阅读说明：本技术 真空冷冻干燥式固液分离的装置 (Vacuum freeze-drying type solid-liquid separation device ) 是由 王梅颖 王倩 林世东 王海兵 于 2019-04-04 设计创作，主要内容包括：本发明涉及一种真空冷冻干燥式固液分离的装置,主要解决现有技术中自动化程度低、安全性差、准确性差的问题。本发明通过采用一种真空冷冻干燥式固液分离的装置,所述装置包括至少一个分离区、冷阱、真空系统、蒸汽发生器,所述分离区包括冻干瓶、通道、收集瓶,通道用于连接冻干瓶和收集瓶,通道上设有与真空系统和蒸汽发生器相连的管线,接收瓶置于冷阱内,冻干瓶置于冷阱顶部上表面上,冷阱内盘绕冷凝管,分离区、冷阱、真空系统、蒸汽发生器及相关控制设备与控制软件工作站相连的技术方案较好地解决了上述问题,可用于检测行业中的固液分离中。(The invention relates to a vacuum freeze-drying type solid-liquid separation device, which mainly solves the problems of low automation degree, poor safety and poor accuracy in the prior art. The invention adopts a vacuum freeze-drying type solid-liquid separation device, which comprises at least one separation area, a cold trap, a vacuum system and a steam generator, wherein the separation area comprises a freeze-drying bottle, a channel and a collecting bottle, the channel is used for connecting the freeze-drying bottle and the collecting bottle, the channel is provided with a pipeline connected with the vacuum system and the steam generator, the receiving bottle is arranged in the cold trap, the freeze-drying bottle is arranged on the upper surface of the top of the cold trap, a condensing pipe is coiled in the cold trap, and the separation area, the cold trap, the vacuum system, the steam generator and related control equipment are connected with a control software workstation.)

1. The utility model provides a device of vacuum freeze-drying formula solid-liquid separation, the device includes at least one disengagement zone, cold-trap, vacuum system, steam generator, the disengagement zone includes freeze-drying bottle, passageway, receiving flask, and the passageway is used for connecting freeze-drying bottle and receiving flask, is equipped with the pipeline that links to each other with vacuum system and steam generator on the passageway, and in the cold-trap was arranged in to the receiving flask, on the cold-trap top upper surface was arranged in to the freeze-drying bottle, coiled the condenser pipe in the cold-trap, disengagement zone, cold-trap, vacuum system, steam generator and relevant controlgear link to each other with the control software workstation.

2. The vacuum freeze-drying solid-liquid separation device of claim 1, wherein the collection bottle is a ground borosilicate glass round-bottomed flask, the freeze-drying bottle is a ground borosilicate glass round-bottomed jar made of borosilicate glass, and the freeze-drying bottle is hung on a channel made of borosilicate glass and used for connecting the freeze-drying bottle with the receiving bottle; connecting one end of the freeze-drying bottle, wherein the channel has two 90-degree bends so that the freeze-drying bottle is connected in the forward direction instead of being placed upside down on the channel; the part of the channel exposed to the atmospheric environment is wrapped by rubber; electromagnetic control valves are arranged on pipelines connecting the channel with the vacuum system and the steam generator, and can be independently controlled to be opened and closed.

3. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the place where the cold trap is connected with the glass is sealed by a sealing ring, the cold trap and the condenser tube are made of 316L stainless steel, corrosion and deformation are prevented, electrolytic polishing treatment is carried out, the condenser tube is exposed in the cold trap, the cold trap pre-freezing function is realized, the cooling temperature can reach minus 105 ℃, and the sublimation of water and organic solvent is ensured; the cold trap can realize the function of rapid cooling, reaches preset temperature and equilibrium temperature within 2min, and the condenser pipe component is arranged in the U-shaped groove of four sides stamping forming.

4. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the cold trap is an embossed stainless steel outer surface, and the opening and closing of the cold trap door is designed to be automatically opened and closed and has a visible window. A powerful fan is arranged in the cold trap cabin, and the temperature rise and the temperature reduction within 2min are guaranteed to reach the set temperature.

5. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the vacuum system is composed of a vacuum pump, a vacuum sensor and a vacuum solenoid valve, the cold trap is connected with the vacuum pump through a pipeline which is resistant to both negative pressure and high pressure, the vacuum degree control range is 2-1000mbar, the display precision is 0.1mbar, the vacuum pump is a chemical membrane vacuum pump, an oil mist filter is configured, the vacuum solenoid valve is used for controlling the vacuum degree, and the vacuum pump is simultaneously provided with an adjusting knob, a key and a control display panel.

6. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the steam generator is used for automatic sanitary steam cleaning, and the steam generator is connected with the glass channel of the separation zone through a pipeline, so that the whole separation flow path can be cleaned.

7. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the cold trap box body is provided with a touch panel and a knob button, and parameters are rapidly changed through the knob button and are displayed on the control panel in real time.

8. The vacuum freeze-drying solid-liquid separation device according to claim 1, wherein the control software workstation can record data, display a flow chart and give a report, a database of common solid-liquid separation operation methods is stored in the workstation, so that a user can conveniently and directly call the database, the database is used as a method reference, the user can also store the common methods in a laboratory and add the common methods into the database, and the functions which can be realized by the software include adjusting the temperature of a cold trap program, changing the vacuum degree, displaying time, real-time temperature and real-time pressure, setting the steam burst volume and the burst time and unloading vacuum; a control software workstation is installed on the mobile equipment or a working computer for remote monitoring and monitoring the solid-liquid separation process at any time.

9. The vacuum freeze-drying solid-liquid separation device of claim 1, wherein the vacuum system pipeline is hermetically connected with the channel, and the collection bottle, the freeze-drying bottle, the waste liquid receiving bottle and the glass channel are connected in a snap-in type quick connector manner.

10. The vacuum freeze-drying solid-liquid separation apparatus according to claim 1, wherein the apparatus for performing solid-liquid separation comprises: (1) sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a prepared liquid nitrogen tank until the liquid is completely frozen into ice; (2) connecting the components of the device in sequence; (3) turning on a power switch of the instrument, setting a proper cold trap temperature for precooling, connecting the prefrozen freeze-drying bottle with the channel after reaching a preset temperature, and starting vacuumizing; (3) separating, editing the gradient temperature control of the cold trap and the gradient vacuum control of the vacuum system on a control interface or software according to the properties of the sample, and pausing the process at any time and changing improper conditions to optimize the separating conditions in the separating process; (4) after the separation operation is finished, stopping the vacuum system, removing the vacuum, recovering the atmospheric pressure state, taking out the collecting bottle and storing for subsequent detection; (5) and taking down the freeze-drying bottle, replacing two ends of the channel with waste liquid receiving bottles, and replacing a vacuum pump with a steam generator to clean the flow path so as to provide a pollution-free environment for next drying and separation.

Technical Field

The invention relates to a vacuum freeze-drying type solid-liquid separation device.

Background

In daily detection activities, one problem is encountered: the extract solution prepared according to the test standard is difficult to perform in this step of filtration and separation. The operation 1 is that the prepared leaching solution, a proper amount of sludge and a soil sample are mixed in an extraction bottle and are placed on an overturning oscillator for full oscillation. Then filtering the extractive solution with vacuum filter or positive pressure filter with 0.6-0.8 μm filter membrane. Operation 2 is that the extraction process takes place in a zero head space extractor (hereinafter referred to as ZHE), after shaking extraction, the filtrate is pressed out and collected under slow pressure.

The above operations are the contents of the standard HJ/T299-2007 sulfuric acid-nitric acid method for leaching toxicity of solid waste, the standard HJ/T300-2007 horizontal oscillation method for leaching toxicity of solid waste, and the standard HJ/T557-2010 horizontal oscillation method for leaching toxicity of solid waste.

First, the difficulty of operation 1 was analyzed: 1. the grain size of samples such as soil sludge and the like is far larger than 0.6-0.8 mu m, the filtering holes are blocked by solid in the filtering process, and the filtering operation cannot be carried out. 2. The strength of the filter membrane cannot resist excessive positive pressure or repeated pressure through decompression (namely vacuum pumping) and pressurization processes, so that the filter membrane is easy to break in the pressure change process, and the filtering operation fails. 3. By manually adjusting the pressure, there is a certain safety risk. 4. In the conventional pressure reduction and pressurization operation, the processed sample needs to be exposed to the atmospheric environment for a long time, and semi-volatile substances in the leaching solution and the extraction solution volatilize into the atmosphere, so that the detection value is smaller.

The difficulty of operation 2 was reanalyzed, similar to that of operation 1: 1. the air compressor has a high risk of pressurization operation. The laboratory inadvertently dropped a portion of the filter device after being blown up onto the ceiling in one pressurized operation, fortunately without any loss. 2. The particle size of the soil sludge is far larger than the aperture of a filter membrane for ZHE filtration, and a filtration channel is blocked.

Based on the above difficulties, researchers are actively adopting measures to solve the difficulties. The mixture is separated by using the existing instrument and separation technology and adopting a low-temperature centrifugation technology. This technique was also found to have an effect on the assay results. Analysis during the high-speed centrifugation process, substances dissolved in the extracting solution are re-precipitated into the soil sludge and are re-adsorbed by the soil sludge. The low temperature process, while effective in mitigating material volatilization, also reduces the solubility of certain materials. Another problem is that some very fine particles, which cannot be separated by centrifugation, remain suspended in the extraction solution. Therefore, the selection of a suitable technique for effective solid-liquid separation is highly considered.

Disclosure of Invention

The invention aims to solve the technical problems of low automation degree, poor safety and poor accuracy in the prior art, provides a novel vacuum freeze-drying type solid-liquid separation device, and has the advantages of high automation degree, good safety and good accuracy.

In order to solve the problems, the technical scheme adopted by the invention is as follows: the utility model provides a device of vacuum freeze-drying formula solid-liquid separation, the device includes at least one disengagement zone, cold-trap, vacuum system, steam generator, the disengagement zone includes freeze-drying bottle, passageway, receiving flask, and the passageway is used for connecting freeze-drying bottle and receiving flask, is equipped with the pipeline that links to each other with vacuum system and steam generator on the passageway, and in the cold-trap was arranged in to the receiving flask, on the cold-trap top upper surface was arranged in to the freeze-drying bottle, coiled the condenser pipe in the cold-trap, disengagement zone, cold-trap, vacuum system, steam generator and relevant controlgear link to each other with the control software workstation.

In the above technical scheme, preferably, the collection bottle is a ground borosilicate glass round-bottomed flask, the freeze-drying bottle is a ground borosilicate glass round-bottomed wide-mouth bottle and is made of borosilicate glass, the freeze-drying bottle is hung on a channel made of borosilicate glass, and the channel is used for connecting the freeze-drying bottle and the receiving bottle; connecting one end of the freeze-drying bottle, wherein the channel has two 90-degree bends so that the freeze-drying bottle is connected in the forward direction instead of being placed upside down on the channel; the part of the channel exposed to the atmospheric environment is wrapped by rubber; electromagnetic control valves are arranged on pipelines connecting the channel with the vacuum system and the steam generator, and can be independently controlled to be opened and closed.

In the technical scheme, preferably, the place where the cold trap is connected with the glass is sealed by a sealing ring, the cold trap and the condensing tube are made of 316L stainless steel, the cold trap and the condensing tube are subjected to corrosion and deformation resistance and electrolytic polishing treatment, the condensing tube is exposed in the cold trap and has the function of pre-freezing the cold trap, the cooling temperature can reach 105 ℃ below zero, and the sublimation of water and an organic solvent is ensured; the cold trap can realize the function of rapid cooling, reaches preset temperature and equilibrium temperature within 2min, and the condenser pipe component is arranged in the U-shaped groove of four sides stamping forming.

In the above technical solution, preferably, the cold trap adopts an embossed stainless steel outer surface, and the opening and closing of the cold trap door adopts an automatic switch design and has a visible window. A powerful fan is arranged in the cold trap cabin, and the temperature rise and the temperature reduction within 2min are guaranteed to reach the set temperature.

Among the above-mentioned technical scheme, preferably, vacuum system comprises vacuum pump, vacuum sensor, vacuum solenoid valve, and the cold trap passes through resistant negative pressure resistant high pressure resistant pipe connection again promptly with the vacuum pump, and vacuum control range is 2-1000mbar, and the display accuracy is 0.1mbar, and the vacuum pump is chemical diaphragm vacuum pump, disposes the oil mist filter, and vacuum solenoid valve is used for controlling the vacuum degree, has adjust knob, button and controls display panel simultaneously on the vacuum pump.

In the above technical solution, preferably, the steam generator is used for automatic sanitary steam cleaning, and the steam generator is connected with the glass channel of the separation region through a pipe, so that the whole separation flow path can be cleaned.

In the above technical scheme, preferably, the cold trap box body is provided with a touch panel and a knob key, parameters are rapidly changed through the knob key, and the parameters are displayed on the control panel in real time.

In the technical scheme, preferably, the control software workstation can record data, display a flow chart and issue a report, a database of common solid-liquid separation operation methods is stored in the workstation, a user can conveniently and directly call the database, the database is used as a method reference, the user can also save the common methods in a laboratory and add the common methods into the database, and the functions which can be realized by the software include adjusting the temperature of a cold trap program, changing the vacuum degree, displaying time, real-time temperature and real-time pressure, setting the steam burst amount and the burst time and unloading vacuum; a control software workstation is installed on the mobile equipment or a working computer for remote monitoring and monitoring the solid-liquid separation process at any time.

Among the above-mentioned technical scheme, preferably, vacuum system pipeline and passageway seal link to each other, and collection bottle, freeze-drying bottle, waste liquid receive and are connected with the form of buckle formula quick-witted bayonet joint between the glass passageway.

In the above technical solution, preferably, the solid-liquid separation includes the following steps: (1) sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a prepared liquid nitrogen tank until the liquid is completely frozen into ice; (2) connecting the components of the device in sequence; (3) turning on a power switch of the instrument, setting a proper cold trap temperature for precooling, connecting the prefrozen freeze-drying bottle with the channel after reaching a preset temperature, and starting vacuumizing; (3) separating, editing the gradient temperature control of the cold trap and the gradient vacuum control of the vacuum system on a control interface or software according to the properties of the sample, and pausing the process at any time and changing improper conditions to optimize the separating conditions in the separating process; (4) after the separation operation is finished, stopping the vacuum system, removing the vacuum, recovering the atmospheric pressure state, taking out the collecting bottle and storing for subsequent detection; (5) and taking down the freeze-drying bottle, replacing two ends of the channel with waste liquid receiving bottles, and replacing a vacuum pump with a steam generator to clean the flow path so as to provide a pollution-free environment for next drying and separation.

The invention relates to a method for carrying out solid-liquid separation on extraction processes in the detection industry by utilizing a vacuum freeze drying technology. The principle is that the liquid in the solid-liquid mixture is pre-frozen into a solid state, the liquid and the substances dissolved in the liquid are partially sublimated into steam in a vacuum state, and then the steam is condensed into the liquid to be collected. The technology can overcome the defects of positive pressure, reduced pressure filtration and centrifugal solid-liquid separation methods. In addition, the main instrument device related in the invention has high automation degree and high safety factor. The air tightness is good, the loss of collected materials is reduced, and a good technical effect is achieved.

Drawings

FIG. 1 is a schematic view of the internal structure of the apparatus of the present invention;

FIG. 2 is a schematic view of the external structure of the apparatus of the present invention;

in fig. 1 and 2, 1 freeze-drying bottle, 2 rotating buckle, 3 channels, 4 condenser tubes, 5 collecting bottles, 6 and 7 electromagnetic control valves, 8 steam generator, 9 vacuum pump, 10 pipelines, 11 cold trap door, 12 transparent visual glass window, 13 knob button, 14 computer and control software, 15 touch screen panel, 16 freeze-drying bottle base.

The present invention will be further illustrated by the following examples, but is not limited to these examples.

Detailed Description

[ example 1 ]

A vacuum freeze-drying type solid-liquid separation device (as shown in figures 1 and 2) comprises a separation area, a cold trap, a vacuum system and a steam generator, wherein the separation area comprises a freeze-drying bottle, a channel and a collecting bottle, the channel is used for connecting the freeze-drying bottle and the collecting bottle, a pipeline connected with the vacuum system and the steam generator is arranged on the channel, the receiving bottle is arranged in the cold trap, the freeze-drying bottle is arranged on the upper surface of the top of the cold trap, a condensing pipe is coiled in the cold trap, and the separation area, the cold trap, the vacuum system, the steam generator and related control equipment are connected with a control software workstation; when solid-liquid separation is carried out, the method comprises the following steps: (1) sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a prepared liquid nitrogen tank until the liquid is completely frozen into ice; (2) connecting the components of the device in sequence; (3) turning on a power switch of the instrument, setting a proper cold trap temperature for precooling, connecting the prefrozen freeze-drying bottle with the channel after reaching a preset temperature, and starting vacuumizing; (3) separating, editing the gradient temperature control of the cold trap and the gradient vacuum control of the vacuum system on a control interface or software according to the properties of the sample, and pausing the process at any time and changing improper conditions to optimize the separating conditions in the separating process; (4) after the separation operation is finished, stopping the vacuum system, removing the vacuum, recovering the atmospheric pressure state, taking out the collecting bottle and storing for subsequent detection; (5) and taking down the freeze-drying bottle, replacing two ends of the channel with waste liquid receiving bottles, and replacing a vacuum pump with a steam generator to clean the flow path so as to provide a pollution-free environment for next drying and separation.

Description of the vacuum freeze-drying liquid-solid separation method:

1. the separation zone consists of three parts: freeze-drying bottle, passageway, collecting flask. 3 freeze-drying bottles, ground round bottom wide-mouth bottles with the volume of 2L and borosilicate glass. The glass material can resist negative pressure.

2. The freeze-drying bottle is hung on the borosilicate glass channel, and the channel is used for connecting the freeze-drying bottle and the receiving bottle. The end of the vial is attached and the channel has two 90 degree bends so that the vial is attached in a forward orientation rather than being inverted over the channel. The part of the channel exposed to the atmospheric environment is covered with rubber. The channel is provided with a thin tube connected with the vacuum pump and the steam generator, and the thin tube can be used for two purposes, is connected with the vacuum pump and is also connected with the steam generator. To realize that one vacuum pump and one steam generator act on 3 parallel channels simultaneously. Electromagnetic control valves are respectively arranged at the three connected thin pipes and can be independently controlled to be opened and closed.

3. The ground borosilicate glass round-bottom flask corresponds to 3 collecting bottles and has the volume of 2L, and can resist negative pressure. The receiving bottle is placed in the cold trap.

4. The place where the cold trap is connected with the glass is sealed by a sealing ring. The cold trap volume is 8-10L. And a condensing pipe is coiled in the cold trap. The cold trap and the condensing pipe are made of 316L stainless steel, are corrosion-resistant and deformation-resistant, are subjected to electrolytic polishing treatment, are exposed in the cold trap and have the pre-freezing function of the cold trap. The cooling temperature can reach minus 105 ℃, and the sublimation of water and organic solvent can be ensured. The cold trap can realize the function of rapid cooling, reaches the preset temperature and balances the temperature within 2min, and improves the working efficiency. The condenser tube element is arranged in a U-shaped groove formed by punching on four sides, so that an excellent condensation effect is realized. The cold trap uses an embossed stainless steel outer surface. The cold trap door is opened and closed by adopting the design of an automatic switch and is provided with a visible window. And a powerful fan is arranged in the cold trap cabin, so that the temperature rise and the temperature drop are guaranteed to reach the set temperature within 2 min.

5. The vacuum system consists of a vacuum pump, a vacuum sensor and a vacuum electromagnetic valve. The cold trap is connected with the vacuum pump through a pipeline which is resistant to negative pressure and high pressure. The vacuum degree control range is 2-1000mbar, and the display precision is 0.1 mbar. The vacuum pump is a chemical diaphragm vacuum pump, an oil mist filter is required to be configured, and the vacuum pump is environment-friendly. The vacuum solenoid valve is used for controlling the vacuum degree and improving the drying rate. The vacuum pump is simultaneously provided with an adjusting knob, a key and an operation and control display panel.

6. The steam generator is used for automatic hygienic steam cleaning. The steam generator is connected with the glass channel of the separation area through a pipeline, and the whole separation flow path can be cleaned.

7. The touch screen control panel has clear layout. And editing parameter methods, such as cold trap temperature, vacuum degree and the like. Parameters are changed rapidly through the knob and the key and are displayed on the control panel in real time.

8. The control software workstation is convenient to operate, and can record data, display a flow chart and issue a report. And a database of common solid-liquid separation operation methods is stored in the workstation, so that a user can directly call the operation method conveniently. The database is used as method reference, so that the time for user method construction and method optimization is saved. The user can also save the method commonly used in own laboratory and add the method into the database. The functions realized by the software comprise adjusting the program temperature of the cold trap, changing the vacuum degree, the display time, the real-time temperature and the real-time pressure, setting the steam burst amount and the burst time, and unloading the vacuum. The software can control the switches of three parallel channels, namely three channels can be independently opened or simultaneously opened, or partially opened and partially closed.

9. A control software workstation is installed on the mobile equipment or a working computer for remote monitoring, and the solid-liquid separation process can be monitored at any time.

The freeze drying solid-liquid separation process of the sample completed by the instrument equipment is as follows:

1. and sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a prepared liquid nitrogen tank until the liquid is completely frozen into ice. When the temperature of the liquid material drops below its freezing point, it begins to freeze like ice. The caution points are that the temperature of liquid nitrogen is ultralow (196 ℃ below zero), and the operation process needs to be protected to prevent frostbite.

2. The components are connected in sequence. The collecting bottle is hung below the channel and in the cold trap. The vacuum pump pipeline is connected with the 3 channels in a sealing mode. The collecting bottle, the freeze-drying bottle, the waste liquid receiving bottle and the glass channel are connected in a snap-fit quick connector mode.

3. And turning on a power switch of the instrument, and setting a proper cold trap temperature for precooling. After reaching the preset temperature, the pre-frozen lyophilized vial was hung on the instrument. And turning on a vacuum pump to start vacuumizing.

4. According to the properties of the sample, the proper cold trap gradient temperature control and the gradient vacuum control of the vacuum pump are edited on a control interface or software. The process can be suspended at any time during the separation process, and improper conditions can be changed to optimize the separation conditions.

5. After the separation operation is completed, the vacuum pump stops working, and the vacuum is removed to recover the atmospheric pressure state. And opening the cold trap door, taking out the collection bottle and storing for subsequent detection. The freeze-drying bottle is taken down.

6. The two ends of the channel are replaced by waste liquid receiving bottles, and the steam generator is used for replacing a vacuum pump to clean the flow path, so that a pollution-free environment is provided for the next drying and separating.

The above is a complete liquid-solid separation process.

The invention is suitable for water matrix and organic matrix, has wider application range, can process a plurality of samples at one time, and the filtration/solid-liquid separation devices on the market can process one sample at one time. The invention has large processing capacity and improves the working efficiency. Degree of automation is high, and is safe high-efficient, liberates both hands. Automatic sanitation and cleanness are realized, the cleanness of the system is ensured, and no cross contamination occurs. Volatile and semi-volatile substances are not lost, so that the aim of preventing the detection result from being inaccurate due to pretreatment is fulfilled.

[ example 2 ]

A vacuum freeze-drying type solid-liquid separation device (as shown in figures 1 and 2) comprises a separation area, a cold trap, a vacuum system and a steam generator, wherein the separation area comprises a freeze-drying bottle, a channel and a collecting bottle, the channel is used for connecting the freeze-drying bottle and the collecting bottle, a pipeline connected with the vacuum system and the steam generator is arranged on the channel, the receiving bottle is arranged in the cold trap, the freeze-drying bottle is arranged on the upper surface of the top of the cold trap, a condensing pipe is coiled in the cold trap, and the separation area, the cold trap, the vacuum system, the steam generator and related control equipment are connected with a control software workstation; when solid-liquid separation is carried out, the method comprises the following steps: (1) 1L of sulfur-containing sludge leaching suspension (the solid-liquid ratio is 1:10) is placed in a freeze-drying bottle for sealing, and the sulfur-containing sludge leaching suspension is placed in a freezing layer of a refrigerator for pre-freezing 4 hours before sample treatment until the liquid is completely frozen into ice; (2) connecting the components of the device in sequence; (3) turning on a power switch of the instrument, setting the temperature of a cold trap to be minus 10 ℃ for precooling, connecting the pre-frozen freeze-drying bottle with the channel, and starting to vacuumize; (3) separating operation is carried out, and cold trap gradient temperature control is edited on software: the temperature is kept at minus 10 ℃ for 5min, and the temperature is reduced to minus 30 ℃ at the speed of reducing the temperature by 2 ℃ per minute. The vacuum degree is automatically set, and the vacuum degree is adjusted according to the real-time state of the sludge leaching liquid. (4) After the separation operation is finished, stopping the vacuum system, removing the vacuum, recovering the atmospheric pressure state, taking out the collecting bottle, sealing, and placing at normal temperature for subsequent detection; (5) and taking down the freeze-drying bottle, replacing two ends of the channel with waste liquid receiving bottles, and replacing a vacuum pump with a steam generator to clean the flow path so as to provide a pollution-free environment for next drying and separation.

Description of the vacuum freeze-drying liquid-solid separation method:

1. the separation zone consists of three parts: freeze-drying bottle, passageway, collecting flask. 3 freeze-drying bottles, ground round bottom wide-mouth bottles with the volume of 2L and borosilicate glass. The glass material can resist negative pressure.

2. The freeze-drying bottle is hung on the borosilicate glass channel, and the channel is used for connecting the freeze-drying bottle and the receiving bottle. The end of the vial is attached and the channel has two 90 degree bends so that the vial is attached in a forward orientation rather than being inverted over the channel. The part of the channel exposed to the atmospheric environment is covered with rubber. The channel is provided with a thin tube connected with the vacuum pump and the steam generator, and the thin tube can be used for two purposes, is connected with the vacuum pump and is also connected with the steam generator. To realize that one vacuum pump and one steam generator act on 3 parallel channels simultaneously. Electromagnetic control valves are respectively arranged at the three connected thin pipes and can be independently controlled to be opened and closed.

3. The ground borosilicate glass round-bottom flask corresponds to 3 collecting bottles and has the volume of 2L, and can resist negative pressure. The receiving bottle is placed in the cold trap.

4. The place where the cold trap is connected with the glass is sealed by a sealing ring. The cold trap volume is 8-10L. And a condensing pipe is coiled in the cold trap. The cold trap and the condensing pipe are made of 316L stainless steel, are corrosion-resistant and deformation-resistant, are subjected to electrolytic polishing treatment, are exposed in the cold trap and have the pre-freezing function of the cold trap. The cooling temperature can reach minus 105 ℃, and the sublimation of water and organic solvent can be ensured. The cold trap can realize the function of rapid cooling, reaches the preset temperature and balances the temperature within 2min, and improves the working efficiency. The condenser tube element is arranged in a U-shaped groove formed by punching on four sides, so that an excellent condensation effect is realized. The cold trap uses an embossed stainless steel outer surface. The cold trap door is opened and closed by adopting the design of an automatic switch and is provided with a visible window. And a powerful fan is arranged in the cold trap cabin, so that the temperature rise and the temperature drop are guaranteed to reach the set temperature within 2 min.

5. The vacuum system consists of a vacuum pump, a vacuum sensor and a vacuum electromagnetic valve. The cold trap is connected with the vacuum pump through a pipeline which is resistant to negative pressure and high pressure. The vacuum degree control range is 2-1000mbar, and the display precision is 0.1 mbar. The vacuum pump is a chemical diaphragm vacuum pump, an oil mist filter is required to be configured, and the vacuum pump is environment-friendly. The vacuum solenoid valve is used for controlling the vacuum degree and improving the drying rate. The vacuum pump is simultaneously provided with an adjusting knob, a key and an operation and control display panel.

6. The steam generator is used for automatic hygienic steam cleaning. The steam generator is connected with the glass channel of the separation area through a pipeline, and the whole separation flow path can be cleaned.

7. The touch screen control panel has clear layout. And editing parameter methods, such as cold trap temperature, vacuum degree and the like. Parameters are changed rapidly through the knob and the key and are displayed on the control panel in real time.

8. The control software workstation is convenient to operate, and can record data, display a flow chart and issue a report. And a database of common solid-liquid separation operation methods is stored in the workstation, so that a user can directly call the operation method conveniently. The database is used as method reference, so that the time for user method construction and method optimization is saved. The user can also save the method commonly used in own laboratory and add the method into the database. The functions realized by the software comprise adjusting the program temperature of the cold trap, changing the vacuum degree, the display time, the real-time temperature and the real-time pressure, setting the steam burst amount and the burst time, and unloading the vacuum. The software can control the switches of three parallel channels, namely three channels can be independently opened or simultaneously opened, or partially opened and partially closed.

9. A control software workstation is installed on the mobile equipment or a working computer for remote monitoring, and the solid-liquid separation process can be monitored at any time.

The freeze drying solid-liquid separation process of the sample completed by the instrument equipment is as follows:

1. and sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a freezing layer of a refrigerator until the liquid is completely frozen into ice. When the temperature of the liquid material drops below its freezing point, it begins to freeze like ice. The operation process needs to be well protected to prevent frostbite.

2. The components are connected in sequence. The collecting bottle is hung below the channel and in the cold trap. The vacuum pump pipeline is connected with the 3 channels in a sealing mode. The collecting bottle, the freeze-drying bottle, the waste liquid receiving bottle and the glass channel are connected in a snap-fit quick connector mode.

3. And turning on a power switch of the instrument, and setting a proper cold trap temperature for precooling. After reaching the preset temperature, the pre-frozen lyophilized vial was hung on the instrument. And turning on a vacuum pump to start vacuumizing.

4. According to the properties of the sample, the proper cold trap gradient temperature control and the gradient vacuum control of the vacuum pump are edited on a control interface or software. The process can be suspended at any time during the separation process, and improper conditions can be changed to optimize the separation conditions.

5. After the separation operation is completed, the vacuum pump stops working, and the vacuum is removed to recover the atmospheric pressure state. And opening the cold trap door, taking out the collection bottle and storing for subsequent detection. The freeze-drying bottle is taken down.

6. The two ends of the channel are replaced by waste liquid receiving bottles, and the steam generator is used for replacing a vacuum pump to clean the flow path, so that a pollution-free environment is provided for the next drying and separating.

The above is a complete liquid-solid separation process.

The invention is suitable for water matrix and organic matrix, has wider application range, can process a plurality of samples at one time, and the filtration/solid-liquid separation devices on the market can process one sample at one time. The invention has large processing capacity and improves the working efficiency. Degree of automation is high, and is safe high-efficient, liberates both hands. Automatic sanitation and cleanness are realized, the cleanness of the system is ensured, and no cross contamination occurs. Volatile and semi-volatile substances are not lost, so that the aim of preventing the detection result from being inaccurate due to pretreatment is fulfilled.

[ example 3 ]

A vacuum freeze-drying type solid-liquid separation device (as shown in figures 1 and 2) comprises a separation area, a cold trap, a vacuum system and a steam generator, wherein the separation area comprises a freeze-drying bottle, a channel and a collecting bottle, the channel is used for connecting the freeze-drying bottle and the collecting bottle, a pipeline connected with the vacuum system and the steam generator is arranged on the channel, the receiving bottle is arranged in the cold trap, the freeze-drying bottle is arranged on the upper surface of the top of the cold trap, a condensing pipe is coiled in the cold trap, and the separation area, the cold trap, the vacuum system, the steam generator and related control equipment are connected with a control software workstation; when solid-liquid separation is carried out, the method comprises the following steps: (1) placing 1L of waste salt acidic leaching solution (solid-liquid ratio is 1:10, main components of the waste salt are sodium chloride, other components are metals, triethylamine and the like) in a freeze-drying bottle, sealing, placing in a refrigerator freezing layer for pre-freezing for 1 night before next work until the liquid is completely frozen into ice, and taking out the frozen freeze-drying bottle from the refrigerator the next day; (2) connecting the components of the device in sequence; (3) turning on a power switch of the instrument, setting the temperature of a cold trap to be-15 ℃ for precooling, connecting the pre-frozen freeze-drying bottle with the channel, and starting vacuumizing; (3) separating operation is carried out, and cold trap gradient temperature control is edited on software: at-15 ℃ for 15 min. The vacuum degree is automatically set, and the vacuum degree is adjusted according to the real-time state of the leaching solution. (4) After the separation operation is finished, stopping the vacuum system, removing the vacuum, recovering the atmospheric pressure state, taking out the collecting bottle, sealing, and placing at normal temperature for subsequent detection; (5) and taking down the freeze-drying bottle, replacing two ends of the channel with waste liquid receiving bottles, and replacing a vacuum pump with a steam generator to clean the flow path so as to provide a pollution-free environment for next drying and separation.

Description of the vacuum freeze-drying liquid-solid separation method:

1. the separation zone consists of three parts: freeze-drying bottle, passageway, collecting flask. 3 freeze-drying bottles, ground round bottom wide-mouth bottles with the volume of 2L and borosilicate glass. The glass material can resist negative pressure.

2. The freeze-drying bottle is hung on the borosilicate glass channel, and the channel is used for connecting the freeze-drying bottle and the receiving bottle. The end of the vial is attached and the channel has two 90 degree bends so that the vial is attached in a forward orientation rather than being inverted over the channel. The part of the channel exposed to the atmospheric environment is covered with rubber. The channel is provided with a thin tube connected with the vacuum pump and the steam generator, and the thin tube can be used for two purposes, is connected with the vacuum pump and is also connected with the steam generator. To realize that one vacuum pump and one steam generator act on 3 parallel channels simultaneously. Electromagnetic control valves are respectively arranged at the three connected thin pipes and can be independently controlled to be opened and closed.

3. The ground borosilicate glass round-bottom flask corresponds to 3 collecting bottles and has the volume of 2L, and can resist negative pressure. The receiving bottle is placed in the cold trap.

4. The place where the cold trap is connected with the glass is sealed by a sealing ring. The cold trap volume is 8-10L. And a condensing pipe is coiled in the cold trap. The cold trap and the condensing pipe are made of 316L stainless steel, are corrosion-resistant and deformation-resistant, are subjected to electrolytic polishing treatment, are exposed in the cold trap and have the pre-freezing function of the cold trap. The cooling temperature can reach minus 105 ℃, and the sublimation of water and organic solvent can be ensured. The cold trap can realize the function of rapid cooling, reaches the preset temperature and balances the temperature within 2min, and improves the working efficiency. The condenser tube element is arranged in a U-shaped groove formed by punching on four sides, so that an excellent condensation effect is realized. The cold trap uses an embossed stainless steel outer surface. The cold trap door is opened and closed by adopting the design of an automatic switch and is provided with a visible window. And a powerful fan is arranged in the cold trap cabin, so that the temperature rise and the temperature drop are guaranteed to reach the set temperature within 2 min.

5. The vacuum system consists of a vacuum pump, a vacuum sensor and a vacuum electromagnetic valve. The cold trap is connected with the vacuum pump through a pipeline which is resistant to negative pressure and high pressure. The vacuum degree control range is 2-1000mbar, and the display precision is 0.1 mbar. The vacuum pump is a chemical diaphragm vacuum pump, an oil mist filter is required to be configured, and the vacuum pump is environment-friendly. The vacuum solenoid valve is used for controlling the vacuum degree and improving the drying rate. The vacuum pump is simultaneously provided with an adjusting knob, a key and an operation and control display panel.

6. The steam generator is used for automatic hygienic steam cleaning. The steam generator is connected with the glass channel of the separation area through a pipeline, and the whole separation flow path can be cleaned.

7. The touch screen control panel has clear layout. And editing parameter methods, such as cold trap temperature, vacuum degree and the like. Parameters are changed rapidly through the knob and the key and are displayed on the control panel in real time.

8. The control software workstation is convenient to operate, and can record data, display a flow chart and issue a report. And a database of common solid-liquid separation operation methods is stored in the workstation, so that a user can directly call the operation method conveniently. The database is used as method reference, so that the time for user method construction and method optimization is saved. The user can also save the method commonly used in own laboratory and add the method into the database. The functions realized by the software comprise adjusting the program temperature of the cold trap, changing the vacuum degree, the display time, the real-time temperature and the real-time pressure, setting the steam burst amount and the burst time, and unloading the vacuum. The software can control the switches of three parallel channels, namely three channels can be independently opened or simultaneously opened, or partially opened and partially closed.

9. A control software workstation is installed on the mobile equipment or a working computer for remote monitoring, and the solid-liquid separation process can be monitored at any time.

The freeze drying solid-liquid separation process of the sample completed by the instrument equipment is as follows:

1. and sealing the solid-liquid mixture in a freeze-drying bottle, and pre-freezing the solid-liquid mixture in a freezing layer of a refrigerator until the liquid is completely frozen into ice. When the temperature of the liquid material drops below its freezing point, it begins to freeze like ice. The operation process needs to be well protected to prevent frostbite.

2. The components are connected in sequence. The collecting bottle is hung below the channel and in the cold trap. The vacuum pump pipeline is connected with the 3 channels in a sealing mode. The collecting bottle, the freeze-drying bottle, the waste liquid receiving bottle and the glass channel are connected in a snap-fit quick connector mode.

3. And turning on a power switch of the instrument, and setting a proper cold trap temperature for precooling. After reaching the preset temperature, the pre-frozen lyophilized vial was hung on the instrument. And turning on a vacuum pump to start vacuumizing.

4. According to the properties of the sample, the proper cold trap gradient temperature control and the gradient vacuum control of the vacuum pump are edited on a control interface or software. The process can be suspended at any time during the separation process, and improper conditions can be changed to optimize the separation conditions.

5. After the separation operation is completed, the vacuum pump stops working, and the vacuum is removed to recover the atmospheric pressure state. And opening the cold trap door, taking out the collection bottle and storing for subsequent detection. The freeze-drying bottle is taken down.

6. The two ends of the channel are replaced by waste liquid receiving bottles, and the steam generator is used for replacing a vacuum pump to clean the flow path, so that a pollution-free environment is provided for the next drying and separating.

The above is a complete liquid-solid separation process.

The invention is suitable for water matrix and organic matrix, has wider application range, can process a plurality of samples at one time, and the filtration/solid-liquid separation devices on the market can process one sample at one time. The invention has large processing capacity and improves the working efficiency. Degree of automation is high, and is safe high-efficient, liberates both hands. Automatic sanitation and cleanness are realized, the cleanness of the system is ensured, and no cross contamination occurs. Volatile and semi-volatile substances are not lost, so that the aim of preventing the detection result from being inaccurate due to pretreatment is fulfilled.

[ COMPARATIVE EXAMPLE ]

1L of soil and sludge leachate is filtered by a pressure filter:

1. opening the upper cover of the filter

2. The pressure filter is internally provided with an adaptive fiber filter membrane

3. Loading the prepared leachate into a filter, sealing the filter, and covering the filter with a cover

4. A beaker is arranged below the pressure filter to receive the filtered leaching solution

5. Connecting filter and air compressor

6. The air compressor was turned on and 2 atmospheres were set to pressurize.

The filter pressing rate is observed to be 1s/2 drops, and the efficiency is lower. Along with the pressurizing process, the filter membrane is completely blocked by sludge particles, the pressure in the filter is too high, and the filter membrane cannot bear the final rupture. The solid-liquid substances in the filter are all spilled out.

As can be seen from the comparative example, the safety factor and the working efficiency are low. The pressurization operation is a potential safety hazard factor in a laboratory, and personal and property losses are easily caused. Compared with the pressurization operation, the decompression operation and the pressurization operation are safe and environment-friendly, and the vacuum pump occupies a floor area which is many times smaller than that of an air compressor. And the vacuum pump can carry out pressure control according to real-time status, and degree of automation is high. The invention has self-cleaning function, reduces the labor of experimenters, and is convenient and quick. The leachate is pre-frozen at night after work, or is pre-frozen while other operations are carried out, so that no time is wasted. After pre-freezing, the solid-liquid separation operation only needs 15 minutes, thus greatly improving the separation efficiency.