, glass, quartz glass, or polytetrafluoroethylene. The second column head cooler 53 condenses the glycerol vapor evaporated in the third column reboiler 51 into liquid glycerol, which is then transported to the finished product storage tank 55. When the vacuum pump 56 is turned on, it can create a vacuum in the third column reboiler 51, the second column head cooler 53, and the finished product storage tank 55, reducing the gas pressure in the system and thus lowering the boiling point of the glycerol. This allows the glycerol to evaporate at a lower temperature, preventing deterioration due to high temperatures. It also accelerates the evaporation rate of the glycerol and improves purification efficiency. Furthermore, the vacuum pump 56 can extract air from the system to prevent the glycerol from being oxidized during evaporation and condensation, ensuring the quality of the glycerol.

[0071] Preferably, industrial glycerol enters the purification unit at a flow rate of 30-1400 L / h. The vacuum pump 56 has a pumping speed of 10-30 m / s. 3 / h. This ensures that the gas pressure within the system remains stable within the preset range, enabling rapid low-temperature evaporation of glycerol, while also controlling energy consumption and raw material loss to ensure stable purification results.

[0072] The specific operational procedure for purifying industrial glycerin into injectable glycerin is as follows: A. Pretreatment preparation: According to the process requirements and actual production conditions, fill the ion exchange columns A11 and B12 in the ion exchange unit with suitable cation exchange resin and anion exchange resin respectively; select and determine the appropriate column diameter and theoretical plate number of the reaction column 21 and the water removal column 31, and fill them with suitable packing materials; select and determine the appropriate diameter and guide plate spacing of the adsorption column 41, and fill the adsorption column 41 with activated carbon that has been boiled and washed with pure water, dried and then heated and activated.

[0073] B. Ion exchange treatment: Industrial glycerin is placed in raw material storage tank 10. The pumping speed of raw material supply pump 1 is adjusted according to process requirements so that the industrial glycerin in raw material storage tank 10 enters the ion exchange column A11 and ion exchange column B12 of the ion exchange unit for ion exchange treatment.

[0074] C. Oxidation treatment: Turn on ozone generator 23 and adjust the ozone generation rate of ozone generator 23 according to process requirements; send the glycerol after ion exchange treatment into the reaction column 21 of the oxidation unit to make it fully contact with ozone, and then send the contacted glycerol into the first column 22 for oxidation reaction.

[0075] D. Dehydration treatment: Turn on the circulating pump 35, set the required heating temperature, and heat the heating jacket of the outer layer of the dehydration tower column 31 in the dehydration unit; turn on the nitrogen generator 33 and adjust the nitrogen generation rate according to process requirements; turn on the first water bath heater 34 and set the required temperature to heat the second tower 32 in a water bath; adjust the pumping speed of the second water pump 3 according to process requirements to pump the glycerol in the first tower 22 in the oxidation unit to the inlet of the dehydration tower column 31 in the dehydration unit, so that the glycerol completes the dehydration process in the dehydration tower column 31. The dehydrated glycerol is collected in the second tower 32, and the removed water is condensed by the first tower head cooler 36 and collected in the first storage tank 37.

[0076] E. Adsorption and decolorization treatment: Adjust the pumping speed of the third water pump 4 according to the process requirements to pump the glycerol in the second tower 32 to the inlet of the adsorption column 41 of the decolorization unit, so that the glycerol can be adsorbed in the adsorption column 41 and the adsorbed glycerol is collected in the second storage tank 42.

[0077] F. Vacuum distillation purification: Adjust the pumping speed of the fourth water pump 5 according to the process requirements to pump the glycerol in the second storage tank 42 into the third tower bottom 51, close the control switch 54 on the fourth pipeline, turn on the vacuum pump 56, turn on the second heating device and set the required temperature; after distillation, the glycerol in the tower bottom is condensed by the second tower head cooler 53, and the condensed glycerol product is collected in the finished product storage tank 55.

[0078] Through the continuous processing of steps B to F above, industrial glycerin can be purified into injectable glycerin that meets the standards.

[0079] The above-mentioned purification process system adopts continuous production line operation, with each process connected sequentially, enabling continuous and stable production of industrial glycerin. It boasts high production efficiency, and the entire process emits no harmful pollutants, exhibiting low energy consumption and excellent environmental performance. The system is adaptable to industrial glycerin from various sources, has a wide range of applications, and can improve glycerin product quality, meeting the needs of the pharmaceutical industry.

[0080] A purification process for injectable glycerol, comprising using the purification process system described in any one of the above claims to sequentially perform ion exchange, oxidation, dehydration, decolorization and purification treatments on industrial glycerol raw materials to obtain a standard glycerol product for injection.

[0081] The specific operating steps of the purification process for injectable glycerin are as follows: SI. Ion exchange, which uses ion exchange units to remove specific ionic impurities and some organic impurities from industrial glycerol, aims to reduce the content of fatty acids, lipids, chlorides and chlorinated compounds in glycerol.

[0082] Ion exchange units achieve purification through columns packed with specific functional resins. Cation exchange resins (H+)+ / Na + Type (CO3²) can convert fatty acid salts into free fatty acids; anion exchange resins (CO3²) can convert fatty acid salts into free fatty acids. - / HCO3 - (Type) adsorbs Cl through ion exchange. - It reacts with free fatty acids to form salts insoluble in glycerol. This treatment can specifically remove the aforementioned target impurities, solving the technical problem of these impurities affecting the stability and safety of glycerol, and providing qualified raw materials for subsequent oxidation, dehydration and other processes.

[0083] SII. Oxidation: This process utilizes an oxidation unit to remove reducing impurities from industrial glycerin, aiming to reduce aldehydes and reducing substances in glycerin.

[0084] Ozone and glycerol come into full contact within reaction column 21. As a strong oxidant, ozone reacts with aldehydes and reducing substances in glycerol, decomposing them into harmless small molecules such as carbon dioxide and water, without introducing new impurities. This oxidation treatment effectively removes aldehydes and reducing substances, solving the technical problem of these impurities affecting the stability and safety of glycerol, and further improving the purity of glycerol.

[0085] SIII. Dehydration: The dehydration unit removes moisture from industrial glycerin, achieving a moisture removal rate of over 95%.

[0086] Nitrogen gas comes into countercurrent contact with glycerol, and heating at the same time promotes the evaporation of water in glycerol. Nitrogen gas can carry away the evaporated water and reduce the partial pressure of water vapor in the tower, thus accelerating the evaporation rate. The second packing in the dehydration tower column 31 increases the gas-liquid contact area, ensuring that water evaporates fully and reducing the water content in glycerol to below 0.5%. This solves the technical problem of water affecting the effect of subsequent decolorization and purification processes, and ensures the stable operation of subsequent processes.

[0087] SIV. Decolorization: Removing pigments from industrial glycerin using a decolorization unit.

[0088] Industrial glycerin flows through the third packing material in the adsorption column 41 at a preset flow rate. The third packing material has a strong adsorption capacity and can efficiently adsorb pigment impurities in glycerin, while also adsorbing a small amount of residual organic impurities. After decolorization, the glycerin is colorless and transparent, which solves the technical problem of pigment impurities affecting the appearance and safety of glycerin and meets the appearance requirements for injection.

[0089] SV. Purification: The purification unit removes high-boiling-point impurities and non-volatile impurities from industrial glycerol. The purpose is to reduce the presence of easily carbonizable substances, metallic impurities, sugars, microorganisms, bacterial endotoxins, ammonium salts, sulfates, and high-boiling-point substances insoluble in glycerol generated in previous processes (ion exchange, oxidation units), thereby producing glycerol that meets injectable standards.

[0090] The decolorized glycerol is conveyed to the third column 51 of the purification unit. The second heating device is activated to heat the third column 51, and simultaneously, the vacuum pump 56 is activated to evacuate the system, reducing the system pressure and causing the glycerol to evaporate at a lower temperature. The vapor formed by the glycerol evaporation enters the second column head cooler 53, where it condenses into liquid glycerol under the action of the cooling medium and is then conveyed to the finished product storage tank 55 for storage. High-boiling-point impurities and non-volatile impurities have boiling points higher than glycerol and cannot evaporate. After purification, they remain in the third column 51 and can be cleaned periodically. Through purification, high-boiling-point impurities and non-volatile impurities in glycerol can be completely removed, and the final output glycerol product meets all the standards for injection.

[0091] The above-described steps for purifying industrial glycerin into injectable glycerin allow for a faster and more efficient process. Specific details will be provided below based on practical applications. However, it should be noted that the following embodiments are merely illustrative of the technical solutions of this invention and are not intended to limit it. Those skilled in the art should understand that modifications can still be made to the technical solutions described in the following embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to depart from the spirit and scope of the technical solutions of the embodiments of this invention.

[0092] Example 1 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions are as follows: A1. Pretreatment Preparation: Fill ion exchange columns A11 and B12 in the ion exchange unit with Na... + Type Ion Exchange Resin and CO3 2- Type Ion Exchange Resin. The reaction column 21 and the water removal column 31 are both selected with a column diameter (i.e., inner diameter) of 10 cm and 10 trays, and are both filled with Raschig rings as packing material. The adsorption column 41 has an inner diameter of 10 cm and a spacing of 300 mm between the guide plates. Activated carbon, which has been boiled, washed, dried, and then activated by heating, is filled into the adsorption column 41.

[0093] B1. Ion exchange treatment: Industrial glycerin is placed in raw material storage tank 10, and raw material supply pump 1 is turned on so that the industrial glycerin in raw material storage tank 10 enters ion exchange column A11 and ion exchange column B12 in the ion exchange unit for ion exchange treatment.

[0094] C1. Oxidation treatment: Turn on the ozone generator 23 and control the ozone generation rate to 0.5L / min. Send the glycerol that has been treated by the ion exchange unit into the reaction column 21 of the oxidation unit to make it fully contact with the ozone. The contacted glycerol is then sent into the first column 22 for oxidation reaction.

[0095] D1. Dehydration treatment: Turn on the circulating pump 35 and set the temperature to 50℃ to heat the heating jacket of the dehydration tower column 31 in the dehydration unit with a water bath; turn on the nitrogen generator 33 and control its nitrogen generation rate to 0.5L / min; turn on the first water bath heater 34 and set the temperature to 50℃ to heat the second tower bottom 32 with a water bath; turn on the second water pump 3 to pump the glycerol in the first tower bottom 22 into the inlet of the dehydration tower column 31, so that the glycerol undergoes the dehydration process in the dehydration tower column 31. After dehydration, the glycerol is collected in the second tower bottom 32, and the dehydrated water is condensed by the first tower head cooler 36 and collected in the first storage tank 37.

[0096] E1. Adsorption and decolorization treatment: Turn on the third water pump 4 to pump the glycerol in the second tower 32 to the inlet of the adsorption column 41 of the decolorization unit, so that the glycerol can complete the adsorption treatment in the adsorption column 41. The adsorbed glycerol is collected in the second storage tank 42.

[0097] F1. Vacuum distillation purification: Turn on the fourth water pump 5 to draw the glycerol in the second storage tank 42 into the third column bottom 51, turn off the control switch 54 on the fourth pipeline, turn on the vacuum pump 56 to reduce the pressure to 0.5kPa-1kPa, turn on the second heating device, and heat the temperature to 200℃-220℃. The glycerol in the third column bottom 51 enters through the second column head cooler 53 and is collected in the finished product storage tank 55.

[0098] Example 2 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the ion exchange columns A11 and B12 in the ion exchange unit are respectively filled with H₂O₂. + Type Ion Exchange Resin and HCO3 - Type Ion Exchange Resin.

[0099] Example 3 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the diameter of both the reaction column 21 and the dehydration column 31 is 50 cm and the number of trays is 10.

[0100] Example 4 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the inner diameter of the adsorption column 41 is 50 cm and the spacing between the guide plates is 800 mm.

[0101] Example 5 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Embodiment 1 in that the heating jacket and the first water bath heater 34 in the dehydration unit are set to a heating temperature of 70°C.

[0102] Example 6 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Embodiment 1 in that the ozone generator 23 in the oxidation unit generates ozone at a rate of 1 L / min.

[0103] Example 7 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the nitrogen generator 33 in the dehydration unit generates nitrogen at a rate of 1 L / min.

[0104] Comparative Example 1 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the industrial glycerin is not treated by an ion exchange unit.

[0105] Comparative Example 2 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the industrial glycerin is not treated by an oxidation unit.

[0106] Comparative Example 3 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that the industrial glycerin is not treated with a dehydration unit.

[0107] Comparative Example 4 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The difference between this purification process and the one in Example 1 is that the industrial glycerin is not treated with a decolorization unit.

[0108] Comparative Example 5 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The difference between this purification process and the one in Example 1 is that the industrial glycerin is not processed by a purification unit.

[0109] Comparative Example 6 This embodiment uses a purification process system for injectable glycerin to purify industrial glycerin. The purification process and conditions differ from those in Example 1 in that no packing material is added to the reaction column 21 in the oxidation unit and the dehydration column 31 in the dehydration unit.

[0110] The purified glycerol products from the above examples and comparative examples were tested using the following methods: Color: Glycerin (for injection) as per the Pharmacopoeia of the People's Republic of China (2025 edition); Chloride: General Chapter 0801 Chloride Test Method in the Pharmacopoeia of the People's Republic of China (2025 Edition); Sulfates: General Chapter 0802, Sulfate Test Method, Pharmacopoeia of the People's Republic of China (2025 Edition); Aldehydes and reducing substances: General Chapter 0401 Ultraviolet-Vis Spectrophotometry of the Pharmacopoeia of the People's Republic of China (2025 Edition); Sugar: Glycerin (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition); Fatty acids and lipids: General Chapter 0401 Ultraviolet-Vis Spectrophotometry of the Pharmacopoeia of the People's Republic of China (2025 Edition); Easily carbonizable substance: Glycerin (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition); Chlorinated compounds: Glycerin (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition); Moisture content: Method I, General Chapter 0832, Moisture Determination, Pharmacopoeia of the People's Republic of China (2025 Edition); Ammonium salts: Glycerin (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition); Iron salts: General Chapter 0807 of the Pharmacopoeia of the People's Republic of China (2025 Edition) Calcium salts: Glycerin (for injection) and iron salts test method (Pharmacopoeia of the People's Republic of China, 2025 edition); Heavy metals: General Chapter 0821, Method I, Heavy Metals Test, of the Pharmacopoeia of the People's Republic of China (2025 Edition); Microbial limits: General Chapter 1105 of the Pharmacopoeia of the People's Republic of China (2025 Edition): Microbial limit test for non-sterile products: microbial counting method; Bacterial endotoxins: General Chapter 1143, Detection Method for Bacterial Endotoxins, Pharmacopoeia of the People's Republic of China (2025 Edition).

[0111] The specific test results are shown in Tables 1 and 2.

[0112] Table 1:

[0113] Table 2:

[0114] As shown in Tables 1 and 2, the glycerol products obtained in Examples 1-7 meet the corresponding indicators for glycerol (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition); however, some items in Comparative Examples 1-6 do not meet the corresponding indicators for glycerol (for injection) in the Pharmacopoeia of the People's Republic of China (2025 edition).

[0115] Furthermore, a comparison of the glycerol products obtained in Example 1 and Comparative Example 1 revealed that industrial glycerol, which has not undergone ion exchange unit treatment, cannot easily remove chlorides, fatty acids and lipids, and chlorinated compounds, and their content is higher than the pharmacopoeia standard.

[0116] Furthermore, a comparison of the glycerol products obtained in Example 1 and Comparative Example 2 revealed that industrial glycerol, which had not undergone oxidation treatment, could not easily remove aldehydes and reducing substances, and its content was higher than the pharmacopoeia standard.

[0117] Furthermore, a comparison of the glycerin products obtained in Example 1 and Comparative Example 3 revealed that industrial glycerin, which had not undergone dehydration treatment, contained water that could not be easily removed and had a content higher than the pharmacopoeia standard.

[0118] Furthermore, a comparison of the glycerol products obtained in Example 1 and Comparative Example 4 revealed that industrial glycerol, which had not undergone a decolorization unit, had a color that could not be easily removed and exceeded pharmacopoeia standards.

[0119] Furthermore, a comparison of the glycerol products obtained in Example 1 and Comparative Example 5 revealed that industrial glycerol, which had not undergone purification, contained sugars, easily carbonizable substances, iron salts, calcium salts, heavy metals, microbial limits, bacterial endotoxins, sulfates, and ammonium salts that could not be easily removed, and their content was higher than the pharmacopoeia standard.

[0120] Furthermore, a comparison of the glycerol products obtained in Example 1 and Comparative Example 6 revealed that the reaction column 21 in the oxidation unit and the dehydration column 31 in the dehydration unit did not have any packing material added. The glycerol products obtained had lower contents of aldehydes, reducing substances, and water compared to Comparative Example 2 and Comparative Example 3, but still did not meet the pharmacopoeia standards.

[0121] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Anyone can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A purification process system for injectable glycerin, characterized in that, It includes an ion exchange unit, an oxidation unit, a dehydration unit, a decolorization unit, and a purification unit that are sequentially fluidized. The ion exchange unit receives industrial glycerol raw material transported upstream, and the purification unit outputs glycerol product.

2. The purification process system according to claim 1, characterized in that, The ion exchange unit includes ion exchange column A and ion exchange column B arranged in series. The ion exchange column A is filled with cation exchange resin, and the ion exchange column B is filled with anion exchange resin.

3. The purification process system according to claim 2, characterized in that, The cation exchange resin is Na. + Type or H + Type; and / or The anion exchange resin is CO3²⁺. - Type or HCO3 - Type; and / or The stacking height of the cation exchange resins is 6 to 12 times the inner diameter of ion exchange column A; and / or The stacking height of the anion exchange resins is 6 to 12 times the inner diameter of ion exchange column B; and / or Industrial glycerin enters the ion exchange unit at a flow rate of 30-4000 L / h.

4. The purification process system according to claim 1, characterized in that, The oxidation unit includes: The reaction column has an input end at the top and an output end at the bottom, and the reaction column is filled with a first packing material to increase the gas-liquid contact area. The first column vessel has its input end connected to the output end of the reaction column and its output end connected to the input end of the dehydration unit; and An ozone generator is connected to the bottom of the reaction column and / or the first column bottom.

5. The purification process system according to claim 4, characterized in that, The theoretical design number of the reaction column is 5-10; and / or Industrial glycerin is introduced into the oxidation unit at a flow rate of 30-1400 L / h; and / or The inner diameter of the reaction column is 10-50 cm; and / or The ozone generator produces an ozone flow rate of 0.5-1 L / min.

6. The purification process system according to claim 1, characterized in that, The water removal unit includes: The water removal tower column has an input end at the upper end and an output end at the lower end. The water removal tower column is filled with a second packing material for gas replenishment and dehydration. The second tower has its input end connected to the output end of the dewatering tower column and its output end connected to the input end of the decolorization unit. A nitrogen generator is connected to the bottom of the dehydration tower column and / or the second tower bottom; and The first heating device is used to regulate the temperature of the dewatering column and / or the second reboiler.

7. The purification process system according to claim 6, characterized in that, The heating temperature of the first heating device is 50-70℃; and / or The theoretical design number of the dewatering tower column is 10-30; and / or The inner diameter of the water removal tower column is 10-50cm; and / or The nitrogen generator produces nitrogen at a flow rate of 0.5-1 L / min; and / or Industrial glycerin enters the dehydration unit at a flow rate of 30-1400 L / h.

8. The purification process system according to claim 1, characterized in that, The decolorization unit includes: An adsorption column, which may be one or multiple columns arranged in series, has an input end at the upper end and an output end at the lower end, and is filled with a third packing material for decolorization treatment. Preferably, industrial glycerin enters the decolorization unit at a flow rate of 30-4000 L / h; and / or The inner diameter of the adsorption column is 10-50 cm; and / or The height of the third packing material stack is 4-15 times the inner diameter of the adsorption column, and more preferably, the height of the third packing material stack is 9-12 times the inner diameter of the adsorption column.

9. The purification process system according to claim 1, characterized in that, The purification unit includes: The third tower is connected to the output of the decolorization unit at its input end; The control switch is located on the pipeline between the third tower reactor and the decolorization unit; The second heating device is used to heat the third tower vessel; The second tower head cooler is connected to the third tower vessel; and A finished product storage tank is connected to the coolant output end of the second tower head cooler, and a vacuum pump is connected to the finished product storage tank. Preferably, industrial glycerol is introduced into the purification unit at a flow rate of 30-1400 L / h; and / or The vacuum pump has a pumping speed of 10-30 m / s. 3 / h.

10. A purification process for injectable glycerin, characterized in that, Using the purification process system described in any one of claims 1 to 9, industrial glycerol raw materials are sequentially subjected to ion exchange, oxidation, dehydration, decolorization, and purification treatments to obtain a standard glycerol product for injection.

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