CN107321007A - A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide - Google Patents

A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide Download PDF

Info

Publication number
CN107321007A
CN107321007A CN201610278698.2A CN201610278698A CN107321007A CN 107321007 A CN107321007 A CN 107321007A CN 201610278698 A CN201610278698 A CN 201610278698A CN 107321007 A CN107321007 A CN 107321007A
Authority
CN
China
Prior art keywords
products pot
tower
inorganic salts
alcoholic solution
supercritical
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610278698.2A
Other languages
Chinese (zh)
Inventor
吴浩
金君素
刘洪涛
崔荣
李云
朱齐白
王丹
卢倩
彭超云
李响
王艳
方刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Original Assignee
Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou Institute for Advanced Materials Beijing University of Chemical Technology filed Critical Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Priority to CN201610278698.2A priority Critical patent/CN107321007A/en
Publication of CN107321007A publication Critical patent/CN107321007A/en
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

There is provided a kind of supercritical carbon dioxide the replaceable continuous method for preparing nano material, it is characterized in that as follows：Choose inorganic salts and be prepared into inorganic salts alcoholic solution with alcohols solvent；Add inorganic salts alcoholic solution is continuous first in tower from preparing tower upper feed inlet；By by CO2Added from tower top and the bottom charging aperture is prepared in tower, make CO2It is in a supercritical state；The alcohols material of inorganic salts alcoholic solution dissolves in supercritical CO in tower2And continuously discharged by preparing tower upper part discharge port；It is inorganic salt out after deposit to products pot；Products pot is deposited after 1/5-1/2 inorganic salt product, the switch closed on products pot connector；Products pot pressure is down to normal pressure；Products pot is separated with preparation tank；The nanometer grade powder material prepared in products pot is removed and nitrogen purging is carried out, remaining alcohols material is removed；Empty products pot is connected to preparation tank, and opens the switch of products pot connector, continues preparation procedure.Realize replaceable continuous preparation nano material.

Description

A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide
Technical field
The invention belongs to separate preparation field, a kind of replaceable continuous preparation nano material of supercritical carbon dioxide is related in particular to Method.
Background technology
Supercritical CO2The principle of fluid extraction (SFE) separation process is the pass of the solvability using supercritical fluid and its density System, i.e., the influence using pressure and temperature to supercritical fluid solvability and carry out.In the supercritical state, will be overcritical Fluid is contacted with material to be separated, make its selectively polarity size, boiling point height and molecular size range composition successively Extract.Certainly, the extract obtained by each pressure limit of correspondence is unlikely to be single, but can be obtained most with control condition The blending constituent of good ratio, then makes supercritical fluid become common gases, is extracted material then by the method for decompression, heating Wholly or substantially separate out, so that the purpose of separating-purifying is reached, so supercritical CO2Fluid extraction process is by extracting and separating What journey was combined.
Nano material broadly refers at least one-dimensional general name in nanoscale scope ultrafine particles material in three dimensions. According to the definition that October 18, EU Committee passed through in 2011, nano material is a kind of powdery being made up of basic granules or group Block natural or artificial material, one or more three-dimensional dimensions of this basic granules between 1 nanometer to 100 nanometers, and The total quantity of this basic granules accounts for more than 50% in all total number of particles of whole material.Nano material has certain uniqueness Property, when material yardstick it is small to a certain extent when, then the viewpoint that must use quantum mechanics substitution traditional mechanicses instead describes its behavior, When powder particle size is by being down to 10 nanometers for 10 microns, though its particle diameter changes into 1000 times, will then have when being converted into volume 10 9 powers times, so obvious difference will be produced in the two behavior.
The content of the invention
A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide, it is characterized in that as follows：Selection can dissolve in alcohol The inorganic salts of solution, inorganic salts alcoholic solution is prepared by mixing into alcohols solvent；Select supercritical CO2Continuously prepare nano-powder material Device (such as accompanying drawing 1) is used as preparation facilities；Added inorganic salts alcoholic solution is continuous first by high-pressure pump from preparing tower upper feed inlet Enter in tower, charging rate according to inorganic salts alcoholic solution concentration and output demand with setting；It is continuous by CO by gas compressor2From system Standby tower top and the bottom charging aperture is added in tower, and supercritical temperature and pressure and CO are set according to the species of alcohols material and action time2Plus Expect speed, make CO2It is in a supercritical state；Inorganic salts alcoholic solution and supercritical CO in tower2Alcohols in mixing, inorganic salts alcoholic solution Material dissolves in supercritical CO2And continuously discharged by preparing tower upper part discharge port；Successive sedimentation is extremely after inorganic salts are separated out in alcoholic solution Prepare the detachable products pot of tower bottom；Products pot is deposited after 1/5-1/2 inorganic salt product, closes opening on products pot connector Close, make to prepare tower and the closing of products pot UNICOM；Products pot relief valve is opened, products pot pressure is down to normal pressure；By products pot with Preparation tank is separated；The nanometer grade powder material prepared in products pot is removed and nitrogen purging is carried out, remaining alcohols material is removed； Empty products pot is connected to preparation tank, and opens the switch of products pot connector, continues preparation procedure.Realize replaceable continuous Prepare nano material.
Brief description of the drawings
Fig. 1 is that supercritical carbon dioxide continuously prepares nano material device and process schematic representation.A1：CO2Gas compression unit； A1-1：Gas compressor；A1-2：CO2Air inlet；A1-3：CO2Gas outlet；B1:Overcritical preparation unit；B1-1：Prepare Tower；B1-2：Detachable products pot；B1-3：Upper feed inlet；B1-4：Heating mantle；B1-5：Upper part discharge port；B1-6： Products pot connector (contains on/off switch)；B1-7：Products pot relief valve；B1-8：Bottom charging aperture
Embodiment
Embodiment 1：
Choose zinc oxide and be prepared by mixing into zinc oxide alcoholic solution with alcohol solvent, concentration is 10%；Select supercritical CO2It is continuous to prepare Nano-powder material device (such as accompanying drawing 1) is used as preparation facilities；It is by high-pressure pump that zinc oxide alcoholic solution is continuous from preparation first Tower upper feed inlet is added in tower, and charging rate is 10L/h；It is continuous by CO by gas compressor2Fed from tower top and the bottom are prepared In mouth addition tower, charging rate is 60m3Temperature is 170 DEG C in/h, tower, and tower pressure interior force 11MPa makes CO2In supercritical state State；Tower internal oxidition zinc alcoholic solution and supercritical CO2Ethanol in mixing, zinc oxide alcoholic solution dissolves in supercritical CO2And by preparing Tower upper part discharge port is continuously discharged；Successive sedimentation is to the detachable products pot for preparing tower bottom after zinc oxide is separated out in alcoholic solution； Products pot is deposited after 1/3 zinc oxide product, the switch closed on products pot connector, makes to prepare tower and the closing of products pot UNICOM； Products pot relief valve is opened, products pot pressure is down to normal pressure；Products pot is separated with preparation tank；By receiving for being prepared in products pot Rice zinc oxide level powder body material removes and carries out nitrogen purging, removes remaining ethanol；The products pot emptied is connected to preparation Tank, and the switch of products pot connector is opened, continue preparation procedure.Realize replaceable continuous preparation nano material.
Product can be detected that obtained material particle size is between 14-29 nanometers by electron microscope；Determined by BET Specific surface area is in 38.3m2/g。

Claims (1)

1. a kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide, it is characterized in that as follows：
Selection can dissolve in the inorganic salts of alcoholic solution, and inorganic salts alcoholic solution is prepared by mixing into alcohols solvent；Select supercritical CO2 Continuously nano-powder material device (such as accompanying drawing 1) is prepared as preparation facilities；Inorganic salts alcoholic solution is connected by high-pressure pump first Continue from preparing in tower upper feed inlet addition tower, charging rate according to inorganic salts alcoholic solution concentration and output demand with setting；Pass through Gas compressor is continuous by CO2Add in tower, set according to the species of alcohols material and action time from tower top and the bottom charging aperture is prepared Supercritical temperature and pressure and CO2Charging rate, makes CO2It is in a supercritical state；Inorganic salts alcoholic solution and supercritical CO in tower2 Alcohols material in mixing, inorganic salts alcoholic solution dissolves in supercritical CO2And continuously discharged by preparing tower upper part discharge port；Inorganic salts Successive sedimentation is to the detachable products pot for preparing tower bottom after being separated out in alcoholic solution；Products pot deposits 1/5-1/2 inorganic salt product Afterwards, the switch closed on products pot connector, makes to prepare tower and the closing of products pot UNICOM；Products pot relief valve is opened, by product Pressure tank is down to normal pressure；Products pot is separated with preparation tank；The nanometer grade powder material prepared in products pot is removed and nitrogen is carried out Air-blowing is swept, and removes remaining alcohols material；Empty products pot is connected to preparation tank, and opens the switch of products pot connector, Continue preparation procedure；Realize replaceable continuous preparation nano material.
CN201610278698.2A 2016-04-28 2016-04-28 A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide Pending CN107321007A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610278698.2A CN107321007A (en) 2016-04-28 2016-04-28 A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610278698.2A CN107321007A (en) 2016-04-28 2016-04-28 A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide

Publications (1)

Publication Number Publication Date
CN107321007A true CN107321007A (en) 2017-11-07

Family

ID=60192394

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610278698.2A Pending CN107321007A (en) 2016-04-28 2016-04-28 A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide

Country Status (1)

Country Link
CN (1) CN107321007A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110681857A (en) * 2019-10-18 2020-01-14 上海交通大学 Purification method of silver nanowires

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050107252A1 (en) * 2003-11-17 2005-05-19 Gaffney Anne M. Process for preparing mixed metal oxide catalyst
CN1671624A (en) * 2002-06-25 2005-09-21 阿尔堡大学 Method for production of a product having sub-micron primary particle size, product produced by the method and apparatus for use of the method
CN101264393A (en) * 2008-04-02 2008-09-17 东北林业大学 Water-soluble nano material supercritical carbon dioxide quick expanding preparing device
CN103214586A (en) * 2012-01-19 2013-07-24 中国科学院化学研究所 Redispersable nanoparticle powder material preparation method
CN104974557A (en) * 2015-07-10 2015-10-14 上海纳米技术及应用国家工程研究中心有限公司 Method for modifying ultrafine oxide powder by using supercritical carbon dioxide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1671624A (en) * 2002-06-25 2005-09-21 阿尔堡大学 Method for production of a product having sub-micron primary particle size, product produced by the method and apparatus for use of the method
US20050107252A1 (en) * 2003-11-17 2005-05-19 Gaffney Anne M. Process for preparing mixed metal oxide catalyst
CN101264393A (en) * 2008-04-02 2008-09-17 东北林业大学 Water-soluble nano material supercritical carbon dioxide quick expanding preparing device
CN103214586A (en) * 2012-01-19 2013-07-24 中国科学院化学研究所 Redispersable nanoparticle powder material preparation method
CN104974557A (en) * 2015-07-10 2015-10-14 上海纳米技术及应用国家工程研究中心有限公司 Method for modifying ultrafine oxide powder by using supercritical carbon dioxide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
廖传华等主编: "《超临界CO2流体萃取技术-工艺开发及其应用》", 31 July 2004, 化学工业出版社 *
张波等: "纳米氧化锌抗磨减磨添加剂的研究", 《润滑油》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110681857A (en) * 2019-10-18 2020-01-14 上海交通大学 Purification method of silver nanowires
CN110681857B (en) * 2019-10-18 2021-06-29 上海交通大学 Purification method of silver nanowires

Similar Documents

Publication Publication Date Title
CN209475639U (en) A kind of supercritical extraction unit
CN105013587A (en) Freeze grinding system
CN107321007A (en) A kind of replaceable continuous method for preparing nano material of supercritical carbon dioxide
CN204093257U (en) Coating raw material powder collecting device
CN101250268B (en) Preparation method of super-fine powdery wax
CN101264393B (en) Water-soluble nano material supercritical carbon dioxide quick expanding preparing device
CN104128096A (en) Ultrasound-assisted method and device for extracting nano-particles from nano-powder organic solvent suspension liquid
CN206051975U (en) Subcritical continuous extraction desolventizing equipment
CN107335252A (en) A kind of replaceable continuous method for preparing nano zinc oxide material of supercritical carbon dioxide
CN106623952B (en) A kind of titanium of the micro- hydrogenation in surface or the preparation method of titanium alloy powder
CN101264431A (en) Water-soluble nano material supercritical carbon dioxide anti-solvent preparing device
CN102688608A (en) Method for recovering mesoporous molecular sieve organic template
CN207287729U (en) A kind of hydrocyclone steady flow system
US9480964B2 (en) Device and method for producing suspensions or wet pastes of nanopowders or ultra-fine powders
CN202638358U (en) Dust dissolution boosting device through pressure conveying
CN206731027U (en) A kind of facial mask emulsion synthesizes filling production lines
CN203972104U (en) A kind of micro mist overflow size separation tank
CN107308686A (en) A kind of method that supercritical carbon dioxide continuously prepares nanometer titanic oxide material
CN110108538A (en) Adding pressure type salinized soil desalter
Nandiyanto et al. Economic Evaluation of the Production Magnesium Oxide Nanoparticles via Liquid-Phase Route
CN110330023B (en) Preparation and drying method of magnesium trisilicate
CN107311221A (en) A kind of method that supercritical carbon dioxide continuously prepares nano zinc oxide material
US20100136149A1 (en) Method for producing vegetable cell sap concentrate and means for the production thereof
CN206730565U (en) A kind of medicinal material extract equipment for extraction of classifying
CN107308685A (en) A kind of method that supercritical carbon dioxide continuously prepares nano material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20171107

WD01 Invention patent application deemed withdrawn after publication