Potassium clavulanate organic solvent dehydration device

Abstract

The utility model discloses a potassium clavulanate organic solvent dehydration device. The device comprises a raw material tank, a raw material pump, a preheater, an evaporator, a superheater, a membrane separation unit, a condenser, a penetrating fluid tank and a penetrating fluid pump which are sequentially connected, the condenser is further connected with a vacuum unit, and a finished product outlet pipeline of the membrane separation unit is further connected with a heating medium inlet pipeline of the preheater. A heating medium outlet pipeline of the preheater is further connected with a finished product cooler, an outlet pipeline of the finished product cooler is connected with a finished product dehydration tank, and an outlet pipeline of the finished product dehydration tank is connected with a finished product pump. By adopting the device disclosed by the utility model, the moisture in the potassium clavulanate organic solvent can be effectively removed, the purity of the organic solvent is improved, and the potassium clavulanate organic solvent is favorably recycled.

Description

Technical Field

[0001] The utility model relates to the technical field of dehydration devices, and particularly relates to a dehydration device for clavulanate potassium organic solvents. Background Technique

[0002] Clavulanate potassium organic solvents refer to organic solvents used in the production process of clavulanate potassium, such as ethanol, isopropanol or their mixtures, etc. These organic solvents are used for extracting, separating and purifying clavulanate potassium to obtain high-quality products.

[0003] In the prior art, in order to reduce the waste of solvents during the production of clavulanate potassium and reduce costs, it is usually necessary to recycle the used organic solvents. However, affected by the production process and operating environment, water will be mixed into the organic solvents during the production of clavulanate potassium, which will reduce the purity of the organic solvents and affect the recycling effect. Therefore, a dehydration device for clavulanate potassium organic solvents is needed to meet the demand for recycling clavulanate potassium organic solvents. Content of the Utility Model

[0004] The purpose of the utility model is to provide a dehydration device for clavulanate potassium organic solvents to solve the problem that affected by the production process and operating environment, water will be mixed into the organic solvents during the production of clavulanate potassium, which will reduce the purity of the organic solvents and affect the recycling effect as mentioned in the above background technique.

[0005] To achieve the above purpose, the utility model provides the following technical solutions:

[0006] A dehydration device for clavulanate potassium organic solvents includes: a raw material tank, a raw material pump, a preheater, an evaporator, a superheater, a membrane separation unit, a condenser, a permeate tank and a permeate pump connected in sequence; wherein, a vacuum unit is also connected to the condenser; the finished product outlet pipeline of the membrane separation unit is connected to the heat medium inlet pipeline of the preheater, the heat medium outlet pipeline of the preheater is also connected with a finished product cooler, the outlet pipeline of the finished product cooler is connected with a finished product dehydration tank, and the outlet pipeline of the finished product dehydration tank is connected with a finished product pump.

[0007] Optionally, the membrane separation unit includes: a plurality of first membrane modules, a heat supplementer and a second membrane module; wherein, a plurality of first membrane modules are connected in series between the superheater and the heat supplementer, and the second membrane module is connected between the heat supplementer and the condenser.

[0008] Optionally, the finished product outlet is located on the membrane upstream side of the second membrane module; the steam outlet pipeline on the membrane downstream side of the first membrane module and the second membrane module is connected to the condenser.

[0009] Optionally, both the first membrane module and the second membrane module are made of sealing materials and are connected in series, with a total membrane area of 20 m 2 .

[0010] Optionally, the feed pump (2) is a magnetic vortex pump with a head of 60 m; the permeate pump (12) is a centrifugal negative pressure pump with a head of 18 m; and the product pump (6) is a magnetic pump with a head of 32 m. Further, the model of the feed pump is CQW40-60 magnetic vortex pump; the model of the product pump is BCQ40-25-160 magnetic pump.

[0011] Optionally, the evaporator, superheater, and makeup heater all adopt a shell-and-tube design, and the preheater and condenser both adopt a spiral-wound tube design.

[0012] In the potassium clavulanate organic solvent dehydration device provided by the present utility model, the raw materials in the raw material tank can be transported by the feed pump, so that the raw materials pass through the preheater, evaporator, and superheater in sequence. After reaching a certain temperature, they enter the membrane separation unit in the form of steam. The water and a small amount of solvent in the raw materials permeate from the upstream side of the membrane to the downstream side of the membrane through the membrane separation unit. The upstream side of the membrane of the last-stage second membrane module can obtain a finished product with a water content meeting the requirements. This finished product will be pre-cooled, cooled, and dehydrated through the preheater, finished product cooling device, and finished product dehydration tank. After cooling and dehydration, it enters the product pump for recovery. The downstream sides of the membranes of the first membrane module and the second membrane module adopt a condenser and a vacuum unit to form a vapor partial pressure difference between the upstream and downstream sides of the membrane by means of vacuum pumping and condensation. The permeate steam enters the condenser under the suction of the vacuum unit and condenses into a liquid. The condensed permeate enters the permeate tank for storage and is then discharged through the permeate pump, thus completing all the dehydration steps.

[0013] Compared with the prior art, the present utility model also has the following advantages:

[0014] 1) For the potassium clavulanate organic solvent raw materials, in this application, before being processed by the membrane separation unit, the raw materials are processed by the preheater, evaporator, and superheater in sequence, so that the raw materials enter the membrane separation unit in the form of steam. Among them, first, the raw materials are preheated to a certain temperature by the preheater. A higher temperature can reduce the viscosity of the solution, making it easier to pass through the subsequent dehydration equipment. After preliminary preheating, an evaporator is used to heat the preheated solution using the evaporation principle. By heating with the evaporator, the water in the raw materials is vaporized and removed, thereby increasing the concentration of the solution. After removing the water vapor by evaporation, the superheater is continued to heat, and the steam is further heated from the saturated temperature to a state higher than the saturated temperature (i.e., the superheat temperature) to form superheated steam, which enters the membrane separation unit in the form of superheated steam. This superheated steam can provide more heat and make the solvent evaporate faster.

[0015] 2) Before the finished product separated by the membrane separation unit enters the finished product dehydration tank, it is cooled by a finished product cooling device. By cooling the finished product, unnecessary chemical reactions or physical changes of the potassium clavulanate finished product at high temperatures are prevented, thereby maintaining its chemical stability and purity.

[0016] 3) The finished product separated by the membrane separation unit is connected to the finished product cooling device (instead of directly connected to the product cooling device) after passing through the preheater. By introducing the finished product from the heat medium inlet into the preheater, while serving as the heat medium to preheat the raw material in the preheater, the temperature of the finished product is initially reduced. After the initial temperature reduction, the finished product then enters the finished product cooling device for cooling, thereby saving heat sources and reducing energy consumption. Description of the Drawings

[0017] Figure 1 It is a schematic structural diagram of a potassium clavulanate organic solvent dehydration device proposed by the present utility model.

[0018] In the figure: 1, raw material tank; 2, raw material pump; 3, preheater; 4, finished product cooler; 5, finished product dehydration tank; 6, finished product pump; 7, evaporator; 8, superheater; 9, membrane separation unit; 91, first membrane module; 92, supplementary heater; 93, second membrane module; 10, condenser; 11, permeate tank; 12, permeate pump; 13, vacuum unit. Detailed Embodiment

[0019] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present utility model.

[0020] Please refer to Figure 1 , a potassium clavulanate organic solvent dehydration device provided in an embodiment of the present utility model includes a raw material tank 1, which stores potassium clavulanate organic solvent; the raw material tank 1 is connected to a raw material pump 2, the raw material pump 2 is connected to a preheater 3, the heat medium outlet and the refrigerant outlet of the preheater 3 are respectively connected to a finished product cooler 4 and an evaporator 7, the outlet of the finished product cooler 4 is connected to a finished product dehydration tank 5, a finished product pump 6 is connected to the finished product dehydration tank 5, the evaporator 7 is connected to a superheater 8, and the superheater 8 is connected to a membrane separation unit 9. In addition, the membrane separation unit 9 is also connected to the preheater 3 so that the finished product enters the finished product cooler after passing through the preheater; the membrane separation unit 9 is also connected to a condenser 10, the condenser 10 is connected to a permeate tank 11 and a vacuum unit 13, and a permeate pump 12 is connected to the permeate tank 11.

[0021] In addition, refer to Figure 1As shown in the figure, the membrane separation unit 9 includes a heat supplementer 92, a second membrane module 93, and a plurality of first membrane modules 91 connected in series. The plurality of first membrane modules 91 are connected between the superheater 8 and the heat supplementer 92, and the second membrane module 93 is connected between the condenser 10 and the heat supplementer 92.

[0022] The potassium clavulanate organic solvent raw material in the raw material tank 1 sequentially enters the preheater 3, the evaporator 7, and the superheater 8 through the raw material pump 2. First, it is preheated by the preheater 3 to reduce the viscosity of the raw material, then evaporated by the evaporator 7 to increase the solution concentration, and finally heated by the superheater 8 to form superheated steam, so that the raw material enters the membrane separation unit 9 in the form of steam after reaching a certain temperature for membrane separation.

[0023] The membrane separation unit 9 is composed of a plurality of first membrane modules 91 and a second membrane module 93 connected in series. The heat supplementer 92 located between the first membrane module 91 and the second membrane module 93 can make the temperature of the material uniform and stable when passing through the membrane separation unit 9, effectively improving the membrane dehydration efficiency and system stability.

[0024] The water and a small amount of solvent in the raw material treated by the preheater, evaporator, and superheater permeate from the upstream side of the membrane to the downstream side of the membrane through the membrane separation unit 9.

[0025] Among them, the finished product with the required water content is obtained on the upstream side of the membrane of the last-stage second membrane module 93. This finished product enters the finished product cooler 4 through the preheater 3 for cooling, preventing unnecessary chemical reactions or physical changes of the potassium clavulanate finished product at high temperatures, thereby maintaining its chemical stability and purity. Finally, it enters the finished product pump 6 for recovery after dehydration by the finished product dehydration tank 5. Further, the finished product dehydration tank 5 is a vacuum dehydration tank. By reducing the pressure in the tank, the water on the surface of the object is vaporized into water vapor, and then the air and water vapor in the tank are pumped out to form a vacuum state, so as to dehydrate quickly.

[0026] On the downstream side of the membrane, the vacuum unit 13 and the condenser 10 are used to form a vapor partial pressure difference between the upstream and downstream sides of the membrane by means of vacuum pumping and condensation. The permeate vapor enters the condenser 10 under the suction of the vacuum unit 13 for condensation, and the condensed permeate will enter the permeate tank 11 for storage and finally be discharged through the permeate pump 12.

[0027] In addition, further, the evaporator 7, the superheater 8, and the heat supplementer 92 can all adopt a shell-and-tube structure design, and the preheater 3 and the condenser 10 can both adopt a spiral wound tube structure design. The shell-and-tube evaporator 7 is more conducive to the vaporization of water in the solution in each tube. The shell-and-tube superheater 8 can heat the steam in each tube into superheated steam. The shell-and-tube heat supplementer 92 is more conducive to the uniform and stable temperature of the membrane separation material. The spiral wound tube preheater 3 can more effectively reduce the solution viscosity. The spiral wound tube condenser 10 is more conducive to improving the condensation effect.

[0028] In addition, the raw material pump 2 can adopt a magnetic vortex pump, the finished product pump 6 can adopt a magnetic pump, and the osmotic pressure pump 12 can adopt a centrifugal negative pressure pump to improve the pumping effect of the materials in each place. In order to enable the relevant instruments and components to further improve the dehydration effect while meeting the requirements of dehydration use. For example, both the first membrane module 91 and the second membrane module 93 adopt JTMZ20 sealing material (purchased from Jiangsu Jiutian High-Tech Co., Ltd.), and are connected in series, with a total membrane area of 20 m 2 . The model of the raw material pump 2 is CQW40-60 magnetic vortex pump, with a head of 60 m. The permeate pump 12 is a centrifugal negative pressure pump, with a head of 18 m. The finished product pump 6 is a BCQ40-25-160 magnetic pump, with a head of 32 m.

[0029] The working principle is as follows:

[0030] The raw materials that meet the requirements for entering the membrane in the raw material tank 1 enter the preheater 3, the evaporator 7 and the superheater 8 in sequence through the raw material pump 2 for treatment. Among them, the main task of the preheater 3 is to preheat the raw materials entering the dehydration equipment to a certain temperature. A higher temperature can reduce the viscosity of the solution, and a low-viscosity solution is more likely to pass through the subsequent dehydration equipment. The evaporator 7 uses the evaporation principle to continue heating the preheated solution, so that the internal moisture is vaporized and removed, thereby increasing the solution concentration. The steam after removing water vapor by the evaporator 7 enters the superheater 8 for heating. The superheater 8 can heat the steam from the saturated temperature to a state higher than its saturated temperature, that is, heat it to the superheated temperature to form superheated steam. This superheated steam can provide more heat during the subsequent dehydration process, enabling the solvent to evaporate faster.

[0031] After the solution raw materials reach a certain temperature, they enter the membrane separation unit 9 in the form of steam. The membrane separation unit 9 is composed of a plurality of first membrane modules 91 and second membrane modules 93 connected in series. A reheater 92 is connected between the first membrane module 91 and the second membrane module 93. Through the reheater 92, the temperature of the materials can be made uniform and stable when passing through the membrane separation unit 9, effectively improving the membrane dehydration efficiency and system stability.

[0032] The water and a small amount of solvent in the raw materials permeate from the upstream side of the membrane to the downstream side of the membrane through the membrane separation unit 9. Among them, the potassium clavulanate solution with a water content meeting the requirements is obtained on the upstream side of the last-stage second membrane module 93. The potassium clavulanate solution can directly pass through the preheater 3 for heat exchange and then enter the finished product cooler 4 for cooling. By cooling the potassium clavulanate solution, unnecessary chemical reactions or physical changes of the potassium clavulanate solution (this finished product is the potassium clavulanate organic solvent) at high temperatures can be prevented, so as to maintain its chemical stability and purity. Finally, it is dehydrated by the finished product dehydration tank 5 and then enters the finished product pump 6, and is pumped out and recycled through the finished product pump 6.

[0033] On the downstream side of the membrane of the membrane separation unit 9, a vacuum unit 13 is used in combination with a condenser 10 to create a vapor partial pressure difference between the upstream and downstream sides of the membrane. By reducing the vapor pressure on the downstream side of the membrane, the vapor partial pressure difference across the membrane is increased, enabling the permeate to be more effectively transferred from the upstream side to the downstream side. The permeate vapor is drawn into the condenser 10 by the vacuum unit 13 for condensation to convert the vapor into a liquid. The condensed permeate enters the permeate tank 11 for storage and is finally discharged through the permeate pump 12.

[0034] In addition, in this embodiment, the raw material meeting the requirements for entering the membrane refers to: isopropanol feedstock with a water content of ≤5 - 7 wt.%, a pH value range of 6.5 - 9, a conductivity <5 μS / cm, a chloride ion content of ≤20 ppm, and after evaporation, the raw material has no residue, no color change, and does not contain pigments, salts, sugars, solid particles, colloids, acidic, basic components, or other substances that may contaminate the equipment and membrane materials. The various indicators of the raw material should be maintained normal and stable in the long term.

[0035] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A dewatering device for potassium clavulanate in an organic solvent, characterized in that, Comprising: A raw material tank (1), a raw material pump (2), a preheater (3), an evaporator (7), a superheater (8), a membrane separation unit (9), a condenser (10), a permeate tank (11) and a permeate pump (12) connected in sequence; Wherein, a vacuum unit (13) is further connected to the condenser (10); The finished product outlet pipeline of the membrane separation unit (9) is connected to the heat medium inlet pipeline of the preheater (3), the heat medium outlet pipeline of the preheater (3) is further connected to a finished product cooler (4), the outlet pipeline of the finished product cooler (4) is connected to a finished product dehydration tank (5), and the outlet pipeline of the finished product dehydration tank (5) is connected to a finished product pump (6).

2. The dehydrating device for clavulanate potassium organic solvents according to claim 1, wherein, The membrane separation unit (9) includes: a plurality of first membrane modules (91), a heat replenisher (92) and a second membrane module (93); wherein, the plurality of first membrane modules (91) are connected in series between the superheater (8) and the heat replenisher (92), and the second membrane module (93) is connected between the heat replenisher (92) and the condenser (10).

3. The potassium clavulanate organic solvent dehydration device according to claim 2, characterized in that, The finished product outlet is located on the membrane upstream side of the second membrane module (93); the steam outlet pipeline on the membrane downstream side of the first membrane module (91) and the second membrane module (93) is connected to the condenser (10).

4. A clavulanic acid potassium organic solvent dehydration device according to claim 2, wherein, Both the first membrane module (91) and the second membrane module (93) use sealing materials and are connected in series with a total membrane area of 20 m 2 .

5. A clavulanic acid potassium organic solvent dehydration device according to claim 1, characterized in that, The raw material pump (2) is a magnetic vortex pump, model CQW40-60, with a head of 60m; the permeate pump (12) is a centrifugal negative pressure pump, with a head of 18m; the finished product pump (6) is a magnetic pump, model BCQ40-25-160, with a head of 32m.

6. A clavulanic acid potassium organic solvent dehydration device according to claim 2, characterized in that, The evaporator (7), the superheater (8) and the heat replenisher (92) all adopt a shell-and-tube design, and the preheater (3) and the condenser (10) both adopt a spiral wound tube design.

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