CN115011819B

CN115011819B - Multistage filter-pressing rupture of membranes mercury purification device

Info

Publication number: CN115011819B
Application number: CN202210934819.XA
Authority: CN
Inventors: 陈彩霞; 李辉; 陆克槨; 单春峰; 李子圣
Original assignee: Beijing Brunt Technology Co ltd
Current assignee: Beijing Brunt Technology Co ltd
Priority date: 2022-08-05
Filing date: 2022-08-05
Publication date: 2022-10-28
Anticipated expiration: 2042-08-05
Also published as: CN115011819A

Abstract

The invention discloses a multistage filter-pressing membrane-breaking mercury purification device, which belongs to the technical field of mercury purification, wherein a multistage filtering and purifying part is used for performing graded fine filtering and purification on coarse mechanical impurities, fine dust after mercury soot membrane breaking and a metal oxide membrane to obtain recyclable fine mercury which meets the requirement of mercury intrusion experimental quality standard; the gas-liquid storage part is used for driving gas, purifying the advancing crude mercury, filtering the mercury by stages of a secondary filter and a tertiary filter, filtering qualified fine mercury, deionizing circulating water and storing the sewage by sub-stations of process flushing; the output end of a nitrogen generator in the air pressure driving unit is connected with the input end of a nitrogen buffer tank through a nitrogen source electromagnetic valve, and an inlet pressure sensor is arranged on a pipeline between the nitrogen source electromagnetic valve and the nitrogen buffer tank. The invention has reliable performance, safety, environmental protection and high environmental applicability, can realize the on-site and timely environmental protection treatment by a mercury laboratory, and reduces the risk of secondary pollution diffusion transfer; and the absolute amount of laboratory mercury can be reduced.

Description

Multistage filter-pressing rupture of membranes mercury purification device

Technical Field

The invention belongs to the technical field of mercury purification, and particularly relates to a multistage filter-pressing membrane-breaking mercury purification device.

Background

Mercury is a silvery white liquid metal, often called "mercury", and is the only metal that naturally exists in a liquid state at room temperature. The mercury has high density (13.6 g/cm < 3 >), low melting point (-38.87 ℃), boiling point of about 357 ℃, and important application in the fields of chemical industry, electrical appliances, instruments, medicine, metallurgy, military industry and new technology.

The rock core mercury intrusion method is widely used in the fields of laboratories of various oil fields in China and the industrial protection research field of energy geological nuclei, is used for detecting the porosity of concrete, mortar and the like in material science and engineering professional laboratories, is used for representing indexes such as air holes in the concrete and the like, and needs to consume a large amount of mercury when detecting a rock core sample every year, particularly the rock core mercury intrusion method is the most reliable method for determining the rock pore structure and knowing the stratum characteristics in the current geological laboratories, and has no better alternative detection means at present. The purity of the polluted mercury which is generated after the detection test and is contacted with the detection medium is reduced, the polluted mercury cannot be used continuously, meanwhile, part of mercury enters the hole of the rock core to form mercury-containing rock core toxic dangerous waste, if the polluted mercury cannot be timely and environmentally-friendly treated and purified, a large amount of storage has huge environmental protection safety risks, and even normal experiment development is influenced by the control limitation of the total quantity of the taken mercury, therefore, the mercury in the mercury-containing rock core needs to be timely extracted and reused, the purity of the generated mercury is generally lower than 98 percent and lower than the use standard, the low-crude mercury or the polluted mercury is purified and reused, the economic value is realized, the combined recycling is realized, and the environmental protection policy of the total quantity is reduced.

At present, mercury purification methods mainly comprise a high-temperature distillation method, a chemical-electrochemical method, a cyclone separation purification method, a high-temperature atomic steam + composite purification method and the like. The disadvantages of high-temperature distillation purification and high-temperature atomic steam + composite purification are that the danger of producing highly toxic mercury vapor is great; the chemical-electrochemical method has the problems that secondary pollution liquid is difficult to treat in an environment-friendly way and secondary pollution chains are retreated; besides the prior purification purity, the application scene of the cyclone separation purification equipment is not suitable for the small-scale and space-limited laboratory on-site purification scene.

Disclosure of Invention

Based on the technical problems in the prior art, the invention provides a multi-stage filter-pressing membrane-breaking mercury purification device, in particular to a multi-stage filter-pressing membrane-breaking mercury purification device under the normal temperature condition, which solves the problem that the traditional mercury purification method harms operators and the environment due to high-temperature highly toxic mercury vapor; meanwhile, the problems of secondary dangerous waste gas, waste liquid and solid pollution caused by a chemical-electrochemical purification method and unsuitability for small-scale mercury purification application scenes are solved.

According to the technical scheme of the invention, the invention provides a multistage filter-pressing membrane-breaking mercury purification device which comprises an automatic process operation and quality control electric part, a multistage filter purification part, a gas-liquid pressure power part, a gas-liquid storage part and a gas pressure driving unit, wherein the automatic process operation and quality control electric part is used for on-off control, flow path conversion, operation sequence control, sensor data acquisition, subprogram skip and identification and judgment on whether a quality control index critical condition is met or not of pump and solenoid valve electric elements in the multistage filter-pressing membrane-breaking mercury purification device so as to realize automatic operation of the device in the treatment process;

the multistage filtration purification part is used for performing graded fine filtration purification on coarse mechanical impurities, mercury soot broken fine dust and a metal oxide film in a multistage filter-pressing membrane-breaking mercury purification device to obtain recyclable fine mercury meeting the experimental quality standard requirement of mercury pressing;

the gas-liquid pressure power part is used for providing driving and pressure for gas liquid in the multistage filter-pressing membrane-breaking mercury purification device;

the gas-liquid storage part is used for driving gas, purifying advanced crude mercury, filtering mercury in stages by a secondary filter and a tertiary filter, filtering qualified refined mercury, deionizing circulating water and storing flow flushing sewage in a multi-stage filter-pressing membrane-breaking mercury purification device in a substation;

the air pressure driving unit comprises a nitrogen generator and a nitrogen buffer tank, the output end of the nitrogen generator is connected with the input end of the nitrogen buffer tank through a nitrogen source electromagnetic valve, and an inlet pressure sensor is arranged on a pipeline between the nitrogen source electromagnetic valve and the nitrogen buffer tank; the output end of the nitrogen buffer tank is connected with the input end of the thick mercury bottle through an electromagnetic valve at the outlet of the buffer tank; an external vent pipe is further arranged on the pipeline between the nitrogen buffer tank and the crude mercury bottle in a branching manner, and a gas-liquid vent electromagnetic valve is arranged in the external vent pipe.

Preferably, the gas-liquid in the multistage filter-press membrane-breaking mercury purification device comprises nitrogen, deionized water and mercury. More preferably, the gas-liquid pressure power part is used for providing driving and pressure for flowing, circulating, membrane breaking, flushing and purifying of nitrogen, deionized water and mercury in the multistage filter-pressing membrane-breaking mercury purification device.

Further, the multistage filter-pressing membrane-breaking mercury purification device further comprises an air pressure driving unit, a coarse mercury bottle, a pre-filtering column, a secondary filter, a tertiary filter and a fine mercury collecting bottle which are sequentially connected through a pipeline assembly. The pneumatic driving unit is used for filling mercury to be filtered in the upper chambers of the secondary filter and the tertiary filter, pressurizing and filtering the lower chambers of the secondary filter and the tertiary filter and flushing the flow line.

Wherein, the crude mercury bottle is used for storing the crude mercury to be treated or quantitatively storing the polluted mercury. The pre-filtering column is used for primary filtering of coarse mechanical impurities in coarse mercury or polluted mercury, and pollution and flow blockage to the secondary filter are reduced.

Further, the secondary filter is used for filtering fine dust impurities and realizing filter pressing and mechanical shock comprehensive membrane breaking of the mercury soot mixture. The three-stage filter is used for further fine filtration of the second-stage filtered mercury, dissolution of an oxidation film and buoyancy reverse washing circulation deep purification of deionized water.

Preferably, the fine mercury collecting bottle is used for collecting and storing fine mercury which reaches the mercury standard for mercury injection experiments after being sequentially and gradually purified by pre-filtration column filtration, secondary filter filtration, tertiary filter filtration and deionized water reverse buoyancy flushing.

Compared with the prior art, the multistage filter-pressing membrane-breaking mercury purification device has the following beneficial technical effects:

1. according to the scheme, the purity of the crude mercury is gradually improved by a multi-stage filter-pressing membrane-breaking deionized water buoyancy reverse circulation purification technology under a normal temperature condition, and finally the purity of the purified mercury is over 99.9%, so that the purity of the purified mercury meets the mercury purity specified in laboratory mercury pressure method capillary pressure curve experimental standard GB/T2650.1-2008.

2. The invention does not adopt high-temperature vacuum distillation or chemical-electrochemical treatment of the traditional mercury purification method, thereby avoiding the generation of high-temperature virulent mercury vapor or secondary dangerous waste and the problem that the application scene of small-scale mercury purification is not suitable; meanwhile, the technical problems of regeneration treatment for purifying pollutants and mercury removal and standard discharge of discharged sewage are solved, and a brand new technical path is opened up for purification treatment and reutilization of laboratory-scale crude mercury.

3. The invention has reliable performance, safety, environmental protection and high environmental applicability, can realize on-site timely environmental protection treatment by a mercury laboratory, and reduces the risk of secondary pollution diffusion transfer; and the absolute amount of mercury in a laboratory can be reduced, the recycling is promoted, and the method has good economic benefit, environmental protection social benefit and meets the requirement of environmental protection policy encouragement.

4. The invention adopts a pre-filtering column, a secondary filter and a tertiary filter to form a multi-stage screen mesh number increasing filtering combination, constructs a pressure extrusion continuous membrane-breaking optimized functional structure system, and fully utilizes the properties of mercury being a normal-temperature high-density liquid and high specific surface tension and the multi-stage screen extrusion friction membrane-breaking effect.

The scheme of the invention adopts PLC programming, synchronous touch screen flow, automatic quality control detection, discharge mercury removal purification and other intelligent technologies for micro integrated manufacturing, and achieves the aims of minimizing field occupation, environment-friendly discharge waste liquid reaching standards and diversified application scenes under normal temperature conditions.

Drawings

FIG. 1 is a schematic structural diagram of a multistage filter-pressing membrane-breaking mercury purification device.

FIG. 2 is a schematic cross-sectional view of a pre-filter column of the present invention.

FIG. 3A is a schematic view of the assembly of the parts of the two-stage filter of the present invention.

FIG. 3B is a schematic cross-sectional view of a two-stage filter according to the present invention.

Fig. 4A is a schematic cross-sectional structure of a three-stage filter of the present invention.

Fig. 4B is a partially enlarged view of a portion of the tertiary filter tube of fig. 4A.

FIG. 5 is a schematic structural diagram of a transmittance detection module and a detection tube according to the present invention.

Fig. 6 is a schematic structural view of a mercury removal filter preferably used in the deionized water circulation mercury removal filter and/or the sewage discharge mercury removal filter according to the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a multistage filter-pressing membrane-breaking mercury purification device, wherein a secondary filter and a tertiary filter which are originally designed are adopted, so that crude mercury with a mercury soot structure passes through a multistage filter screen under the action of air pressure driving, and the multistage filter-pressing membrane-breaking purification under the normal temperature condition is realized. The device is a multi-stage filter-pressing membrane-breaking mercury purification device under the normal temperature condition, wherein the normal temperature condition is a working environment under the room temperature and the standard atmospheric pressure.

The invention discloses a multistage filter-pressing membrane-breaking mercury purification device, which comprises an automatic process operation and quality control electrical part, a multistage filtering and purification part, a gas-liquid pressure power part and a gas-liquid storage part, wherein the multistage filtering and purification part is used for performing graded fine filtering and purification on coarse mechanical impurities, fine dust after mercury soot membrane breaking and a metal oxide membrane so as to obtain recyclable fine mercury meeting the experimental quality standard requirement of mercury pressing; the gas-liquid storage part is used for driving gas, purifying advanced crude mercury, filtering mercury by stages of a secondary filter and a tertiary filter, filtering qualified fine mercury, deionizing circulating water and storing flow flushing sewage in substations. The invention adopts a pre-filtering column, a secondary filter and a tertiary filter to form a multi-stage screen mesh increasing filtration combination, constructs a pressure extrusion continuous membrane breaking optimization functional structure system, and fully utilizes the properties of mercury being a normal-temperature high-density liquid and high specific surface tension and the multi-stage screen extrusion friction membrane breaking effect.

The technical principle of the multistage filter-pressing membrane-breaking mercury purification device provided by the invention is as follows: compared with the traditional high-temperature distillation purification method, the chemical-electrochemical and other traditional methods, the technical scheme of the invention has the advantages of safer personnel operation environment and less harm of secondary diffusion transfer of environmental pollution, and is suitable for popularization and utilization in small-scale scenes of professional laboratories in a plurality of professional fields of mercury utilization. The multi-stage filter-pressing membrane-breaking mercury purification device ensures that the discharged sewage meets the relevant environmental protection standard. The method adopts an automatic and miniaturized integrated process flow for manufacturing, improves the applicability of the application environment, realizes the on-site timely environment-friendly treatment by a mercury laboratory, and reduces the risk of secondary pollution diffusion transfer.

In the crude mercury having impurities, mercury and most of the media have a characteristic of high interfacial tension, so that an oxide film or a dust interfacial film may be formed on an outer layer of mercury. For example, mercury soot is a loose substance formed in the mercury refining process and composed of small mercury beads, fine mineral dust, arsenic antimony oxide, hydrocarbon, water, mercury sulfide, mercury sulfate and the like, and mercury soot structure also exists in the polluted mercury detected by mercury overpressure method. The mercury beads are surrounded by a tough film and dispersed in the medium, so that the film needs to be broken during the physical purification treatment to release mercury and polymerize the mercury together, which is called "membrane rupture". For example, mercury is recovered by washing with water to remove most of the soot and separate mercury which is easily polymerized, and then placing into a mercury soot machine to destroy the membrane on the surface of mercury under mechanical compression to polymerize mercury.

The multi-stage filter-pressing membrane-breaking mercury purification device is explained below with reference to the accompanying drawings. The multi-stage filter-pressing membrane-breaking mercury purification device comprises an automatic flow operation and quality control electric part, a multi-stage filtration purification part, a gas-liquid pressure power part and a gas-liquid storage part, wherein:

the automatic flow operation and quality control electrical part is used for on-off control, flow path conversion, operation sequence control, sensor data acquisition, subprogram skipping and identification and judgment on whether quality control index critical conditions are met or not of electrical elements such as pumps and electromagnetic valves in the multistage filter-pressing membrane-breaking mercury purification device so as to realize automatic operation of the device in the treatment process;

the gas-liquid pressure power part is used for providing drive and pressure for gas-liquid (nitrogen, deionized water and mercury) flowing, circulating, membrane breaking, flushing and purifying in the multistage filter-pressing membrane-breaking mercury purification device;

the air pressure driving unit comprises a nitrogen generator and a nitrogen buffer tank, the output end of the nitrogen generator is connected with the input end of the nitrogen buffer tank through a nitrogen source electromagnetic valve, and an inlet pressure sensor is arranged on a pipeline between the nitrogen source electromagnetic valve and the nitrogen buffer tank; the output end of the nitrogen buffer tank is connected with the input end of the thick mercury bottle through an outlet electromagnetic valve of the buffer tank; an external vent pipe is further arranged on the pipeline between the nitrogen buffer tank and the crude mercury bottle in a branching manner, and a gas-liquid vent electromagnetic valve is arranged in the external vent pipe.

Further, referring to fig. 1, the automatic process operation and quality control electrical part includes a nitrogen source inlet control solenoid valve 1 (normally closed type), a buffer tank outlet solenoid valve 2 (normally closed type), a gas-liquid vent solenoid valve 3 (normally closed type), a coarse mercury charging control solenoid valve 4 (normally closed type), a process isolation solenoid valve 5 (normally open type), a coarse mercury outlet solenoid valve 6 (normally open type), a pre-filter column outlet solenoid valve 7 (normally open type), a filter flushing bypass solenoid valve 8 (normally open type), a secondary filter isolation solenoid valve 9 (normally open type), a secondary filter flushing solenoid valve 10 (normally open type), a tertiary filter inlet solenoid valve 11 (normally open type), a tertiary filter top cleaning solenoid valve 12 (normally open type), a tertiary filter mercury outlet solenoid valve 13 (normally closed type), a transmittance detection module 41, a detection tube top isolation solenoid valve 14 (normally closed type), a drug liquid pump outlet solenoid valve 15 (normally closed type), a deionized water circulation pump outlet solenoid valve 16 (normally closed type), a fine mercury filling control solenoid valve 17 (normally closed type), a deionized water return liquid inlet solenoid valve 18 (normally open type), a discharge circulation conversion solenoid valve 19 (normally open type), and a wastewater discharge conversion solenoid valve 20 (normally closed type); and control circuits and devices connected with the components, such as a PLC (programmable logic controller) electric automation control system (including PLC control software and the like) and a touch screen for displaying and operating.

The multi-stage filtration and purification part comprises a pre-filtration column 21, a secondary filter 22 (which is a coarse mercury vibration screening filter), a tertiary filter 23 (which is a fine static filter or a precision filter), a deionized water circulation mercury removal filter 24 and a sewage discharge mercury removal filter 25.

The gas-liquid pressure power part comprises a sample injection pressurizing pump 26, a liquid medicine pump 27, a deionized water circulating pump 28 (preferably, the three pumps are all peristaltic pumps), a nitrogen generator 29, a vortex oscillator 30, an inlet pressure sensor 31, an intermediate pressure sensor 32 and an outlet pressure sensor 33.

The gas-liquid storage part comprises a low-pressure nitrogen buffer tank 34, a coarse mercury bottle 35, a fine mercury collecting bottle 36, a detection tube 37 (which is a quartz glass tube and is matched with a light transmittance detection module 41 to realize gas-water mercury detection), a purified liquid medicine bottle 38, a deionized water bottle 39 and an outlet sewage bottle 40.

In one embodiment, the multistage filter-pressing membrane-breaking mercury purification device comprises an air pressure driving unit, a coarse mercury bottle 35, a pre-filtering column 21, a secondary filter 22, a tertiary filter 23 and a fine mercury collecting bottle 36 which are sequentially connected through a pipeline assembly.

The pneumatic driving unit is used for filling mercury to be filtered in the upper chambers of the secondary filter and the tertiary filter, pressurizing and filtering the lower chambers of the secondary filter and the tertiary filter and flushing a flow pipeline;

a coarse mercury bottle 35 for storing the coarse mercury to be treated or quantitatively storing the polluted mercury;

the pre-filtering column 21 is used for primary filtering of coarse mechanical impurities in coarse mercury or polluted mercury, and pollution and flow blockage to a secondary filter are reduced;

a secondary filter 22, which is used for filtering fine dust impurities and realizing filter pressing and mechanical vibration comprehensive rupture of the mercury soot mixture;

the third filter 23 is used for further fine filtration of the second-stage filtered mercury, oxidation film dissolution, reverse flushing circulation of deionized water buoyancy and other deep purification;

and the fine mercury collecting bottle 36 is used for collecting and storing fine mercury which reaches the mercury standard for mercury intrusion experiments after being sequentially and gradually purified by pre-filtering column filtering, secondary filter filtering, tertiary filter filtering, deionized water reverse buoyancy flushing and the like.

The air pressure driving unit comprises a nitrogen generator 29 and a nitrogen buffer tank 34, the output end of the nitrogen generator 29 is connected with the input end of the nitrogen buffer tank 34 through a nitrogen source electromagnetic valve 1, and an inlet pressure sensor 31 is arranged on a pipeline between the nitrogen source electromagnetic valve 1 and the nitrogen buffer tank 34; the output end of the nitrogen buffer tank 34 is connected with the input end of the thick mercury bottle 35 through the buffer tank outlet electromagnetic valve 2; an external vent pipe is further arranged on the pipeline between the nitrogen buffer tank 34 and the crude mercury bottle 35 in a branching manner, and a gas-liquid vent electromagnetic valve 3 is arranged in the external vent pipe.

The input end of the thick mercury bottle 35 is further connected with a thick mercury feeding unit, the thick mercury feeding unit comprises a sample feeding pipe, the input end of the sample feeding pipe is used for being connected with an external thick mercury container for storing mercury to be purified, the output end of the sample feeding pipe is connected with a sample feeding pressurizing pump 26, and the output end of the sample feeding pressurizing pump 26 is connected with the feed inlet of the thick mercury bottle 35 through a thick mercury feeding electromagnetic valve 4.

The output end of the coarse mercury bottle 35 is connected with the input end of the pre-filter column 21 through a coarse mercury outlet electromagnetic valve 6. The output end of the pre-filter column 21 is connected with the input end of the secondary filter 22 through the pre-filter column outlet electromagnetic valve 7.

The secondary filter 22 is provided with a secondary upper cavity, a secondary filter pipe and a secondary lower cavity which are sequentially communicated from top to bottom, a discharge hole at the bottom of the secondary lower cavity is connected with the input end of the tertiary filter 23 through a tertiary filter inlet electromagnetic valve 11, and a middle pressure sensor 32 is arranged on a pipeline between the secondary filter 22 and the tertiary filter inlet electromagnetic valve 11.

The three-stage filter 23 is provided with a three-stage upper cavity, a three-stage filter pipe and a three-stage lower cavity which are sequentially communicated from top to bottom, and a discharge hole at the bottom of the three-stage lower cavity is sequentially connected with a fine mercury collecting bottle 36 through a three-stage filter mercury outlet electromagnetic valve 13 and a fine mercury filling control electromagnetic valve 17.

In another embodiment, the system further comprises a fine mercury standard-reaching detection unit, a deionized water washing unit, a dosing unit and a clean pollution discharge unit.

The fine mercury standard-reaching detection unit is used for detecting the cleanliness (light transmittance) of a circulating liquid obtained after fine mercury filtered by the three-stage filter is circularly flushed by deionized water so as to indirectly judge whether mercury subjected to deep filtration treatment by the three-stage filter reaches the standard or not; if the flushing time does not reach the standard, further determining to continue circulating flushing; if the standard is reached, opening a fine mercury bottle filling valve to carry out fine mercury filling;

the deionized water cleaning unit is used for pumping deionized water from a second outlet at the bottom cavity or the top of the second-stage filter or the bottom cavity or the top of the third-stage filter by using a circulating pump, flushing, cleaning and unblocking filter screens and upper cavities of the second-stage filter and the third-stage filter, and guiding sewage into a sewage bottle through a sewage discharge pipeline;

the dosing unit is used for dissolving trace chemical agents in the filtered mercury which still has a metal oxide film after three-stage filtration (preferably physical filtration) so as to improve the purity of the mercury and ensure that the mercury is finally purified to reach the standard;

and the cleaning and sewage discharging unit is used for flushing and back flushing non-pure mercury substances such as impurity, dust and particles generated in the purification processes of pre-filtration, secondary filtration, tertiary filtration, reverse buoyancy circulating flushing and the like, and discharging the non-pure mercury substances into the sewage bottle, and then removing mercury through the mercury removal filter, so that the environment is protected and discharged after reaching the standard.

The accurate mercury detection unit up to standard includes the detection tube 37 and is arranged in detecting the luminousness of fluid luminousness among them and detects module 41, and the lower extreme of detection tube 37 is connected with the pipeline between tertiary filter mercury export solenoid valve 13 and the accurate mercury filling control solenoid valve 17.

The deionized water cleaning unit comprises a deionized water bottle 39, and the output end of the deionized water bottle 39 is connected with the upper end of the detection tube 37 through the deionized water circulating pump 28 and the outlet electromagnetic valve 16 of the deionized water circulating pump in sequence. An outlet pressure sensor 33 is provided on a line between the deionized water circulating pump outlet solenoid valve 16 and the detection pipe 37. The upper cavity of the third level is connected with an upper outlet of a third level filter, and is connected with an input end of a deionized water bottle 39 through a top cleaning electromagnetic valve 12 of the third level filter, a deionized water circulating mercury removing filter 24 and a deionized water return inlet electromagnetic valve 18 in sequence. The pipeline between the deionized water circulating pump outlet electromagnetic valve 16 and the detection pipe 37 is branched and connected with the pipeline between the three-stage filter top cleaning electromagnetic valve 12 and the deionized water circulating mercury removing filter 24 through the detection pipe top isolation electromagnetic valve 14.

The medicine adding unit comprises a purification liquid medicine bottle 38, and the output end of the purification liquid medicine bottle 38 is connected with the upper end of the detection tube 37 through the liquid medicine pump 27 and the liquid medicine pump outlet electromagnetic valve 15 in sequence.

The cleaning and sewage discharging unit comprises an outlet sewage bottle 40, a branch pipe is branched on a pipeline between the flow Cheng Geli electromagnetic valve 5 and the crude mercury outlet electromagnetic valve 6 and is connected with the input end of the outlet sewage bottle 40 through a secondary filter isolation electromagnetic valve 9. The output end of the outlet sewage bottle 40 is a sewage discharge pipe, and a sewage discharge mercury removal filter 25 and a sewage discharge electromagnetic valve 20 are arranged in the sewage discharge pipe. A branch line branches off the line between stream Cheng Geli solenoid valve 5 and secondary filter isolation solenoid valve 9 and connects to secondary filter 22 through a filtrate flush bypass solenoid valve 8. The secondary upper chamber of the secondary filter 22 has a drain outlet and is connected to the input of an outlet dirty water bottle 40 via a secondary filter flush solenoid valve 10. A branch pipe is branched from the pipeline between the top cleaning electromagnetic valve 12 of the three-stage filter and the deionized water circulating mercury removing filter 24 and is connected with the input end of the outlet sewage bottle 40 through a discharge circulating conversion electromagnetic valve 19.

The structure of the pre-filter column 21 in the multistage filter-press membrane-breaking mercury purification device is shown in fig. 2, and comprises a pre-filter column outlet end cover 213, a pre-filter column filter pipe 214, and a pre-filter column inlet end cover 215. The pre-filter column filter tube 214 is, for example, a double-threaded quartz glass tube, two ends of the pre-filter column filter tube are respectively connected with the pre-filter column outlet end cover 213 and the pre-filter column inlet end cover 215 in a threaded manner, and the two ends and the pre-filter column inlet end cover 215 together form a space for accommodating a filter structure of the pre-filter column 21, and the filter structure includes two glass fiber portions 211 close to the pre-filter column outlet end cover 213 and the pre-filter column inlet end cover 215 and a quartz glass ball portion 212 located in the middle. Specifically, in a preferred embodiment, the filter structure is a filter layer which is sequentially packed in a sandwich structure along the filtering direction, namely, a glass fiber part 211 (high temperature resistant glass fiber) with a thickness of one third at the front end (length of the pre-filter column filter tube 214), a quartz glass ball part 212 (for example, a 20-mesh quartz glass ball) with a thickness of one third at the middle, and a glass fiber part 211 (high temperature resistant glass fiber) with a thickness of one third at the rear end, wherein the glass fiber part 211 and the quartz glass ball part 212 fill the space for accommodating the filter structure. The outlet end cover 213 of the pre-filter column and the inlet end cover 215 of the pre-filter column are both provided with a connector for connection, the connectors penetrate through the inner space and the outer space of the pre-filter column 21, and the pre-filter column 21 is in a sealing structure except for the two connectors. During operation, coarse mercury enters the internal filter structure through the input end of the pre-filter column 21 (the interface of the inlet end cap 215 of the pre-filter column), passes through the three-layer structure of the filter structure layer by layer, and is finally discharged from the output end (the interface of the outlet end cap 213 of the pre-filter column), so as to realize the pre-filter process. The coarse mercury passes through the pre-filter column 21 to filter out most of the particle impurity components (which cannot pass through the gap between the glass fiber part 211 and the quartz glass ball part 212 and are blocked).

The structure of the secondary filter 22 in the multistage filter-press membrane-breaking mercury purification device is shown in fig. 3A (assembly drawing) and fig. 3B (sectional drawing), and comprises a secondary top spiral end cover 2201, a secondary vibrating screen friction cavity 2202, a first O-shaped sealing ring 2206, a secondary filter first-stage screen 2205, a secondary intermediate reducing pipe 2203 (pressurization and acceleration are realized by a reducing structure), a second O-shaped sealing ring 2208, a secondary filter second-stage filtering screen 2207 and a secondary crude mercury receiving cavity 2204 which are sequentially connected from top to bottom.

The upper part of the second-stage top spiral end cover 2201 is a cover plate, a second-stage filter feeding hole 2209 and a second-stage filter sewage discharge port 2210 which are communicated are arranged on the cover plate side by side, and the second-stage filter feeding hole 2209 and the second-stage filter sewage discharge port 2210 are provided with interfaces for connection. The lower portion of the secondary top helical end cap 2201 is a cylindrical first connecting section with external threads. Secondary top helical end cap 2201 is preferably polytetrafluoroethylene.

The upper section of the second-stage vibrating screen friction cavity 2202 is a cylindrical second connecting section with internal threads, and is connected with the first connecting section at the lower part of the second-stage top spiral end cover 2201 in a matching manner. The inner side of the middle section of the second-stage vibrating screen friction cavity 2202 is an inverted frustum-shaped through hole which is wide at the top and narrow at the bottom. The lower section of the second-stage vibrating screen friction cavity 2202 is a cylindrical third connecting section with external threads. The second-stage vibrating screen friction cavity 2202 is preferably made of polytetrafluoroethylene.

The second-stage intermediate reducing pipe 2203 is embedded in the third connecting section of the second-stage vibrating screen friction cavity 2202 in a matching manner, and the bottom end faces of the second-stage vibrating screen friction cavity and the third connecting section are flush. The inner side of the second-stage middle reducing pipe 2203 is an inverted truncated cone-shaped through hole with a wide upper part and a narrow lower part, and a first blocking shoulder is arranged at the opening of the through hole at the upper part. The secondary intermediate diameter reducer 2203 is preferably a metal or quartz glass tubing string and is replaceable.

The first O-ring 2206 (preferably made of silica gel) and the first-stage screen 2205 (preferably made of stainless steel or nylon, 40 mesh) of the second-stage filter are clamped and fixed between the bottom of the middle section of the second-stage vibrating screen friction cavity 2202 and the first blocking shoulder of the second-stage intermediate reducing pipe 2203.

The upper section of the secondary coarse mercury receiving cavity 2204 is a cylindrical fourth connecting section with internal threads, and is connected with the third connecting section of the secondary vibrating screen friction cavity 2202 in a matching manner. The lower section of the secondary coarse mercury receiving cavity 2204 is cylindrical with a bottom surface. A second shoulder is formed between the upper section and the lower section of the secondary coarse mercury-receiving cavity 2204. The secondary coarse mercury receiving cavity 2204 is preferably made of polytetrafluoroethylene.

A second O-ring 2208 (preferably made of silica gel) and a second-stage filtering screen 2207 (preferably made of stainless steel or nylon and 80-mesh) of the second-stage filter are clamped and fixed between the bottom of the third connecting section of the second-stage vibrating screen friction cavity 2202 and the second stop shoulder of the second-stage coarse mercury receiving cavity 2204.

A secondary filter discharge port 2211 is arranged at the bottom of the lower section of the secondary coarse mercury receiving cavity 2204, and the outward end of the secondary filter discharge port 2211 is a connector for connection.

In one embodiment, the secondary filter 22 is a fully detachable structure, and is integrally formed with a secondary upper cavity, a secondary filter tube and a secondary lower cavity which are sequentially communicated from top to bottom. The second-stage upper cavity is surrounded by a second-stage top spiral end cover 2201, a second-stage vibrating screen friction cavity 2202 and a second-stage filter first-stage screen 2205 and is in a shape formed by a cone, a cylinder and an inverted circular truncated cone from top to bottom. The secondary filter pipe consists of a secondary filter first-stage screen 2205, a secondary intermediate reducing pipe 2203 and a secondary filter screen 2207. The second-stage lower cavity is surrounded by a second-stage filter screen 2207 of the second-stage filter and a second-stage coarse mercury receiving cavity 2204 and is in a shape formed by a cylinder and an inverted cone from top to bottom.

And referring to fig. 1, a vortex oscillator 30 is installed at a lower portion of the secondary filter 22 for oscillating it.

The operation and principle of the secondary filter 22 is as follows. Coarse mercury is pressed into a cavity at the upper part of the second stage, and a vibrating screen is used for friction rupture of membranes. And then, the pressure is continuously utilized to enable the coarse mercury to pass through a first-stage screen 2205 of the secondary filter and a second-stage filter screen 2207 of the secondary filter, filter pressing, friction and membrane breaking are carried out, meanwhile, the vortex oscillator 30 is utilized to carry out vortex oscillation operation, and during filter pressing and membrane breaking filtration, homogenization is fully oscillated so as to obtain a better membrane breaking and purifying effect. After being filtered by the secondary filter 22, the low-density coarse mercury rich in impurities and oxide films is distributed on the upper part of the secondary filter secondary filtering screen 2207 or is positioned in a secondary upper cavity, and relatively pure high-density mercury is mutually attracted, polymerized and deposited on the bottom layer of the inverted cone at the bottommost part of the secondary lower cavity to form a primary gravity differentiation layering effect.

The structure of the tertiary filter 23 in the multistage filter-press membrane-breaking mercury purification device is shown in fig. 4A (whole cross-sectional view) and fig. 4B (partial enlarged view of the tertiary filtration tube section in fig. 4A), and includes a tertiary upper inlet seat 2302, a tertiary upper flange seat 2303, a tertiary filtration tube, a tertiary lower flange seat 2306, and a tertiary lower outlet seat 2308, which are sequentially connected from top to bottom.

The third-stage upper inlet seat 2302 is in an inverted bowl shape, and a third-stage filter feed opening 2301 and a third-stage filter upper outlet 2321 which are communicated with each other are arranged at the upper part of the third-stage upper inlet seat 2302 and are provided with interfaces for connection. Third O-ring 2304 is disposed between third-stage upper inlet seat 2302 and third-stage upper flange seat 2303, specifically, for example, an annular accommodating groove is opened on the upper surface of third-stage upper flange seat 2303, third O-ring 2304 is embedded in the accommodating groove, and the top of third O-ring 2304 is in contact with the lower surface of third-stage upper inlet seat 2302. Tertiary upper inlet seat 2302 is coupled to tertiary upper flange seat 2303, for example, by bolts. The bottom of the third-stage upper flange seat 2303 is provided with a through hole and is communicated with the upper end of the third-stage filter pipe.

Tertiary lower part export seat 2308 is the bowl form, is provided with the tertiary filter discharge gate 2309 that has the interface in tertiary lower part export seat 2308's lower part, is provided with fourth O type sealing washer 2307 between tertiary lower part export seat 2308 and tertiary lower part flange seat 2306, specifically for example annular holding tank has been seted up at tertiary lower part export seat 2308 upper surface, fourth O type sealing washer 2307 embedding sets up in this holding tank, and the top of fourth O type sealing washer 2307 is inconsistent with tertiary lower part flange seat 2306's lower surface. Tertiary lower outlet seats 2308 are connected to tertiary lower flange seats 2306, for example by bolts. The upper portion of the third stage lower flange seat 2306 has a through hole and communicates with the lower end of a third stage filter tube in the form of a filter column.

A plurality of through holes which run through from top to bottom are correspondingly formed in the positions close to the edges of the three-level upper flange seat 2303 and the three-level lower flange seat 2306, so that the through holes penetrate through a plurality of double-end studs 2305, the two ends of each double-end stud 2305 are fixed by adopting matched nuts, and therefore the three-level filter pipe is clamped and fixed between the three-level upper flange seat 2303 and the three-level lower flange seat 2306. Further, the bottom of the third-stage upper flange seat 2303 and the top of the third-stage lower flange seat 2306 are both provided with a groove or a flange for positioning, and two ends of the third-stage filter pipe are respectively embedded into the groove or the flange, so that the fixing position of the third-stage filter pipe is ensured.

In a preferred embodiment, the third-stage filtering pipe comprises a third-stage hollow filtering column 2311 (preferably made of quartz glass) which is through from top to bottom. An annular groove is formed at the bottom of the third-stage upper flange seat 2303, the upper end of the third-stage hollow filter column 2311 is embedded into the annular groove, and an upper sealing ring 2310 (preferably a fluororubber sealing ring) is arranged between the third-stage hollow filter column and the third-stage hollow filter column; and an upper inner O-ring 2312 is clamped with the annular groove at the inner side of the upper end of the three-stage hollow filter column 2311.

A plurality of layers of three-stage filter screens 2320 are distributed in the three-stage hollow filter column 2311 along the length direction, for example, three layers are provided, and the three layers are respectively 100 meshes, 150 meshes and 250 meshes from top to bottom. The three-stage filter filtering net 2320 of each layer is clamped and fixed through a pressing ring 2313 and an inner column (preferably made of quartz glass), the pressing ring 2313 and the inner column are both in a hollow cylinder shape, the pressing ring 2313 is provided with a cylindrical wall in a protruding and extending mode at a position close to the inner side face, a blocking shoulder is formed at a position close to the outer side face, the inner column is provided with a cylindrical wall in a protruding and extending mode at a position close to the outer side face, and a blocking shoulder is formed at a position close to the inner side face, so that the two three-stage filter filtering nets 2320 are inserted in a convex-concave mode in a matched mode, and the three-stage filter filtering net 2320 is clamped in the middle. And, an O-ring 2318 of a bayonet portion is interposed between the outer side surface of the pressing ring 2313 and the inner side surface of the inner column. Specifically, for example, as shown in fig. 4B, the uppermost portion is a first extrusion ring in an inverted convex shape, the lower portion of the first extrusion ring is connected to the first inner column 2314 in a fitting manner, the upper portion of the first inner column 2314 is in a concave shape, the lower portion of the first inner column 2314 is in an inverted concave shape, the lower portion of the first inner column is connected to the second extrusion ring in a fitting manner, the lower portion of the second extrusion ring is a second inner column 2316 in an inverted concave shape, and the lowermost portion of the first extrusion ring is connected to the third extrusion ring in a convex shape; thus, the three-layer three-stage filter net 2320 is fixed at a predetermined distance. A gap O-ring 2315 is further provided between the outer side surface of each extrusion ring 2313 and/or inner column and the inner side surface of the tertiary hollow filter column 2311.

The top of tertiary lower flange seat 2306 is provided with annular flange to set up annular holding tank in the inboard face, the embedding has lower part O type sealing washer 2317 in this annular holding tank, and the lower extreme embedding of tertiary hollow filtration post 2311 is in the annular flange at tertiary lower flange seat 2306 top, and the side is inconsistent with lower part O type sealing washer 2317. A stainless steel mesh sheet 2319 (with a thickness of, for example, 1 mm) is further provided between the bottom surface of the third-stage hollow filter column 2311 and the top surface of the third-stage lower flange seat 2306.

In one embodiment, the third-stage filter 23 is a fully detachable structure and is designed in a combined manner of an upper and a lower double-cone dumbbell-shaped structures, and after assembly, a third-stage upper cavity, a third-stage filter tube and a third-stage lower cavity which are sequentially communicated from top to bottom are integrally formed. Tertiary upper portion cavity is enclosed by tertiary upper portion entry seat 2302, tertiary upper portion flange seat 2303 and the tertiary filter screen 2320 that tertiary filtration post was the top, and tertiary lower part cavity is enclosed by tertiary filter screen 2320, tertiary lower part flange seat 2306, the tertiary lower part export seat 2308 that tertiary filtration post was the bottom, and tertiary upper portion cavity and tertiary lower part cavity are bipyramid dumbbell shape cavity (for example, regular cone + cylinder + inverted cone). The structure of the middle part connecting the two double-cone dumbbell-shaped cavities is a three-stage filter tube of a reducing visual filter tube, the three-stage filter tube is provided with a series combination structure of three-stage filter screens 2320 with multiple stages (preferably three or more stages) of different screen meshes increasing gradually (preferably the filter aperture is gradually reduced), so that mercury beads containing impurities or oxide films can be squeezed to deform and rub to break the films by using pressure, the re-polymerization effect is realized, the purpose is to break the mercury soot particles, adsorbed impurities and other aggregate surface adsorption films in crude mercury, and further, the broken pure mercury aggregate units and the impurity water-containing light component system are respectively subjected to layer polymerization, and further, mercury with higher purity and high density and low density mixtures (such as mercury impurities, water and other metal oxide mixtures) are subjected to layer separation extraction and purification and impurity removal.

The operation and principle of the three-stage filter 23 are as follows. Firstly, pressurizing a system flow path, so that the high-density polymerized filtered mercury in the second-stage lower cavity of the second-stage filter 22 is extruded into the third-stage upper cavity of the third-stage filter 23, and the mercury sequentially passes through the multi-layer third-stage filter filtering net 2320 step by step to perform gradually fine membrane breaking filtration. The mercury liquid of higher purity is finally filtered into the lower tertiary chamber of the tertiary filter 23, during which floating dust, metal oxide, more fine impurities and mercury soot coated particles in the crude mercury are retained on the tertiary filter screen 2320 by the fractional membrane rupture filtration.

In addition, a reverse circulation flushing technology of the buoyancy of the deionized water is adopted in the three-stage filter 23, the deionized water is reversely pumped into a three-stage lower cavity containing the filtered mercury in the three-stage filter 23 from a three-stage filter discharge port 2309 at the bottommost part of the three-stage filter 23 by using a deionized water circulating pump 28, the deionized water can freely and reversely float and flush from bottom to top from the bottom of the three-stage lower cavity without pressure under the buoyancy effect generated by the huge density difference of the mercury, a reverse convection purification effect is formed, and the filtered mercury is further purified.

Furthermore, according to the purification quality requirement of mercury in the tertiary filter 23 and the condition of oxidized impurities, the liquid medicine pump 27 fills a trace amount of purification liquid into the tertiary filter 23 to improve the purification effect. Thus, through the processes of multi-stage extrusion membrane-breaking filtration, reverse buoyancy circulating flushing, impurity removal, purification and purification of trace purification liquid medicine and the like, crude mercury or polluted mercury is purified step by step, and finally, refined mercury with purity meeting the requirement is obtained.

The structure of luminousness detection module 41 and detection tube 37 in the multistage filter-press membrane-breaking mercury purification device is shown in fig. 5, the detection tube 37 is a vertically placed quartz glass tube, and two ends of the detection tube are respectively provided with an upper detection tube interface 371 and a lower detection tube interface 372. The light transmittance detection module 41 comprises a vertically arranged linear guide 4105, a detection tube upper end fixing support 4103 is fixedly arranged above the linear guide 4105, and a detection tube lower end fixing support 4104 is fixedly arranged below the linear guide 4105. The upper end fixing holder 4103 and the lower end fixing holder 4104 are fixed (for example, clamped) to the upper and lower ends of the detection tube 37. A detector mounting plate 4106 is slidably connected to the linear guide 4105, a light transmittance detector 4101 is mounted on the detector mounting plate 4106, and the detection position of the light transmittance detector 4101 faces the detection tube 37. Still including being used for driving the step motor 4102 that detector installation splint 4106 reciprocated to can adjust the detection position of luminousness detector 4101 to high level detection line U (being close to the detecting tube 37 top) or low level detection line D (being close to the detecting tube 37 bottom), realize that gas water mercury three-phase detects.

The operation and principle of the transmittance detection module 41 and the detection tube 37 are as follows. A static gas-water-mercury three-phase detection state interface is established in the detection tube 37, the light transmittance detection module 41 is controlled and adjusted, the light transmittance detector 4101 is used for detecting the water phase cleanliness, namely the light transmittance, in the detection tube 37 at a reasonable detection state position, the deionized water phase light transmittance value when the mercury purity reaches the standard is used as an end condition for confirming that the purification of the circulating filtration mercury reaches the standard, the mercury purification at normal temperature reaches the standard and is recycled, and meanwhile, in the mercury purification process, the external sewage is subjected to mercury removal purification standard reaching treatment to meet the requirement of the environmental protection discharge standard.

On the other hand, luminousness detection module 41 still plays the effect of judging wherein smart mercury's volume at smart mercury filling in-process to control smart mercury filling control solenoid valve 17 and close when smart mercury is about to the earial drainage to finish, guarantee that the water of smart mercury top can not get into smart mercury receiving flask 36. The basic principle is that the light transmittance detection module 41 is adjusted to a low detection line D to emit detection light for detection, and if the mercury column completely shields the detection light, the light transmittance is basically 0; when the light transmittance is greater than 50, even close to 100, it indicates that the mercury-water interface is at or below the detection point, and this can be used as the condition for ending the filling action.

In addition, in the preferred embodiment, the volumes of the two-stage upper cavity and the two-stage lower cavity of the two-stage filter 22 and the three-stage upper cavity and the three-stage lower cavity of the three-stage filter 23 are substantially equal to each other, and equal to or slightly larger than the volume of the crude mercury added to the crude mercury bottle 35 in one purification process. Therefore, the crude mercury in the crude mercury bottle 35 is completely filtered to the second-level lower cavity and then completely filtered to the third-level lower cavity, the upper scale mark of the mercury does not exceed the height range of the second-level and third-level lower cavities, and the filtering process can be completed through the pressurization process and the volume-fixing process control. And when the mercury is pressed from the second-stage lower cavity to the third-stage upper cavity, even if the mercury in the third-stage upper cavity is not filtered through the third-stage filter pipe under pressure at the beginning, the mercury does not overflow from the upper outlet 2321 of the third-stage filter during the pressurization driving in the period, and only water, gas or impurity floating dust is extruded from the upper outlet 2321 of the third-stage filter and flows through the top cleaning electromagnetic valve 12 of the third-stage filter, the discharge circulation switching electromagnetic valve 19, the outlet sewage bottle 40, the sewage discharge mercury removal filter 25 and the sewage discharge electromagnetic valve 20 for discharge.

The volume of the detection tube 37 is preferably smaller than the volume of the crude mercury added into the crude mercury bottle 35, so that when the mercury outlet electromagnetic valve 13 of the three-stage filter is opened, the three-stage filter 23 and the detection tube 37 form a communicating vessel structure, the mercury water interface is kept consistent, and the mercury water interface in the lower cavity of the three stages cannot be greatly reduced due to the formation of the communicating vessel because the detection tube 37 is a small-volume thin tube. And, when the fine mercury is filled, mercury can be easily and rapidly discharged to the fine mercury collecting bottle 36 under the action of gravity, and it is required to ensure that the discharge process is not too rapid, otherwise, controllable filling and detection are not easy to realize. Therefore, the detection tube 37 adopts a small-volume thin tube, and the detection of the mercury-water interface level and the light transmittance of the aqueous solution in the detection tube 37 through the light transmittance detection module 41 is facilitated, so that controllable automatic filling can be realized.

The structure of the filter is shown in fig. 6, and the filter comprises a hollow mercury-removing filter tube 243 (preferably, a double-end threaded quartz glass tube), wherein mercury-removing resin 242 is contained, two ends of the mercury-removing filter tube 243 are respectively provided with a mercury-removing filter inlet sealing end cover 241 and a mercury-removing filter outlet sealing end cover 244, and the mercury-removing filter inlet sealing end cover 241 and the mercury-removing filter outlet sealing end cover 244 are both provided with through interfaces, so that wastewater can enter the mercury-removing filter tube from the interface of the mercury-removing filter inlet sealing end cover 241, is purified by the mercury-removing resin 242, and is discharged from the interface of the mercury-removing filter outlet sealing end cover 244. The mercury removal resin is also called ion exchange resin and is used for adsorbing mercury and heavy metals, CH-97 type renewable mercury removal resin is preferably adopted, and the mercury removal resin loaded with mercury after being used can be regenerated by mercury recovery enterprises and then put into use again. In the laboratory mercury purification process, CH-97 type mercury removal resin is filled in a quartz tube to remove and purify trace mercury, so that the environmental protection and safety can be ensured to reach the standard.

The part of the multistage filter-pressing membrane-breaking mercury purification device for controlling the work of each element preferably adopts a PLC (programmable logic controller) electric automatic control system, is provided with PLC control software and is connected with a touch screen for operation. The control system realizes the manual operation and the automatic programming operation of 20 electromagnetic valves on a touch screen of a PLC (programmable logic controller) electrical automatic control system, realizes the start and stop control of one nitrogen generator 29, controls the programming and parameter acquisition of three pumps (comprising a sample injection pressurizing pump 26, a liquid medicine pump 27 and a deionized water circulating pump 28) according to the process requirements by utilizing PLC control software (preferably, PLC support software) in the system, and performs the program setting control and the detection data acquisition and storage of detection positions in three pressure sensors (comprising an inlet pressure sensor 31, a middle pressure sensor 32 and an outlet pressure sensor 33) and a light transmittance detection module 41. The PLC control software program is programmed according to the process flow sequence and the operation requirements, and the functions of automatically controlling the whole series of work flows from the pulsating pressure balance adjustment of the nitrogen generator 29, the mercury injection of the coarse mercury bottle 35, the mercury injection and filtration of the secondary filter 22, the mercury injection of the tertiary filter 23, the cleaning and circulating cleaning, the dosing, the recycling cleaning, the mercury cleanliness detection and the automatic sub-packaging of the refined mercury to the end are realized.

In the multi-stage filter-pressing membrane-breaking mercury purification device, all the following steps can be automatically completed by a PLC (programmable logic controller) electric automatic control system or manually controlled except that manual operation is required for device assembly, shutdown maintenance and the like. All the mentioned parameters can be input and set in the PLC electrical automation control system, only recommended values are given below, and the optimization and the adjustment can be specifically carried out according to actual conditions.

In addition, the detailed working process of the multistage filter-pressing membrane-breaking mercury purification device is as follows:

first, preparation is carried out, and control connection building of each component is carried out according to the layout shown in fig. 1. The connecting pipeline can adopt a Teflon pipeline with the diameter of 6 multiplied by 9mm or the diameter of 5 multiplied by 7mm, the connecting line can adopt a Teflon straight pipe joint or a right-angle joint for connection, the three-line junction can adopt a matched Teflon three-way joint for connection, and the four-line junction can adopt a matched Teflon four-way joint for connection. The operation is not described in detail according to the flow connection specification. And, the cleaning chemical solution (preferably chemical cleaning solution) is added to the cleaning chemical solution bottle 38, and the deionized water is added to the deionized water bottle 39.

Step S1, pressure level checking: the nitrogen generator 29 is correctly preset to start, regulating the output pressure to 0.6MPa. The method comprises the following steps of powering off a nitrogen source inlet control electromagnetic valve 1 and a buffer tank outlet electromagnetic valve 2, placing the valves in a normally closed state, starting an automatic pressure regulating program of a PLC (programmable logic controller) electric automation control system, collecting pressure P1 measured by an inlet pressure sensor 31, opening the nitrogen source inlet control electromagnetic valve 1 if the pressure P1 is less than or equal to 0.3MPa, communicating the inlet pressure sensor 31 with an output pipeline of a nitrogen generator 29, starting the nitrogen generator 29 to operate, not performing action if the pressure P1 is greater than 0.3MPa, and continuing collection and monitoring until the measured pressure P1 is less than or equal to 0.3MPa; subsequently, as the nitrogen generator 29 pressurizes the low pressure nitrogen buffer tank 34, P1 is gradually increased, and when P1 is equal to or greater than 0.55MPa, the nitrogen source inlet control solenoid valve 1 is closed and the nitrogen generator 29 is closed. The process is automatically monitored and controlled by a PLC electric automatic control system in the whole process, so that the working pressure range of the low-pressure nitrogen buffer tank 34 is basically kept between 0.3MPa and 0.55 MPa.

Step S2, adding crude mercury to the crude mercury bottle 35: if the crude mercury is filled manually, the touch screen can be clicked manually to open the gas-liquid vent electromagnetic valve 3, an external vent pipe at the front end of the electromagnetic valve and an external crude mercury container are connected, and the crude mercury in the external waste mercury container is filled into the crude mercury bottle 35 by utilizing a potential difference or a funnel; if the electric filling is adopted, a touch screen 'electric filling' function button can be manually clicked, the situation that the electromagnetic valve 2 at the outlet of the buffer tank and the electromagnetic valve 3 at the gas-liquid vent are powered off and are in a closed state is confirmed, the electromagnetic valve 5 is isolated in a flow process and powered on and is in a closed state, then a sample inlet pipe at the input end of the sample inlet pressurizing pump 26 is inserted into an external crude mercury container, the rotating speed, the flow and the volume parameters of the sample inlet pressurizing pump 26 are set, the electromagnetic valve 4 for controlling the crude mercury feeding is powered on and is placed in an open state, the sample inlet pressurizing pump 26 is started, and crude mercury is filled into the crude mercury bottle 35. The filled crude mercury is for example about 1000-1500 grams.

And S3, performing a pressure filtration process of the secondary filter: the PLC electric automation control system operates a nitrogen source electromagnetic valve 1, a buffer tank outlet electromagnetic valve 2, a gas-liquid vent electromagnetic valve 3, a crude mercury charging control electromagnetic valve 4, a flow isolating electromagnetic valve 5, a filtering and flushing bypass electromagnetic valve 8, a secondary filter isolating electromagnetic valve 9, a tertiary filter inlet electromagnetic valve 11, a tertiary filter top cleaning electromagnetic valve 12 and a discharge circulation conversion electromagnetic valve 19 to be in a closed (cut-off) state; the coarse mercury outlet electromagnetic valve 6, the pre-filter column outlet electromagnetic valve 7, the secondary filter flushing control electromagnetic valve 10 and the sewage discharge electromagnetic valve 20 are in an open (conducted) state; after the flow path on-off state is ensured to be correct through a self-checking program of a PLC electric automatic control system or manually observing the working state of each electromagnetic valve displayed on a display screen, starting a vortex oscillator 30, opening an outlet electromagnetic valve 2 of a buffer tank, and performing a secondary filter pressurization filtering process; the PLC electric automation control system calls a pressure comparison condition judgment sub-program, when the difference value of the pressure P1 of the inlet pressure sensor 31 and the pressure P2 of the intermediate pressure sensor 32, namely P1-P2 is not more than the pressure head difference dPh when the filtering is finished, and the pressurizing and filtering time Tosc of the secondary filter is more than 60s or longer, the electromagnetic valve 2 at the outlet of the buffer tank is closed, the vortex oscillator 30 is continuously kept to run in an oscillating mode, and the operation is finished according to the oscillator timing parameters (the oscillator timing parameters can be generally selected within 120s-600s, for example, the oscillator timing parameters are set to be 120s, and the PLC program controls the vortex oscillator 30 to be closed after the Tosc reaches 120 s), so that the oscillating and filtering processes of the coarse mercury vibrating screen are finished.

The pressure head difference dPh after filtration is a self-defined parameter and can be determined through experiments or calculation. The specific explanation is as follows. A horizontal plane tangent to the bottom of the secondary lower cavity of the secondary filter 22 is set as a reference plane of a pressure head (also called a pressure head), P1-P2 is the difference between the pressure head of the inlet pressure sensor 31 and the pressure point of the middle pressure sensor 32, the difference between the pressure heads is the difference between the installation height position pressure difference and the friction resistance pressure difference, and the difference between the total pressure heads of two points generated by the height change of mercury columns in each pipeline in the direction perpendicular to the reference plane of the pipeline in the filling process of the secondary lower cavity of the secondary filter 22, and according to an energy conservation equation, the P1-P2 in the system presents low, high and low approximate single pulse square wave shape characteristics along with a pressurizing filtering time interval. In this example, P1-P2 ≈ 0.050MPa at about 6s after the start of pressure filtration; when the pressure is about 7s-60s, P1-P2 is approximately equal to 0.105MPa; after about 60s, P1-P2 is approximately equal to 0.042MPa; this feature can be used to determine the end condition of the two-stage filter pressure filtration process. For this embodiment, the head difference dPh at the completion of filtration may be set to, for example, 0.05MPa, and when the secondary filter pressure filtration time Tosc acquired by the PLC program is greater than 65s and P1-P2 < dPh, it may be determined that the pressure filtration of the secondary filter 22 is completed.

And S4, carrying out a filtering process of a three-stage filter: firstly, ensuring that a nitrogen source electromagnetic valve 1, a buffer tank outlet electromagnetic valve 2, a gas-liquid vent electromagnetic valve 3, a crude mercury feeding control electromagnetic valve 4, a flow isolation electromagnetic valve 5, a filtering and flushing bypass electromagnetic valve 8, a secondary filter isolation electromagnetic valve 9, a tertiary filter inlet electromagnetic valve 11, a tertiary filter top cleaning electromagnetic valve 12, a tertiary filter mercury outlet electromagnetic valve 13, a detection pipe top isolation electromagnetic valve 14, a liquid medicine pump outlet electromagnetic valve 15, a deionized water circulating pump outlet electromagnetic valve 16, a fine mercury filling control electromagnetic valve 17, a deionized water return liquid inlet electromagnetic valve 18 and a discharge circulation conversion electromagnetic valve 19 are in a closed (cut-off) state in an initial state; the crude mercury outlet electromagnetic valve 6, the pre-filter column outlet electromagnetic valve 7, the secondary filter flushing control electromagnetic valve 10 and the sewage discharge electromagnetic valve 20 are in an open (conducted) state; then an inlet electromagnetic valve 11 of the tertiary filter, a top cleaning electromagnetic valve 12 of the tertiary filter and a discharge circulation conversion electromagnetic valve 19 are opened, a flushing control electromagnetic valve 10 of the secondary filter is closed, the system flow path is continuously pressurized, filtered mercury polymerized at high density at the bottom of the secondary filter 22 is extruded into the tertiary filter 23, and finally the filtered mercury enters a lower cavity of the tertiary filter.

Specifically, for example, the system flow path is continuously pressurized for a period of time (e.g., 60 seconds), mercury filtered by the secondary lower cavity of the secondary filter 22 is forced to flow along the path through the tertiary filter inlet solenoid valve 11 and all into the tertiary upper cavity of the tertiary filter 23; then closing a top cleaning electromagnetic valve 12 of the tertiary filter, opening a mercury outlet electromagnetic valve 13 of the tertiary filter and a top isolation electromagnetic valve 14 of the detection pipe, and continuing pressurization, wherein at the moment, mercury in the upper cavity of the tertiary filter can only be filtered along the tertiary filter pipe, and finally enters the lower cavity of the tertiary filter, and further enters a detection pipe 37 through the electromagnetic valve 13; the detection position of the light transmittance detection module 41 is placed in a high detection line U of the detection tube 37 for detection, along with the gradual rise of the mercury liquid level in the detection tube 37, the fluid at the position of the high detection line U is converted into mercury from air or waste water on the upper layer of crude mercury, and the light transmittance detection value is changed from a high-value (generally more than 60 percent) casting to be close to 0 (the detection point is completely blocked by mercury); therefore, a first light transmittance reference value lt0 is set, the range of the first light transmittance reference value is a meaningful range of light transmittance, the value is generally 0-99.5%, for example, 60%, and the first light transmittance reference value can be flexibly selected according to needs; when the detection value of the light transmittance detection module 41 is less than or equal to the first light transmittance reference value lt0, it indicates that the mercury liquid level is located near the high detection line U, and further indicates that all mercury is filtered and enters the three-level lower cavity, so that the PLC electric automatic control system can serve as a finishing condition to stop the pressurizing and filtering process of the three-level filter.

Step S5, deionized water rinsing of mercury is performed in the tertiary filter 23: closing an inlet electromagnetic valve 11 of the three-stage filter, a top isolation electromagnetic valve 14 of the detection pipe, an outlet electromagnetic valve 15 of the liquid medicine pump and a fine mercury filling control electromagnetic valve 17, and then opening a top cleaning electromagnetic valve 12 of the three-stage filter, a mercury outlet electromagnetic valve 13 of the three-stage filter, an outlet electromagnetic valve 16 of the deionized water circulating pump and a discharge circulation conversion electromagnetic valve 19; next, the deionized water circulating pump 28 is opened, a first operating flow speed V1 of the deionized water circulating pump 28 is set (specific values can be selected in the working condition of the pump), deionized water (and mercury is pushed) enters from a discharge port 2309 of the tertiary filter, and then reversely passes through the tertiary filter 23, the tertiary filter top cleaning electromagnetic valve 12, the discharge circulation conversion electromagnetic valve 19, the outlet sewage bottle 40, the sewage discharge mercury removal filter 25 and the sewage discharge electromagnetic valve 20 to be discharged, so that low-density scum impurities on the water surface at the top of mercury in the tertiary filter 23 are cleaned and washed, and the washing time T1 (the washing time T1 is a time parameter input into the PLC electrical automatic control system, and the specific values can be set as required, for example, 60s-90s can be generally taken); after the rinsing is finished, the deionized water circulation pump 28 is turned off.

Further, the three-stage filter 23 is subjected to deionized water reverse buoyancy circulation washing: the discharge circulation switching solenoid valve 19 is closed and the deionized water return inlet solenoid valve 18 is opened. Opening the deionized water circulating pump 28 again, setting a second running flow speed V2 (specific value can be selected in the working condition of the pump), starting closed-loop circulating flushing of the tertiary filter 23, after the deionized water is pumped out by the deionized water circulating pump 28, sequentially passing through the deionized water circulating pump outlet electromagnetic valve 16, the outlet pressure sensor 33, the detection pipe 37, the tertiary filter mercury outlet electromagnetic valve 13, the tertiary filter 23, the tertiary filter top cleaning electromagnetic valve 12, the deionized water circulating mercury removal filter 24 and the deionized water return liquid inlet electromagnetic valve 18, and returning to the deionized water bottle 39 to form a deionized water mercury washing continuous circulating flushing loop; setting the circulating flushing time T2 (the specific value can be set according to the requirement, for example, 300-600 s can be taken generally); after the rinsing sequence is complete, the deionized water circulation pump 28 is turned off.

Step S6, adding a purifying liquid medicine to perform chemical purification circulation: closing an inlet electromagnetic valve 11 of the three-stage filter, a top isolation electromagnetic valve 14 of the detection pipe, an outlet electromagnetic valve 16 of the deionized water circulating pump and a fine mercury filling control electromagnetic valve 17, opening a top cleaning electromagnetic valve 12 of the three-stage filter, a mercury outlet electromagnetic valve 13 of the three-stage filter, an outlet electromagnetic valve 15 of the liquid medicine pump and a discharge circulation conversion electromagnetic valve 19, opening a liquid medicine pump 27, setting the speed and the volume of the pump, setting the pump parameters to be constant-volume CV3 operation (the value range of the volume CV3 can be 0-50 ml), and enabling the purified liquid medicine to enter the three-stage filter 23 through the detection pipe 37; and after the constant volume CV3 is reached, the liquid medicine pump 27 is closed, and the electromagnetic valve 15 of the liquid medicine pump outlet is closed.

Further, the outlet electromagnetic valve 16 of the deionized water circulating pump is opened, the deionized water circulating pump 28 is opened, and the three-stage filter 23 is subjected to secondary circulating deionized water washing: closing the discharge circulation conversion electromagnetic valve 19, opening the deionized water return inlet electromagnetic valve 18, opening the deionized water circulating pump 28, starting closed-loop washing of the tertiary filter 23 at a set third flow rate V3 (the specific value can be selected in the working condition of the pump), and setting secondary circulation washing time T3 (the value can be 300 s).

Further, the deionized water circulating pump 28 is closed after the above-mentioned long-term circulation of T3 is completed, the detection tube 37 and the three-stage lower chamber form a communicating vessel, mercury enters the detection tube 37 through the three-stage filter mercury outlet electromagnetic valve 13, the mercury water interface of the three-stage lower chamber is level with the mercury water interface in the detection tube 37, and mercury does not enter a subsequent flow pipeline above the detection tube 37, but forms a relatively stable mercury water interface for light transmittance detection. But the deionized water circulating liquid above the mercury-water interface can continuously pass through the outlet pressure sensor 33, the detection tube top isolation electromagnetic valve 14, the discharge circulation conversion electromagnetic valve 19, the outlet sewage bottle 40, the sewage discharge mercury removal filter 25 and the sewage discharge electromagnetic valve 20 to form a flushing cleaning flow path.

Step S7, detecting whether the mercury purification reaches the standard: the detection position of the light transmittance detection module 41 is arranged on the high-position detection line U for light transmittance detection, and if the light transmittance detection value is not less than the second light transmittance standard value ltu, the purification standard value is indicated. ltu is the second transmittance standard value, which corresponds to the transmittance standard value when the purity of the purified mercury is satisfied after the crude mercury is finally filtered, washed and purified, and the highest allowable content of the impurities in the deionized water circulating liquid is satisfied when the purity of the mercury is satisfied as specified in the laboratory pressure curve of capillary tube, GB/T2650.1-2008, and the second transmittance standard value ltu specifically sets the range according to the corresponding relationship between the deionized water washing pollution degree standard value and the mercury purification standard reaching cleanliness of 99.5%, wherein the range is a meaningful range, for example, the value is taken in the range of 50% -99.5% according to the actual sample condition, and the transmittance detection value is not less than ltu, which indicates that the mercury purity is up to the standard (the purity is more than 99.9%), thereby completing the mercury purification process. If the light transmittance detection value is less than the second light transmittance standard value ltu, the (deionized water reverse) closed-loop flushing of the three-stage filter 23 is repeated, the three-stage filter is stopped after a period of time, mercury enters the detection tube 37 to form a communicating vessel, light transmittance detection is carried out, and the steps are repeated until the light transmittance detection value reaches the standard.

For example, in a 20# series crude mercury sample purification experiment, after filtering through the third filter 23 and four times of circulating washing, the transmittance values of circulating washing liquid of the detection tube corresponding to 8 samples are 65.3%, 68.2%, 71.3%, 73.2%, 75.8%, 76.9%, 77.3% and 78.8%, respectively, and the purities of mercury of the corresponding samples tested by the method are 99.48%, 99.56%, 99.72%, 99.85%, 99.93%, 99.95%, 99.96% and 99.96% in sequence. The transmittance value corresponding to the mercury purity of 99.93 percent is selected to be 75.8 percent through the preliminary evaluation of the sample experiment, the second transmittance standard value ltu is set to be 75.8 percent, and the transmittance is used as the lower limit value for judging the mercury treatment standard reaching under the working condition. The ltu value is influenced by the sectional shape and characteristics of the glass tube of the detection tube 37 and the composition of impurity particles and dust in a processed sample to a certain extent, a more complete classification and identification mode is gradually formed by continuously enriching sample experiments, and the second light transmittance is optimized to reach the selection of a standard value ltu.

Step S8, taking out and subpackaging mercury: placing the light transmittance detection module 41 in a low-level detection line D for light transmittance detection, opening the top cleaning solenoid valve 12 of the tertiary filter, the mercury outlet solenoid valve 13 of the tertiary filter, the discharge cycle switching solenoid valve 19 and the sewage discharge solenoid valve 20, and intermittently opening and closing the fine mercury filling control solenoid valve 17 in a pulsating manner (the time interval of intermittent opening and closing can be 3 levels, dt1, dt2 and dt3, generally dt 1> dt2 > dt3, preferably dt1=300ms, dt2=200ms, dt3=50ms, or selected according to conditions, the range is 0ms-500000 ms), and simultaneously setting the filling intermittent on-off cycle (closing the fine mercury control solenoid valve 17) of the fine mercury filling control solenoid valve 17 when the detection position of the light transmittance detection module 41 is at the low-level detection line D, and when the light transmittance detection value is greater than or equal to the light transmittance value (namely the water-mercury interface has dropped to the lowest allowable control interface, the light transmittance value is the third light transmittance value, which is generally recommended to be set to be 30), ending the filling process of the fine mercury. In short, PLC control software is adopted to automatically control the intermittent opening and closing of the fine mercury filling control electromagnetic valve 17, the opening and closing interval time window is gradually narrowed, meanwhile, the light transmittance of the mercury water interface is detected through the light transmittance, and the condition that the light transmittance threshold value is reached is used as the finishing condition for finishing the fine mercury filling.

The specific process is as follows. Opening the fine mercury filling control electromagnetic valve 17, draining mercury to the fine mercury collecting bottle 36 by means of gravity, closing the fine mercury filling control electromagnetic valve 17 after a duration dt1 (for example, 300 ms), setting the light transmittance detection module 41 at the position of the low-position detection line D, detecting the light transmittance at the bottom of the detection tube 37, and if the light transmittance detection value is approximately equal to 0 (for example, between 0% and 2%), indicating that the detection point is completely shielded by mercury, continuously repeating the above-mentioned intermittent opening and closing with the duration dt1, and detecting the light transmittance when the detection point is closed; and (3) entering a second stage, continuously and intermittently opening and closing the fine mercury filling control electromagnetic valve 17 repeatedly and intermittently until the light transmittance detection value is larger than or equal to ltd1 (for example, 10%), but the duration time of each opening is shortened to dt2 (for example, 200 ms), the light transmittance is detected when the fine mercury filling control electromagnetic valve is closed, entering a third stage, continuously and intermittently opening and closing the fine mercury filling control electromagnetic valve 17 repeatedly and intermittently when the light transmittance detection value is larger than or equal to ltd2 (for example, 30%), but the duration time of each opening is further shortened to dt3 (for example, 50 ms), the light transmittance is detected when the fine mercury filling control electromagnetic valve is closed, and when the light transmittance detection value is larger than or equal to ltd3 (for example, 50), the mercury interface is positioned at the center of the detection point or below the center of the detection point, the fine mercury is basically and completely leaked to the fine mercury collecting bottle 36, so that the fine mercury filling control electromagnetic valve 17 is not opened, and the filling process is ended. This process realizes control and detects mercury water interface, prevents that the quick earial drainage in-process water of mercury from leaking and flowing to smart mercury collecting bottle 36: when the filling process is just started, because the mercury-water interface is higher, the detection is stopped after the leakage flow is allowed to be carried out for a relatively long time, and therefore, the long-time interval and the small light transmittance value are matched; along with the reduction of the mercury-water interface, the limitation is gradually carried out by adopting short time intervals and large light transmittance values, so that the filling can be more quickly confirmed and stopped when the mercury-water interface is close to the lower line allowed by filling.

And S9, cleaning and initializing the device: resetting the light transmittance detection module 41 to the position of the low detection line D, and checking the cleaning state of the device; and then operating the PLC electrical automation control system to turn off the power supply of the device, stopping supplying power to each electromagnetic valve and each pump, turning off or waiting each part of the device, finishing all work, and performing sorting, storage and other cleaning work according to operation rules.

When the cleaning state of the device is checked, if the pre-filtering column 21 is found to be seriously polluted by visual inspection, the pre-filtering column 21 can be detached for cleaning or replacement, the pre-filtering column 21 adopted by the invention is a high-temperature reproducible filtering column, when the pollution is serious, each part can be detached, and the pre-filtering column filtering tube 214 (quartz tube) and the high-temperature resistant glass fiber and the quartz sand/quartz glass ball filled in the pre-filtering column filtering tube are put into a high-temperature armor tube furnace mercury extraction device together for high-temperature reproducible treatment; or, the pre-filter column flushing path of the device can be adopted, and the back flushing cleaning is carried out by using deionized water, specifically, the flow isolation solenoid valve 5, the crude mercury outlet solenoid valve 6, the filtration flushing bypass solenoid valve 8, the secondary filter flushing control solenoid valve 10, the tertiary filter top cleaning solenoid valve 12, the detection tube top isolation solenoid valve 14, the liquid medicine pump outlet solenoid valve 15, the fine mercury filling control solenoid valve 17 and the discharge circulation conversion solenoid valve 19 are placed in a stop state, the deionized water circulation pump outlet solenoid valve 16, the tertiary filter mercury outlet solenoid valve 13, the tertiary filter inlet solenoid valve 11, the pre-filter column outlet solenoid valve 7, the secondary filter isolation solenoid valve 9 and the sewage discharge solenoid valve 20 are placed in an open state, the deionized water circulation pump 28 is opened, and a passage is formed by sequentially passing through the opened solenoid valves from the deionized water circulation pump 28 for flushing.

If the secondary filter 22 and the tertiary filter 23 are seriously polluted by visual inspection, an automatic flushing flow path program set in a PLC (programmable logic controller) electrical automation control system can be selected in a corresponding interface on the touch screen, or a flow path design is carried out on an electromagnetic valve at a corresponding position set on the touch screen through manual operation to form a flushing sewage discharge path, the deionized water circulating pump 28 is used for flushing and cleaning the secondary filter 22 and/or the tertiary filter 23, and the flushing sewage flows through the outlet sewage bottle 40 and the sewage discharge mercury removal filter 25 for mercury removal and purification, so that the environment-friendly standard reaching of the discharge sewage is ensured.

For example, the flush path of the secondary filter 22 may be set to: the process isolation electromagnetic valve 5, the crude mercury outlet electromagnetic valve 6, the pre-filter column outlet electromagnetic valve 7, the filtration flushing bypass electromagnetic valve 8, the secondary filter isolation electromagnetic valve 9, the tertiary filter top cleaning electromagnetic valve 12, the detection tube top isolation electromagnetic valve 14, the liquid medicine pump outlet electromagnetic valve 15, the fine mercury filling control electromagnetic valve 17 and the discharge circulation conversion electromagnetic valve 19 are in a cut-off state, the deionized water circulating pump outlet electromagnetic valve 16, the tertiary filter mercury outlet electromagnetic valve 13, the tertiary filter inlet electromagnetic valve 11, the secondary filter flushing control electromagnetic valve 10 and the sewage discharge electromagnetic valve 20 are in an open state, and a passage is formed by sequentially passing through the opened electromagnetic valves from the deionized water circulating pump 28 for flushing.

For another example, the flush path of the tertiary filter 23 may be set to: the two-stage filter isolation electromagnetic valve 9, the two-stage filter flushing control electromagnetic valve 10, the three-stage filter inlet electromagnetic valve 11, the detection tube top isolation electromagnetic valve 14, the liquid medicine pump outlet electromagnetic valve 15, the fine mercury filling control electromagnetic valve 17 and the deionized water return inlet electromagnetic valve 18 are in a stop state, the deionized water circulating pump outlet electromagnetic valve 16, the three-stage filter mercury outlet electromagnetic valve 13, the three-stage filter top cleaning electromagnetic valve 12, the discharge circulation conversion electromagnetic valve 19 and the sewage discharge electromagnetic valve 20 are in an open state, and a passage is formed by sequentially passing through the opened electromagnetic valves from the deionized water circulating pump 28 for flushing.

In addition, a small circulation loop can be formed along the outlet electromagnetic valve 16 of the deionized water circulating pump, the top isolation electromagnetic valve 14 of the valve detection tube, the deionized water circulating mercury removal filter 24, the deionized water liquid return inlet electromagnetic valve 18 and the deionized water tank 39, so that the functions of cleaning the upper part of the detection tube 37 and washing, overhauling and testing the deionized water circulating mercury removal filter 24 are realized.

On the basis of the above embodiment, a multistage filter-press membrane-breaking mercury purification device is provided according to fig. 4A and 4B, and is a multistage visual filter which uses multistage filter-press membrane-breaking and deionized water buoyancy reverse circulation flushing and trace chemical reagent oxide impurity removal purification technology, and experimental filtering conditions for specific crude mercury working conditions can be optimized by adopting mesh screen combinations with different mesh numbers in the filter, so that a mixed liquid phase system consisting of impurity oxides and dust particles in mercury with mercury purity of 99.5% or less can be filtered, membrane-breaking, purified and purified under normal temperature conditions. The multi-stage filter-pressing membrane-breaking mercury purification device comprises an upper cavity, a middle part and a lower cavity which are connected in a combined manner, wherein the upper cavity and the lower cavity are of inner cavity structures which are same in size and are conical at two ends of a middle cylinder, the middle part is a reducing multi-stage filtering visual tube, the whole structure is in a dumbbell shape vertically arranged from top to bottom, and waste mercury liquid enters from an inlet at the top end of the upper cavity and flows out from an outlet at the bottom of the lower cavity; the upper cavity body comprises a three-level upper inlet seat and a three-level upper flange seat which are hermetically connected up and down, the inner cavity of the three-level upper inlet seat is in an inverted cylindrical funnel shape, the inner cavity of the three-level upper flange seat is in a conical funnel shape, and the calibers of the inner cavities of the three-level upper inlet seat and the three-level upper flange seat are the same; the lower cavity comprises a third-level lower flange seat and a third-level lower outlet seat which are hermetically connected up and down, the inner cavity of the third-level lower flange seat is an inverted conical funnel, the inner cavity of the third-level lower outlet seat is in a cylindrical funnel shape, and the calibers of the inner cavities of the upper cavity and the lower cavity are the same; the middle part is a necking cylindrical quartz glass three-stage hollow filter column, and a plurality of homocircular filter screens with different holes are arranged in the middle part; the periphery of the filter screen is hermetically connected with a three-stage hollow filter column, and the three-stage hollow filter column is connected with the inner cavity of the upper and lower flange bases.

Preferably, the three-stage hollow filter column comprises a first inner column and a second inner column which are made of quartz glass materials, the first inner column and the second inner column are both in a hollow cylinder shape, the bottom area of the first inner column is the same as that of the second inner column, and the first inner column and the second inner column are in sealing connection through a flange and a sealing gasket; the first inner column is internally and hermetically connected with a first-stage filter screen and a second-stage filter screen which are in equal circles with the first inner column; the second inner column is internally and hermetically connected with a third-level filter screen which is in an equal circle with the second inner column and a stainless steel mesh sheet at the bottom; the top end of the first inner column is hermetically connected with the bottom end of the inner cavity of the three-level upper flange seat, the bottom end of the second inner column is connected with the top end of the inner cavity of the three-level lower flange seat, and all the joints are provided with sealing rings for sealing connection; the three-stage hollow filter column is respectively connected with the upper flange seat and the lower flange seat. The first inner column is provided with 100 meshes, a 160-mesh filter screen is arranged below the first inner column, and the second inner column is provided with a 200-mesh filter screen or other mesh combination schemes are optimally combined according to the requirement of filter precision. And extrusion rings are respectively arranged at the positions of the filter screens between the three-stage hollow filter columns and the inner column. The inlet end at the top of the inner cavity of the upper inlet seat at the third stage is connected with a quick connector for filling nitrogen; the outlet end of the bottom of the inner cavity of the third-level lower outlet seat is connected with a quick connector for connecting a deionized water pipe, and the deionized water pipe is connected with a circulating pump, so that deionized water is pumped into the inner cavity of the third-level lower outlet seat, and the inner cavity of the device is repeatedly washed from bottom to top.

Further, in another preferred embodiment, the upper end and the lower end of the overall structure of the multistage filter-pressing membrane-breaking mercury purification device are designed by adopting a dumbbell-like structure, namely a cone and cylindrical cone combined inner cavity, the middle of the overall structure is connected by adopting a reducing-hole multistage filtering visible tube in a combined manner, and the structure is a dumbbell structure vertically arranged up and down; waste mercury liquid flows in from the top of the upper end and flows out from an outlet at the lower end, and the outlet at the lower end is connected with a deionized water pipe and a circulating pump; the multi-stage membrane breaking purification, the buoyancy reverse circulation flushing filtration and the layered extraction purification can be realized by controlling the gravity difference and the flow direction of the system pressure and the fluid with different densities in the process, so that the normal-temperature physical separation and purification function of a mercury-impurity oxide membrane-water ternary combination system is realized, and the advantages of environmental protection, safety and reliability are realized.

The upper end of the multistage filter-pressing membrane-breaking mercury purification device can be connected with a filter press or a pressure source to provide pressure input. The multistage filter-pressing membrane-breaking mercury purification device comprises an upper cavity, a middle necking quartz tube and a lower cavity from top to bottom. The upper chamber body includes tertiary upper portion entry seat and tertiary upper portion flange seat, and tertiary upper portion entry seat inner chamber is for invering cylindrical funnel shape, and tertiary upper portion flange seat inner chamber is for the toper hourglass hopper-shaped, and both inner chamber bores are the same. The third-level upper inlet seat is positioned on the third-level upper flange seat, and the inner cavities of the third-level upper inlet seat and the third-level upper flange seat are butted. And a third O-shaped sealing ring larger than the inner cavity is arranged between the third-level upper inlet seat and the third-level upper flange seat, and the third O-shaped sealing ring are hermetically connected through screws and nuts. The inverted cone-shaped cylindrical design of the three-level upper inlet seat can reduce the adsorption of mercury beads and maximize the internal storage. The tertiary upper inlet seat and the tertiary upper flange seat form a compact shape, and the upper half part of the sealed mercury collecting cavity is formed. The toper design of tertiary upper portion flange seat, natural transition reduces inside mercury pearl and adsorbs, and the flange formula design can bear higher pressure, the harmless dismouting of being convenient for simultaneously. The lower cavity is the same as the upper cavity in volume, the lower cavity comprises a third-level lower flange seat and a third-level lower outlet seat, the third-level lower flange seat is the same as the third-level upper flange seat in size and opposite in direction, the third-level lower outlet seat is the same as the third-level upper inlet seat in size and opposite in direction, the third-level lower flange seat is arranged on the third-level lower outlet seat, and a fourth O-shaped sealing ring 7 larger than the inner cavity is arranged between the third-level lower flange seat and the third-level lower outlet seat and is in sealing connection with the upper cavity through screws and nuts.

Stud bolts are symmetrically connected to two sides of the three-level upper flange seat and the three-level lower flange seat. The upper and lower joints are connected through nuts and screws. The middle quartz column is positioned in the double-ended stud. The three-level upper flange seat, the stud and the three-level lower flange seat form a compaction shape, the upper part and the lower part are extruded and sealed, the middle part is firmly fixed, and the whole device is integrated. The inlet end at the top of the inner cavity of the upper inlet seat at the third stage is connected with a quick connector, and high-purity nitrogen can be filled for generating protective gas inside the cavity; the outlet end of the bottom of the inner cavity of the third-level lower outlet seat is connected with a quick connector, the quick connector is connected with a deionized water pipe, the deionized water pipe is connected with a circulating pump, deionized water is pumped into the lower cavity through the quick connector, and floating and sinking and metal oxides in the crude mercury are washed from bottom to top, so that the further purification effect of the mercury is achieved. The quick-connection joint adopts a form of a thread at one end and a quick-connection joint at the other end, so that the whole body can be conveniently assembled and disassembled with the outside; the quick-connection joint can be changed into a form of a one-head screw thread one-head double quick-connection joint. The middle part, namely the middle quartz column, is a cylindrical quartz glass three-stage hollow filter column, the upper part is connected with the bottom end of the inner cavity of the flange seat at the upper part, and the lower part is connected with the top end of the inner cavity of the flange seat at the lower part. The middle part is provided with a circular three-stage filter screen vertical to the axial direction of the three-stage hollow filter column.

The middle part main part material is quartz glass, realizes visually, is convenient for observe the pollution state, in time washs or changes the filter screen. The cylindrical hollow first inner column and the cylindrical hollow second inner column which are made of quartz glass are sequentially arranged in the three-stage hollow filter column from top to bottom, the bottom areas of the first inner column and the second inner column are the same, and the first inner column and the second inner column are connected in a sealing mode through flanges, O-shaped sealing rings of the inserting parts and screws and nuts. The first inner column is internally provided with a first-stage filter screen and a second-stage filter screen which are vertical to the axial direction of the first inner column, the first-stage filter screen is positioned on the second-stage filter screen and has a certain distance relatively, the filter screens are circular, and the size of the filter screens is equal to the bottom area of the first inner column. Furthermore, all be equipped with in first interior post and the second with its axle direction perpendicular tertiary filter screen and stainless steel mesh sheet, the filter screen is circular, and its size equals with post bottom surface area in the second, and stainless steel mesh sheet is located post bottom in the second. The filter screen and the periphery of the mesh slice are hermetically connected with the inner column. Preferably, the first-stage filter screen is 100 meshes, the second-stage filter screen is 150 meshes, the third-stage filter screen is 200 meshes, and the filter screens can also be replaced by nylon screens. After the filter pressing is carried out for a certain pressure, the mercury liquid is subjected to the filter pressing step by step from top to bottom. More preferably, the three-stage filter screen forms three-stage filtration, which filters pollutant particles adsorbed in mercury liquid from large to small, and has a filtering and membrane breaking effect under certain pressure to overcome surface tension and filter aggregates with smaller primary particle size step by step. In a preferred embodiment, according to the purity standard, a multi-stage filtering screen combination design can be adopted, and the screen mesh combination and the control times of the screening cycle can be replaced and optimized according to the characteristics of the filtering fluid, so that the expected purification standard reaching the purity standard can be realized.

Extrusion rings are arranged between the three-level hollow filter column and the inner column at positions corresponding to the first-level filter screen, the second-level filter screen and the third-level filter screen. The damage of the inner column caused by the downward flow and extrusion of the mercury liquid is reduced. The top of the first inner column is connected with the bottom end of the inner cavity of the flange seat at the upper part of the third level, an O-shaped sealing ring at the inner side of the upper part is arranged between the connecting positions of the first inner column and the third inner column, the bottom of the second inner column is connected with the top end of the inner cavity of the flange seat at the lower part of the third level, and an O-shaped sealing ring at the lower part is arranged between the connecting positions. Realize the sealing connection and avoid the side leakage of the mercury liquid. The top of the three-level hollow filter column is connected with a three-level upper flange seat, an upper sealing ring is arranged between the top of the three-level hollow filter column and the three-level upper flange seat, the upper sealing ring is extruded and sealed, an O-shaped sealing ring on the inner side of the upper portion and the three-level upper flange seat are compressed, top sealing is formed, mercury can only penetrate out from a middle through hole, and side leakage cannot be generated. The bottom of the three-stage hollow filter column is connected with a three-stage lower flange seat, and a lower O-shaped sealing ring is arranged between the three-stage hollow filter column and the three-stage lower flange seat for extrusion sealing. Similarly, the lower O-shaped sealing ring and the three-level lower flange seat are tightly pressed to form top sealing, and mercury can only penetrate out of the middle through hole without side leakage.

The quartz column structure on both sides is more withstand voltage, reduces the damaged condition. The connecting ends of the two inner columns adopt a screw and nut detachable combined sealing structure, so that the disassembly, the cleaning, the part replacement and the repair are convenient; the flow system can realize the back flushing cleaning function under the condition of not being disassembled. The inlet and outlet quick assembly and disassembly structure can realize quick assembly, sealing and fault detection. The upper and lower two parts of main body material is polytetrafluoroethylene, and the sealing washer is the fluorine glue material, all does not produce chemical reaction with mercury.

According to the technical scheme, the functional structure performs multi-stage filter pressing, membrane breaking, flushing and purification in a specially designed closed cavity (a visible filter) according to the principle that mercury is in a normal-temperature maximum-density liquid phase and has huge density difference with a mechanical impurity particle oxidation membrane and water. According to the multi-phase system large-density differential layer extraction principle, the buoyancy reverse circulating flushing filtration and layered extraction purification effects of the mercury-impurity oxide film-water ternary combination system are realized, the normal-temperature physical purification of mercury is realized, and the advantages of environmental protection, safety and reliability are achieved.

In summary, the multistage filter-pressing membrane-breaking mercury purification device mainly has the following beneficial technologies:

1. according to the scheme, the purity of the crude mercury is gradually improved by a multi-stage filter-pressing membrane-breaking deionized water buoyancy reverse circulation purification technology under a normal temperature condition, and finally the purity of the purified mercury is more than 99.9%, so that the purity of the purified mercury meets the mercury purity specified in laboratory mercury pressure method capillary pressure curve experimental standard GB/T2650.1-2008; high-temperature vacuum distillation or chemical-electrochemical treatment of the traditional mercury purification method is not adopted, so that the problems that high-temperature virulent mercury vapor or secondary dangerous waste is generated and the application scene of small-scale mercury purification is not suitable are solved; meanwhile, the technical problems of regeneration treatment for purifying pollutants and mercury removal and standard discharge of discharged sewage are solved, and a brand new technical path is opened up for purification treatment and reutilization of laboratory-scale crude mercury.

2. The scheme of the invention has reliable performance, safety, environmental protection and high environmental applicability, can realize on-site timely environmental protection treatment by a mercury laboratory, and reduces the risk of secondary pollution diffusion transfer; and the absolute amount of mercury in a laboratory can be reduced, the recycling is promoted, and the method has good economic benefit, environmental protection social benefit and meets the requirement of environmental protection policy encouragement.

3. The upper and lower ends of the coarse mercury vibrating screen secondary filter and the tertiary fine filter developed and designed by the scheme of the invention adopt a cone-like body + cylinder combined inner cavity design, the middle of the coarse mercury vibrating screen secondary filter and the tertiary fine filter is connected with the secondary or tertiary filter pipe in a diameter reducing hole mode, the structure is a dumbbell-shaped structure with the wide upper end and the wide lower end and the thin middle, and the secondary filter can realize the vibrating screen friction and constant flow variable cross section tubule acceleration effect and the front-back differential pressure expansion effect of a Venturi tube narrow tube throttling interface to enhance the friction mixing filtering effect; the three-stage filter structure design not only applies the Venturi tube effect, but also adopts three layers of screens which gradually reduce meshes (namely increase the mesh number of the screens), so that more tiny variable flow cross section mesh effects are formed, and the microsphere particle high-interfacial tension microsphere liquid drops containing dust and oxide films are further extruded and deformed and frictionally deformed when passing through the mesh holes, so that the filtering effect is further improved.

4. According to the scheme, the pre-filtering column, the secondary filter and the tertiary filter are adopted to form a multi-stage screen mesh number increasing filtering combination, a pressure extrusion continuous membrane breaking optimization functional structural system is constructed, and the properties of normal-temperature high-density liquid and high specific surface tension of mercury and the multi-stage screen extrusion friction membrane breaking effect are fully utilized.

5. The scheme of the invention realizes the buoyancy reverse circulating flushing filtration and layered extraction purification effects of the mercury-impurity oxide film-water ternary combination system by utilizing the multiphase system high-density differential layer extraction principle, realizes the normal-temperature physical purification of mercury, and has the advantages of environmental protection, safety and reliability.

6. The scheme of the invention adopts PLC programming, synchronous touch screen flow, automatic quality control detection, discharge mercury removal purification and other intelligent technologies for micro-integration manufacturing, and achieves the aims of minimizing field occupation, environment-friendly discharge waste liquid reaching standards and diversified application scenes under normal temperature conditions.

All the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and all other extended embodiments obtained by a person of ordinary skill in the art without making innovative efforts based on the embodiments of the present invention belong to the protection scope of the present invention. Although the present invention has been described in detail with reference to the foregoing examples, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. .

Claims

1. The utility model provides a multistage filter-pressing broken membrane mercury purification device, its characterized in that, it includes automatic flow operation and matter accuse electrical part, multistage filtration purification part, gas-liquid pressure power part, gas-liquid storage part and atmospheric pressure drive unit, and it is multistage filter-pressing broken membrane mercury purification device under the normal atmospheric temperature condition, wherein:

the automatic flow operation and quality control electrical part is used for on-off control, flow path conversion, operation sequence control, sensor data acquisition, subprogram skip and identification and judgment on whether a quality control index critical condition is met or not of pump and electromagnetic valve electrical elements in the multistage filter-pressing membrane-breaking mercury purification device so as to realize automatic operation of the treatment process of the multistage filter-pressing membrane-breaking mercury purification device;

the multistage filtration purification part is used for performing graded fine filtration purification on coarse mechanical impurities, mercury soot broken fine dust and a metal oxide film in a multistage filter-pressing membrane-breaking mercury purification device to obtain recyclable fine mercury meeting the experimental quality standard requirement of mercury pressing; the multi-stage filtration and purification part comprises a pre-filtration column, a secondary filter, a tertiary filter, a deionized water circulating mercury removal filter and a sewage discharge mercury removal filter;

the air pressure driving unit comprises a nitrogen generator and a nitrogen buffer tank, the output end of the nitrogen generator is connected with the input end of the nitrogen buffer tank through a nitrogen source electromagnetic valve, and an inlet pressure sensor is arranged on a pipeline between the nitrogen source electromagnetic valve and the nitrogen buffer tank; the output end of the nitrogen buffer tank is connected with the input end of the thick mercury bottle through an electromagnetic valve at the outlet of the buffer tank; an external blow-down pipe is further branched on a pipeline between the nitrogen buffer tank and the crude mercury bottle, and a gas-liquid blow-down port electromagnetic valve is arranged in the external blow-down pipe;

the pre-filtering column comprises a pre-filtering column outlet end cover, a pre-filtering column filtering pipe and a pre-filtering column inlet end cover; the pre-filtering column filtering pipe is a quartz glass pipe with double threads, the two ends of the pre-filtering column filtering pipe are respectively connected with the outlet end cover of the pre-filtering column and the inlet end cover of the pre-filtering column in a threaded mode, the pre-filtering column filtering pipe, the two ends of the pre-filtering column filtering pipe and the inlet end cover of the pre-filtering column surround a space for accommodating a filtering structure of the pre-filtering column together, and the filtering structure comprises two glass fiber parts close to the outlet end cover of the pre-filtering column and the inlet end cover of the pre-filtering column and a quartz glass ball part positioned in the middle;

the secondary filter comprises a secondary top spiral end cover, a secondary vibrating screen friction cavity, a first O-shaped sealing ring, a secondary filter primary screen, a secondary middle reducing pipe, a second O-shaped sealing ring, a secondary filter secondary filtering screen and a secondary coarse mercury receiving cavity which are sequentially connected from top to bottom;

the third-stage filter comprises a third-stage upper inlet seat, a third-stage upper flange seat, a third-stage filter pipe, a third-stage lower flange seat and a third-stage lower outlet seat which are sequentially connected from top to bottom; the third-stage filtering pipe comprises a third-stage hollow filtering column which is communicated up and down, the bottom of a third-stage upper flange seat is provided with an annular groove, the upper end of the third-stage hollow filtering column is embedded into the annular groove, and an upper sealing ring is arranged between the third-stage hollow filtering column and the third-stage hollow filtering column; an upper inner side O-shaped sealing ring is clamped between the inner side of the upper end of the three-stage hollow filter column and the annular groove;

and a plurality of layers of filter screens of the three-stage filter are distributed in the three-stage hollow filter column along the length direction.

2. The multi-stage filter-press membrane-breaking mercury purification device of claim 1, wherein gas-liquid in the multi-stage filter-press membrane-breaking mercury purification device comprises nitrogen, deionized water and mercury.

3. The multi-stage filter-press membrane-breaking mercury purification device of claim 2, wherein the gas-liquid pressure power part is used for providing driving and pressure for flowing, circulating, membrane-breaking, flushing and purifying of nitrogen, deionized water and mercury in the multi-stage filter-press membrane-breaking mercury purification device.

4. The multi-stage filter-press membrane-breaking mercury purification device according to claim 1, further comprising an air pressure driving unit, a coarse mercury bottle, a pre-filter column, a secondary filter, a tertiary filter and a fine mercury collecting bottle which are sequentially connected through a pipeline assembly.

5. The multi-stage filter-press membrane-breaking mercury purification device as claimed in claim 4, wherein the pneumatic drive unit is used for filling the upper chambers of the secondary filter and the tertiary filter with mercury to be filtered, pressurizing and filtering the lower chambers of the secondary filter and the tertiary filter, and flushing the flow line.

6. The multi-stage pressure filtration membrane-breaking mercury purification device of claim 4, wherein the crude mercury bottle is used for quantitative storage of crude mercury or polluted mercury to be treated.

7. The multi-stage filter-pressing membrane-breaking mercury purification device according to claim 4, wherein the pre-filtration column is used for primary filtration of coarse mechanical impurities in coarse mercury or polluted mercury, and pollution and flow blockage to the secondary filter are reduced.

8. The multi-stage pressure filtration membrane-breaking mercury purification device of claim 4, wherein the secondary filter is used for fine dust impurity filtration and realizes pressure filtration and mechanical shock comprehensive membrane breaking of the mercury soot mixture.

9. The multi-stage pressure filtration membrane-breaking mercury purification device according to claim 8, wherein the three-stage filter is used for further fine filtration of the two-stage filtered mercury, oxidation membrane dissolution and reverse-flushing circulation deep purification of the buoyancy of deionized water; the deionized water buoyancy reverse flushing circulation is characterized in that a deionized water circulating pump is used for reversely pumping deionized water into the tertiary filter from a tertiary filter discharge port at the bottommost part of the tertiary filter to accommodate a filtered mercury three-level lower cavity, the deionized water can be freely reversely floated and flushed from the bottom of the three-level lower cavity from bottom to top without pressure under the buoyancy effect generated by the huge density difference of mercury, a reverse convection purification effect is formed, and the filtered mercury is further purified.

10. The multi-stage filter-pressing membrane-breaking mercury purification device according to claim 4, wherein the fine mercury collecting bottle is used for collecting and storing fine mercury which reaches mercury standards for mercury pressing experiments after being sequentially and gradually purified by pre-filtration column filtration, secondary filter filtration, tertiary filter filtration and deionized water reverse buoyancy flushing.