CN110065940A - A kind of equipment and technology for intervening subcritical solvent pressure changeable removing carbon material - Google Patents
A kind of equipment and technology for intervening subcritical solvent pressure changeable removing carbon material Download PDFInfo
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- CN110065940A CN110065940A CN201910529220.6A CN201910529220A CN110065940A CN 110065940 A CN110065940 A CN 110065940A CN 201910529220 A CN201910529220 A CN 201910529220A CN 110065940 A CN110065940 A CN 110065940A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
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Abstract
A kind of equipment and technology for intervening subcritical solvent pressure changeable removing carbon material, equipment store assembly, solid-liquid mixing assembly by powdery carbon material raw material, vacuumize assembly, pressure changeable intercalation separating assembly, gas solid separation assembly, gas compression assembly, heat exchange cooling unit, storage assembly is constituted in solvent；The subcritical solvent mixture of powdery carbon material and liquid that quantitative and even is mixed is sent into diaphragm pump, and the process requirement time is stopped in diaphragm pump；Due to the transformation stress effect that diaphragm vibrates up and down in diaphragm pump housing, mixture Subcritical solvent converts mixture between liquid and gaseous state, realizes intercalation stripping.
Description
Technical field
The present invention relates to materials processing technologies, in particular to a kind of to intervene setting for subcritical solvent pressure changeable removing carbon material
Standby and technique.
Background technique
Graphite is strategic important carbon goods and materials, and because of structure difference, graphite is divided into phenocrystalline (also known as scale matter) and cryptocrystalline；
Scale matter graphite can produce graphene with stripping method, and aphanitic graphite is also required to first remove dispersion, can just produce high purity graphite；
Intercalation stripping uses the concentrated sulfuric acid more at present, and hydrogen peroxide etc. has contaminated materials, and low efficiency, at high cost, it is difficult to continuous automatic
Metaplasia produces；It is necessary to develop new equipment and technology thus；
It is carbonized using biological material into porous carbon, it is also desirable to which removing is dispersed into nano material, just there is more advanced purposes；
The subcritical state of substance is a kind of form relative to critical state and supercriticality；The temperature of vehicle substance
When higher than its boiling point, exist with gaseous state, certain pressure compression is imposed to it makes its liquefaction, its phase is utilized under this liquefaction
The molten physical property of patibhaga-nimitta, the solvent as extracting substances are subcritical abstraction solvent, and extraction process is known as subcritical abstraction
Technique；The solvent boiling point for being suitable for subcritical abstraction is below environment temperature around us, and general boiling point is at 0 DEG C hereinafter, 20
DEG C when liquefaction pressure in 0.8MPa or less (gauge pressure)；Common subcritical abstraction solvent, there is propane, butane, R22, R134a etc.；
Current subcritical solvent is served only for active components of plants extraction, and uranidin is such as extracted from marigold, has no and is used for
Carbon material intercalation stripping, the carbon materials such as graphite are hydrophobic material, and propane, butane, R22, R134a etc. are compressed into liquid Shi Xianfei
Polarity, therefore the gap of the intrusion carbon materials intergranular such as graphite can be facilitated, solvent gasification expansion when decompression, with regard to carbon such as spalling graphite
The carbon materials intercalation strippings such as graphite are realized in the gap of material intergranular.
Summary of the invention
A kind of equipment intervening subcritical solvent pressure changeable removing carbon material, stores assembly by powdery carbon material raw material, Gu
Liquid mixing assembly vacuumizes assembly, pressure changeable intercalation separating assembly, gas solid separation assembly, gas compression assembly, heat exchange cooling
Assembly, storage assembly is constituted in solvent, it is characterized in that powdery carbon material raw material storage assembly passes through pipeline and solid-liquid mixing assembly company
It connects, solid-liquid mixing assembly is connect by pipeline with pressure changeable intercalation separating assembly, is vacuumized assembly and is mixed by pipeline with solid-liquid
Assembly is connected with pressure changeable intercalation separating assembly threeway, and pressure changeable intercalation separating assembly is connected by pipeline and gas solid separation assembly
It connects, gas solid separation assembly is connect by pipeline with gas compression assembly, and gas compression assembly is cooling total by pipeline and heat exchange
At connection, heat exchange cooling unit is connect by pipeline with solid-liquid mixing assembly, and assembly is store in solvent and passes through pipeline and heat exchange
Cooling unit is connected with solid-liquid mixing assembly threeway；
Powdery carbon material raw material storage assembly measures isolating valve 1, connecting tube 1 by staving 1, upper capping, gate valve 1, and pressure is put down
Weighing apparatus pipe, pressure balance sluice valve 10 are constituted；
1 main body of staving is cylinder, and lower part is inverted conical shape, and 1 upper end of connecting tube and 1 lower part inverted conical shape top of staving connect
It connects, 1 lower end of connecting tube is connect with the upper top surface of the staving 2 of solid-liquid mixing assembly；Gate valve 1 is housed from the top down in connecting tube 1,
Measure isolating valve 1；The upper surface of 1 main body cylinder shape of staving, equipped with the openable upper capping for being packed into powdery carbon material raw material；Pressure
Balance pipe upper end is connect with 1 main body upper end of staving, and pressure-equalizing pipe lower end connects with the upper top surface of the staving 2 of solid-liquid mixing assembly
It connects, the pressure of balance powdery carbon material raw material storage assembly and solid-liquid mixing assembly, pressure-equalizing pipe is provided with pressure-equalizing pipe
Gate valve 10；
Solid-liquid mixing assembly measures isolating valve 4, connecting tube 3, lock by staving 2, blender, connecting tube 2, gate valve 2, gate valve 3
Valve 4 measures isolating valve 3 and constitutes；
Staving 2 is cylinder, and inside staving 2, blender axis is stretched out from 2 upper surface of staving to be driven blender by motor
Dynamic, 2 one end of connecting tube is connect with 2 upper surface of staving, and 2 other end of connecting tube goes out cold liquid mouth with heat exchange cooling unit and connect,
Nearly 2 end of staving of connecting tube 2 is equipped with gate valve 2, gate valve 3 is housed at 2 near-thermal of connecting tube exchange cooling unit end, in gate valve 3 and threeway
Equipped with metering isolating valve 4 between mouthful；3 one end of connecting tube is connect with 2 threeway of connecting tube, and storage is total in 3 other end of connecting tube and solvent
At connection；Assembly end is store in connecting tube 3 in nearly solvent, gate valve 4 is housed, equipped with metering isolating valve 3 between gate valve 4 and three ports；
It is that pressure-bearing receiver is commercialized in oneself that assembly is store in solvent；
Pressure changeable intercalation separating assembly is made of diaphragm pump, connecting tube 4, gate valve 5, connecting tube 5, gate valve 6, the own quotient of diaphragm pump
Product, 4 one end of connecting tube connect membrane pump feeding mouth, and 4 other end of connecting tube connects the lower end surface of solid-liquid mixing assembly staving 2,
Nearly diaphragm pump end is equipped with gate valve 5 in connecting tube 4；5 one end of connecting tube connects diaphragm pump discharge port, the connection of 5 other end of connecting tube
The cylindrical surface lower end of the staving 3 of gas solid separation assembly, nearly diaphragm pump end is equipped with gate valve 6 in connecting tube 5；
Gas solid separation assembly measures isolating valve by staving 3, inclined plate isolator, purpose ceramic-film filter, connecting tube 6, gate valve 7
2, connecting tube 7, gate valve 8 is constituted,
3 main body of staving is cylinder, and lower part is inverted conical shape, and 6 upper end of connecting tube and 3 lower part inverted conical shape top of staving connect
It connects, gate valve 7 is housed from the top down in connecting tube 6, measure isolating valve 2；6 lower end of connecting tube, which leads to atmosphere, sends out processing good material；
In 3 inside upper semisection of staving, from bottom to top equipped with oneself commercialization inclined plate isolator, purpose ceramic-film filter is commercialized in oneself；Connecting tube 7
One end is connect with 3 upper surface of staving, and 7 other end of connecting tube is connect with the gas compression pump steam inlet of gas compression assembly, connection
3 end of nearly staving is equipped with gate valve 8 in pipe 7；
Oneself is configured with high pressure gas backwashing system by commercialization purpose ceramic-film filter；
Gas compression assembly is made of gas compression pump, connecting tube 8,
Oneself is commercialized gas compression pump, and gaseous solvent propane, butane, R22, R134a etc. are compressed into liquid by gas compression pump
State is sent into the hydrothermal solution import of heat exchange cooling unit by connecting tube 8；
The own commercialization of heat exchange cooling unit；
Assembly is vacuumized by vacuum pumping pump, connecting tube 9 is constituted,
Oneself commercialization of vacuum pumping pump, 9 one end of connecting tube connect with vacuum pumping pump air inlet, 9 other end of connecting tube with connect
4 threeway of pipe connection, in 9 inside of connecting tube, nearly vacuum pumping pump inlet port is equipped with gate valve 9；
The removing of carbon material pressure changeable is carried out using the equipment that the present invention intervenes subcritical solvent pressure changeable removing carbon material
Technique is for example following:
1. setting primary condition, all valves of system are to close, and in following process, valve state is shown in valve state table
Explanation；The staving 1 of powdery carbon material raw material storage assembly has been charged into powdery carbon material raw material, covers capping；
2. pair solid-liquid mixing assembly, pressure changeable intercalation separating assembly, gas solid separation assembly vacuumize, after reaching technique requirement
Stopping vacuumizes；
3. injecting the subcritical solvent of liquid to solid-liquid mixing assembly, cube is wanted to technique；
4. powdery carbon material raw material, powdery carbon material raw material and the subcritical solvent solid-liquid of liquid is added to solid-liquid mixing assembly
Than being required to technique；
Powdery carbon material is uniformly mixed with the subcritical stirring solvent of liquid；
5. the subcritical solvent mixture of powdery carbon material and liquid that quantitative and even is mixed is sent into diaphragm pump, in diaphragm pump
The interior stop process requirement time；Mixture in diaphragm pump housing due to the transformation stress effect that diaphragm vibrates up and down, in mixture
Subcritical solvent converts between liquid and gaseous state, realizes intercalation stripping；
6. the powdery carbon material of own intercalation stripping and the subcritical solvent mixture of liquid are sent into gas solid separation assembly, Asia is faced
Boundary's solvent under reduced pressure is in gaseous state, and the subcritical solvent of gaseous state is separated with the powdery carbon material of the own intercalation stripping of solid-state, the own intercalation stripping of solid-state
From powdery carbon material deposition 3 lower part inverted conical shape bucket bottom of staving through metering isolating valve 2 send out；
7. decompression is in the subcritical solvent of gaseous state in gas solid separation assembly, through inclined plate isolator, after purpose ceramic-film filter filtering,
Solid-liquid mixing assembly is sent back to by gas compressor and boil down to liquid, then through heat exchange cooling, is recycled；8. circulation losses are sub-
Critical solvent is by storing assembly Subcritical solvent make-up in solvent；
It sends the amount of the subcritical solvent of liquid of solid-liquid mixing assembly back to, is sent into the amount of powdery carbon material raw material, and be added to
The amount of subcritical solvent meets technique requirement；Metering and the own commercialization of proportional controlling device；
Each technique period valve state is for example following, and wherein "-" indicates that valve state is same as above a process or valve state changes
Do not influence this production technology；
Upper table is illustrated:
When process 6. is quantitatively packed into mixture to diaphragm pump, the switch time of control gate valve 5, the powder that quantitative and even is mixed
Shape carbon material and the subcritical solvent mixture of liquid are sent into diaphragm pump；
When 7. intercalation stripping of process, control gate valve 5 and 6 shut-in time of gate valve, i.e. the powdery carbon of control quantitative and even mixing
Material and the subcritical solvent mixture of liquid stop the process requirement time in diaphragm pump
Process 8. is when sending to solid gas separation, program 6, program 7, and 8 automatic cycle of program carries out
When process 10. releases finished product, metering isolating valve 2 is closed, gate valve 7 is opened, processed material and enter gate valve 7 and metering
6 inner space of connecting tube between isolating valve 2, closing gate valve 7, rotary metering isolating valve 2 process material and are sent equipment；
Automatically the switch of above-mentioned valve is managed, so that it may the present invention be maintained to intervene subcritical solvent pressure changeable removing carbon material
The technique that equipment carries out the removing of carbon material pressure changeable automatically continuously produces.
Detailed description of the invention
Attached drawing 1 is the device structure schematic diagram that the present invention intervenes subcritical solvent pressure changeable removing carbon material.
Specific embodiment
Make below in conjunction with the equipment and technology that attached drawing 1 is the subcritical solvent pressure changeable removing carbon material of present invention intervention into one
Step explanation, but be not to a kind of limitation of the invention；
A kind of equipment intervening subcritical solvent pressure changeable removing carbon material, stores assembly (1) by powdery carbon material raw material,
Solid-liquid mixing assembly (2) vacuumizes assembly (3), pressure changeable intercalation separating assembly (4), gas solid separation assembly (5), gas compression
Assembly (6), heat exchange cooling unit (7), storage assembly (8) is constituted in solvent, it is characterized in that powdery carbon material raw material stores assembly
(1) it is connect by pipeline with solid-liquid mixing assembly (2), it is total that solid-liquid mixing assembly (2) separates (4) by pipeline with pressure changeable intercalation
At connection, vacuumizes assembly (3) and is connect by pipeline with solid-liquid mixing assembly (2) and pressure changeable intercalation separating assembly (4) threeway,
Pressure changeable intercalation separating assembly (4) connect by pipeline with gas solid separation assembly (5), gas solid separation assembly (5) pass through pipeline and
Gas compression assembly (6) connection, gas compression assembly (6) are connect by pipeline with heat exchange cooling unit (7), and heat exchange is cooling
Assembly (7) is connect by pipeline with solid-liquid mixing assembly (2), and assembly (8) are store in solvent and pass through pipeline and heat exchange cooling unit
(7) it is connected with solid-liquid mixing assembly (2) threeway；
Powdery carbon material raw material stores assembly (1) by staving 1 (1-1), upper capping (1-2), gate valve 1 (1-5), metering isolation
Valve 1 (1-6), connecting tube 1, (1-7) pressure-equalizing pipe (1-4), pressure balance sluice valve 10 (1-3) are constituted；
(1-1) main body of staving 1 is cylinder, and lower part is inverted conical shape, under the upper end (1-7) of connecting tube 1 and staving 1 (1-1)
The connection of portion inverted conical shape top, the lower end (1-7) of connecting tube 1 is connect with the upper top surface of the staving 2 (2-3) of solid-liquid mixing assembly (2)；?
Gate valve 1 (1-5) is housed from the top down in connecting tube 1 (1-7), is measured isolating valve 1 (1-6)；Staving 1 (1-1) main body cylinder shape
Upper surface, equipped with the openable upper capping (1-2) for being packed into powdery carbon material raw material；The pressure-equalizing pipe upper end (1-4) and staving 1
The connection of (1-1) main body upper end, the pressure-equalizing pipe lower end (1-4) connect with the upper top surface of the staving 2 (2-3) of solid-liquid mixing assembly (2)
It connects, the pressure of balance powdery carbon material raw material storage assembly (1) and solid-liquid mixing assembly (2), pressure-equalizing pipe (1-4) is provided with
Pressure balance sluice valve 10 (1-3)；
Solid-liquid mixing assembly (2) is by staving 2 (2-3), blender (2-2), connecting tube 2 (2-1), gate valve 2 (2-4), gate valve 3
(7-1) is measured isolating valve 4 (7-4), connecting tube 3, and (8-2, metering isolating valve 3 (8-3) are constituted gate valve 4；
Staving 2 (2-3) is cylinder, and blender (2-2) is internal mounted in staving 2 (2-3), and blender (2-2) axis is from staving 2
The upper surface (2-3) is stretched out and is driven by motor, and the one end (2-1) of connecting tube 2 is connect with the upper surface staving 2 (2-3), connecting tube 2 (2-1)
The other end goes out cold liquid mouth with heat exchange cooling unit (7) and connect, and gate valve 2 is housed at connecting tube 2 (2-1) nearly staving 2 (2-3) end
(2-4) is equipped with gate valve 3 (7-1) at (2-1) near-thermal of connecting tube 2 exchange cooling unit (7) end, in gate valve 3 (7-1) and three ports
Between equipped with metering isolating valve 4 (7-4)；The one end (8-1) of connecting tube 3 is connect with connecting tube 2 (2-1) threeway, connecting tube 3 (8-1)
The other end is connect with storage assembly (8) in solvent；Assembly (8) end is store in connecting tube 3 (8-1) in nearly solvent, gate valve 4 (8-2) is housed,
Equipped with metering isolating valve 3 (8-3) between gate valve 4 (8-2) and three ports；
It is that pressure-bearing receiver is commercialized in oneself that assembly (8) are store in solvent；
Pressure changeable intercalation separating assembly (4) is by diaphragm pump (4-2), connecting tube 4 (4-5), gate valve 5 (4-1), 5 (4- of connecting tube
6), gate valve 6 (4-7) is constituted, oneself is commercialized diaphragm pump (4-2), and the one end (4-5) of connecting tube 4 connects diaphragm pump (4-2) feed inlet,
(4-5) other end of connecting tube 4 connect solid-liquid mixing assembly (2) staving 2 (2-3) lower end surface, in connecting tube 4 (4-5) closely every
Membrane pump end is equipped with gate valve 5 (4-1)；The one end (4-6) of connecting tube 5 connects diaphragm pump (4-2) discharge port, connecting tube 5 (4-6) other end
The cylindrical surface lower end for connecting the staving 3 (5-1) of gas solid separation assembly (5), nearly diaphragm pump end is equipped with lock in connecting tube 5 (4-6)
Valve 6 (4-7)；
Gas solid separation assembly (5) is by staving 3 (5-1), inclined plate isolator (5-5), purpose ceramic-film filter (5-7), connecting tube 6
(5-3), gate valve 7 (5-4) measure isolating valve 2 (5-2), connecting tube 7 (5-9), and gate valve 8 (5-8) is constituted,
(5-1) main body of staving 3 is cylinder, and lower part is inverted conical shape, under the upper end (5-3) of connecting tube 6 and staving 3 (5-1)
The connection of portion inverted conical shape top, is equipped with gate valve 7 (5-4) from the top down in connecting tube 6 (5-3), measures isolating valve 2 (5-2)；Connection
The lower end (5-3) of pipe 6, which leads to atmosphere, sends out processing good material；In the internal upper semisection of staving 3 (5-1), from bottom to top equipped with oneself commercialization
Inclined plate isolator (5-5), purpose ceramic-film filter (5-7) is commercialized in oneself；The one end (5-9) of connecting tube 7 and the upper surface staving 3 (5-1)
Connection, (5-9) other end of connecting tube 7 are connect with the gas compression pump steam inlet of gas compression assembly (6), in connecting tube 7 (5-9)
Nearly staving 3 (5-1) end is equipped with gate valve 8 (5-8)；
Oneself is configured with high pressure gas backwashing system at commercialization purpose ceramic-film filter (5-7)；
Gas compression assembly (6) is made of gas compression pump, connecting tube 8 (6-1),
Oneself is commercialized gas compression pump, and gaseous solvent propane, butane, R22, R134a etc. are compressed into liquid by gas compression pump
State is sent into heat exchange cooling unit (7) hydrothermal solution import by connecting tube 8 (6-1)；
The own commercialization of heat exchange cooling unit (7)；
Assembly is vacuumized by vacuum pumping pump, connecting tube 9 (3-2) is constituted,
Oneself is commercialized vacuum pumping pump, and the one end (3-2) of connecting tube 9 is connect with vacuum pumping pump air inlet, and connecting tube 9 (3-2) is another
One end is connect with connecting tube 4 (4-5) threeway, and 9 (3- of gate valve is housed in connecting tube 9 (3-2) internal nearly vacuum pumping pump inlet port
1)；
The removing of carbon material pressure changeable is carried out using the equipment that the present invention intervenes subcritical solvent pressure changeable removing carbon material
Technique is for example following:
1. setting primary condition, all valves of system are to close, and in following process, valve state is shown in valve state table
Explanation；The staving 1 (1-1) of powdery carbon material raw material storage assembly (1) has been charged into powdery carbon material raw material, covers capping (1-
2)；
2. pair solid-liquid mixing assembly (2), pressure changeable intercalation separating assembly (4), gas solid separation assembly (5) vacuumize, reach
Technique stops vacuumizing after requiring；
3. to the staving 2 of solid-liquid mixing assembly (2), ((2-3) injects the subcritical solvent of liquid, wants cube to technique；Note
Enter the subcritical solvent volume of liquid and accounts for (the 70-90% of (2-3) of staving 2
It is subcritical solvent selection propane, butane, No. four solvents (propane, butane mixture), a kind of in R22, R134a；
4. to the staving 2 of solid-liquid mixing assembly (2), (powdery carbon material raw material, powdery carbon material raw material and liquid is added in (2-3)
The subcritical solvent solid-to-liquid ratio of state is required to technique；
The volume ratio 1:4-20 of powdery carbon material raw material and the subcritical solvent solid-liquid of liquid
Powdery carbon material is uniformly mixed with the subcritical stirring solvent of liquid；
5. the subcritical solvent mixture of powdery carbon material and liquid that quantitative and even is mixed is sent into diaphragm pump (4-2),
The process requirement time is stopped in diaphragm pump diaphragm pump (4-2)；
The switch time of control gate valve 5 just controls mixed uniformly powdery carbon material and the subcritical solvent mixture of liquid
It is sent into quantifying for diaphragm pump, the ETAD expected time of arrival and departure of gate valve 5 0.1-1 seconds；
Process requirement time 3- is stopped in mixed uniformly powdery carbon material and the subcritical solvent mixture diaphragm pump of liquid
60 seconds；
Mixture is in diaphragm pump (4-2) cavity due to the transformation stress effect that diaphragm vibrates up and down, mixture Subcritical
Solvent converts between liquid and gaseous state, realizes intercalation stripping；
6. the powdery carbon material of own intercalation stripping and the subcritical solvent mixture of liquid are sent into gas solid separation assembly (5),
Subcritical solvent under reduced pressure is in gaseous state, and the subcritical solvent of gaseous state separates with the powdery carbon material of the own intercalation stripping of solid-state, oneself is slotting for solid-state
The powdery carbon material deposition of layer removing is sent out at the lower part inverted conical shape bucket bottom staving 3 (5-1) through metering isolating valve 2 (5-2)；
7. decompression is in the subcritical solvent of gaseous state in gas solid separation assembly (5), through inclined plate isolator (5-5), ceramic membrane filter
After device (5-7) filtering, by the gas compressor of gas compression assembly (6) and boil down to liquid, then through heat exchange cooling unit (7)
Solid-liquid mixing assembly (2) is sent in cooling back to, is recycled；
8. the subcritical solvent of circulation losses is by storing assembly (8) Subcritical solvent make-up in solvent；
It sends the amount of the subcritical solvent of liquid of solid-liquid mixing assembly (2) back to, the amount of powdery carbon material raw material is sent into, with supplement
The amount for entering subcritical solvent meets technique requirement；Metering and the own commercialization of proportional controlling device；
Each technique period valve state is for example following, and wherein "-" indicates that valve state is same as above a process or valve state changes
Do not influence production technology；
Upper table is illustrated:
When process 6. is quantitatively packed into mixture to diaphragm pump, the switch time of control gate valve 5, the powder that quantitative and even is mixed
Shape carbon material and the subcritical solvent mixture of liquid are sent into diaphragm pump；
When 7. intercalation stripping of process, control gate valve 5 and 6 shut-in time of gate valve, i.e. the powdery carbon of control quantitative and even mixing
Material and the subcritical solvent mixture of liquid stop the process requirement time in diaphragm pump
Process 8. is when sending to solid gas separation, program 6, program 7, and 8 automatic cycle of program carries out
When process 10. releases finished product, metering isolating valve 2 is closed, gate valve 7 is opened, processed material and enter gate valve 7 and metering
6 inner space of connecting tube between isolating valve 2, closing gate valve 7, rotary metering isolating valve 2 process material and are sent equipment；
Automatically the switch of above-mentioned valve is managed, so that it may the present invention be maintained to intervene subcritical solvent pressure changeable removing carbon material
The technique that equipment carries out the removing of carbon material pressure changeable automatically continuously produces.
Embodiment 1
Scale matter graphite powder is sent into the equipment that the present invention intervenes subcritical solvent pressure changeable removing carbon material and carries out carbon materials
Expect pressure changeable removing, ultrasonic dispersing machine dispersion is sent into after removing, harvests graphene；
Embodiment 2
Aphanitic graphite powder is sent into the equipment that the present invention intervenes subcritical solvent pressure changeable removing carbon material and carries out carbon materials
Expect pressure changeable removing, the purification of high temperature purification stove heating is sent into after removing, harvests high purity graphite；
Embodiment 3
Highly purified biogenic matter porous carbon is sent into the equipment that the present invention intervenes subcritical solvent pressure changeable removing carbon material to carry out
The removing of carbon material pressure changeable, harvests high-purity nm carbon material.
Claims (2)
1. a kind of equipment for intervening subcritical solvent pressure changeable removing carbon material, stores assembly (1) by powdery carbon material raw material, Gu
Liquid mixing assembly (2) vacuumizes assembly (3), and pressure changeable intercalation separating assembly (4), gas solid separation assembly (5), gas compression is total
At (6), heat exchange cooling unit (7), storage assembly (8) is constituted in solvent, it is characterized in that powdery carbon material raw material storage assembly (1)
It is connect by pipeline with solid-liquid mixing assembly (2), solid-liquid mixing assembly (2) separates (4) assembly by pipeline with pressure changeable intercalation
Connection vacuumizes assembly (3) and is connect by pipeline with solid-liquid mixing assembly (2) and pressure changeable intercalation separating assembly (4) threeway, become
Pressure intercalation separating assembly (4) is connect by pipeline with gas solid separation assembly (5), and gas solid separation assembly (5) passes through pipeline and gas
Body compresses assembly (6) connection, and gas compression assembly (6) is connect by pipeline with heat exchange cooling unit (7), and heat exchange is cooling total
It is connect by pipeline with solid-liquid mixing assembly (2) at (7), assembly (8) is store in solvent and pass through pipeline and heat exchange cooling unit (7)
It is connected with solid-liquid mixing assembly (2) threeway；
Powdery carbon material raw material stores assembly (1) by staving 1 (1-1), upper capping (1-2), gate valve 1 (1-5), metering isolating valve 1
(1-6), connecting tube 1, (1-7) pressure-equalizing pipe (1-4), pressure balance sluice valve 10 (1-3) are constituted；
(1-1) main body of staving 1 is cylinder, and lower part is inverted conical shape, and the upper end (1-7) of connecting tube 1 is fallen with the lower part staving 1 (1-1)
Cone top connection, the lower end (1-7) of connecting tube 1 is connect with the upper top surface of the staving 2 (2-3) of solid-liquid mixing assembly (2)；It is connecting
Gate valve 1 (1-5) is housed from the top down in pipe 1 (1-7), is measured isolating valve 1 (1-6)；The upper end of staving 1 (1-1) main body cylinder shape
Face, equipped with the openable upper capping (1-2) for being packed into powdery carbon material raw material；The pressure-equalizing pipe upper end (1-4) and staving 1 (1-1)
The connection of main body upper end, the pressure-equalizing pipe lower end (1-4) are connect with the upper top surface of the staving 2 (2-3) of solid-liquid mixing assembly (2), are put down
The powdery carbon material raw material that weighs stores the pressure of assembly (1) and solid-liquid mixing assembly (2), and pressure-equalizing pipe (1-4) is provided with pressure
It balances sluice valve 10 (1-3)；
Solid-liquid mixing assembly (2) is by staving 2 (2-3), blender (2-2), connecting tube 2 (2-1), gate valve 2 (2-4), 3 (7- of gate valve
1) isolating valve 4 (7-4), is measured, connecting tube 3, (8-2, metering isolating valve 3 (8-3) are constituted gate valve 4；
Staving 2 (2-3) is cylinder, and blender (2-2) is internal mounted in staving 2 (2-3), and blender (2-2) axis is from 2 (2- of staving
3) upper surface is stretched out and is driven by motor, and the one end (2-1) of connecting tube 2 is connect with the upper surface staving 2 (2-3), and connecting tube 2 (2-1) is another
One end goes out cold liquid mouth with heat exchange cooling unit (7) and connect, and 2 (2- of gate valve is housed at connecting tube 2 (2-1) nearly staving 2 (2-3) end
4) gate valve 3 (7-1), is housed at (2-1) near-thermal of connecting tube 2 exchange cooling unit (7) end, between gate valve 3 (7-1) and three ports
Equipped with metering isolating valve 4 (7-4)；The one end (8-1) of connecting tube 3 is connect with connecting tube 2 (2-1) threeway, and connecting tube 3 (8-1) is another
End is connect with storage assembly (8) in solvent；Assembly (8) end is store in connecting tube 3 (8-1) in nearly solvent, gate valve 4 (8-2) is housed, in lock
Equipped with metering isolating valve 3 (8-3) between valve 4 (8-2) and three ports；
It is that pressure-bearing receiver is commercialized in oneself that assembly (8) are store in solvent；
Pressure changeable intercalation separating assembly (4) is by diaphragm pump (4-2), connecting tube 4 (4-5), gate valve 5 (4-1), connecting tube 5 (4-6),
Gate valve 6 (4-7) is constituted, oneself is commercialized diaphragm pump (4-2), and the one end (4-5) of connecting tube 4 connects diaphragm pump (4-2) feed inlet, connection
(4-5) other end of pipe 4 connects the lower end surface of solid-liquid mixing assembly (2) staving 2 (2-3), the nearly diaphragm pump in connecting tube 4 (4-5)
End is equipped with gate valve 5 (4-1)；The one end (4-6) of connecting tube 5 connects diaphragm pump (4-2) discharge port, the connection of (4-6) other end of connecting tube 5
The cylindrical surface lower end of the staving 3 (5-1) of gas solid separation assembly (5), nearly diaphragm pump end is equipped with gate valve 6 in connecting tube 5 (4-6)
(4-7)；
Gas solid separation assembly (5) is by staving 3 (5-1), inclined plate isolator (5-5), purpose ceramic-film filter (5-7), 6 (5- of connecting tube
3), gate valve 7 (5-4) is measured isolating valve 2 (5-2), connecting tube 7 (5-9), and gate valve 8 (5-8) is constituted,
(5-1) main body of staving 3 is cylinder, and lower part is inverted conical shape, and the upper end (5-3) of connecting tube 6 is fallen with the lower part staving 3 (5-1)
Cone top connection, is equipped with gate valve 7 (5-4) from the top down in connecting tube 6 (5-3), measures isolating valve 2 (5-2)；Connecting tube 6
The lower end (5-3), which leads to atmosphere, sends out processing good material；In the internal upper semisection of staving 3 (5-1), from bottom to top equipped with oneself commercialization inclined plate
Isolator (5-5), purpose ceramic-film filter (5-7) is commercialized in oneself；The one end (5-9) of connecting tube 7 is connect with the upper surface staving 3 (5-1),
(5-9) other end of connecting tube 7 is connect with the gas compression pump steam inlet of gas compression assembly (6), nearly bucket in connecting tube 7 (5-9)
Body 3 (5-1) end is equipped with gate valve 8 (5-8)；
Oneself is configured with high pressure gas backwashing system at commercialization purpose ceramic-film filter (5-7)；
Gas compression assembly (6) is made of gas compression pump, connecting tube 8 (6-1),
Oneself is commercialized gas compression pump, and gaseous solvent propane, butane, R22, R134a etc. are compressed into liquid by gas compression pump, leads to
It crosses connecting tube 8 (6-1) and is sent into heat exchange cooling unit (7) hydrothermal solution import；
The own commercialization of heat exchange cooling unit (7)；
Assembly is vacuumized by vacuum pumping pump, connecting tube 9 (3-2) is constituted,
Oneself is commercialized vacuum pumping pump, and the one end (3-2) of connecting tube 9 is connect with vacuum pumping pump air inlet, connecting tube 9 (3-2) other end
It is connect with connecting tube 4 (4-5) threeway, gate valve 9 (3-1) is housed in connecting tube 9 (3-2) internal nearly vacuum pumping pump inlet port.
According to claim 1,2. carrying out carbon material pressure changeable using the equipment for intervening subcritical solvent pressure changeable removing carbon material
The technique of removing is for example following:
1.) primary condition is set, all valves of system are to close, and in following process, valve state is shown in that valve state table is said
It is bright；The staving 1 (1-1) of powdery carbon material raw material storage assembly (1) has been charged into powdery carbon material raw material, covers capping (1-2)；
2.) to solid-liquid mixing assembly (2), pressure changeable intercalation separating assembly (4), gas solid separation assembly (5) is vacuumized, and reaches technique
Stop vacuumizing after it is required that；
3.) to the staving 2 of solid-liquid mixing assembly (2), ((2-3) injects the subcritical solvent of liquid, wants cube to technique；Inject liquid
The subcritical solvent volume of state accounts for the (70-90% of (2-3) of staving 2
It is subcritical solvent selection propane, butane, No. four solvents (propane, butane mixture), a kind of in R22, R134a；
4.) to the staving 2 of solid-liquid mixing assembly (2), (powdery carbon material raw material, powdery carbon material raw material and liquid is added in (2-3)
Subcritical solvent solid-to-liquid ratio is required to technique；
The volume ratio 1:4-20 of powdery carbon material raw material and the subcritical solvent solid-liquid of liquid
Powdery carbon material is uniformly mixed with the subcritical stirring solvent of liquid；
5.) the powdery carbon material and the subcritical solvent mixture of liquid mixed quantitative and even is sent into diaphragm pump (4-2), every
The process requirement time is stopped in membrane pump diaphragm pump (4-2)；
The switch time of control gate valve 5 just controls mixed uniformly powdery carbon material and the subcritical solvent mixture of liquid is sent into
Diaphragm pump quantifies, the ETAD expected time of arrival and departure of gate valve 5 0.1-1 seconds；
It is stopped the process requirement time 3-60 seconds in mixed uniformly powdery carbon material and the subcritical solvent mixture diaphragm pump of liquid；
Mixture is in diaphragm pump (4-2) cavity due to the transformation stress effect that diaphragm vibrates up and down, mixture Subcritical solvent
It is converted between liquid and gaseous state, realizes intercalation stripping；
6.) the powdery carbon material of own intercalation stripping and the subcritical solvent mixture of liquid are sent into gas solid separation assembly (5), Asia is faced
Boundary's solvent under reduced pressure is in gaseous state, and the subcritical solvent of gaseous state is separated with the powdery carbon material of the own intercalation stripping of solid-state, the own intercalation stripping of solid-state
From powdery carbon material deposition the lower part inverted conical shape bucket bottom staving 3 (5-1) through metering isolating valve 2 (5-2) send out；
7.) decompression is in the subcritical solvent of gaseous state in gas solid separation assembly (5), through inclined plate isolator (5-5), purpose ceramic-film filter
It is then cold through heat exchange cooling unit (7) by the gas compressor of gas compression assembly (6) boil down to liquid again after (5-7) filtering
But it sends solid-liquid mixing assembly (2) back to, is recycled；
8.) the subcritical solvent of circulation losses is by storing assembly (8) Subcritical solvent make-up in solvent；
It sends the amount of the subcritical solvent of liquid of solid-liquid mixing assembly (2) back to, is sent into the amount of powdery carbon material raw material, and be added to Asia
The amount of critical solvent meets technique requirement；Metering and the own commercialization of proportional controlling device；
Each technique period valve state is for example following, and wherein "-" indicates that valve state is same as above a process or valve state changes not shadow
Ring production technology；
Upper table is illustrated:
When process f. is quantitatively packed into mixture to diaphragm pump, the switch time of control gate valve 5, the powdery carbon that quantitative and even is mixed
Material and the subcritical solvent mixture of liquid are sent into diaphragm pump；
When process g. intercalation stripping, control gate valve 5 and 6 shut-in time of gate valve, i.e. the powdery carbon material of control quantitative and even mixing
The process requirement time is stopped in diaphragm pump with the subcritical solvent mixture of liquid
Process h. is when sending to solid gas separation, program 6, program 7, and 8 automatic cycle of program carries out
Process j. release finished product when, close metering isolating valve 2, open gate valve 7, process material enter gate valve 7 with measure be isolated
6 inner space of connecting tube between valve 2, closing gate valve 7, rotary metering isolating valve 2 process material and are sent equipment；
Automatically the switch of above-mentioned valve is managed, so that it may the equipment for maintaining the present invention to intervene subcritical solvent pressure changeable removing carbon material
The technique for carrying out the removing of carbon material pressure changeable automatically continuously produces.
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Application publication date: 20190730 |