CN101310846B - supercritical fluid-cosolvent deposition method for preparing nano composite material reactor - Google Patents
supercritical fluid-cosolvent deposition method for preparing nano composite material reactor Download PDFInfo
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- CN101310846B CN101310846B CN2008100103712A CN200810010371A CN101310846B CN 101310846 B CN101310846 B CN 101310846B CN 2008100103712 A CN2008100103712 A CN 2008100103712A CN 200810010371 A CN200810010371 A CN 200810010371A CN 101310846 B CN101310846 B CN 101310846B
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- 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
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- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a reactor which adopts a supercritical fluid-cosolvent sedimentation method for preparing nanocomposites and essentially consists of a reactor shell body, a carrier charging basket, a top cover of the charging basket, a feed inlet and a feed outlet, a reactor end cover and a seal washer; a toroidal platform in which the carrier charging basket is arranged is arranged at the place 3/7 to 2/3 high away from the bottom of the reactor. A supporting plate at the bottom of the charging basket and a cover plate at the top of the charging basket are respectively cut with a plurality of orifices, and the top cover of the charging basket and a basket body are connected by adopting clamping type fast-assembly structure. Filter paper, absorbent cotton, or polymer film is spread on the bottom of the charging basket. Two side walls of the reactor shell body are respectively provided with the feed inlet and the feed outlet which are both positioned above the carrier charging basket; the bottom of the reactor is the structure of a round plane while the end part of the reactor is ring-grooved structure. An end cover and the shell body are connected by screw thread; the seal washer is positioned between the shell body and the end cover and is O-shaped self-tightening seal structure. The reactor of the invention has the advantages that carriers and solution do not directly contact each other, the structure is simple and the processing, production and disassembly are convenient, with reliable high-pressure sealing.
Description
Technical field
The present invention relates to Composite Preparation technology and green process equipment technology field, relate in particular to a kind of supercritical fluid-cosolvent sedimentation and prepare nano composite material reactor.
Background technology
Supercritical fluid deposition (Supercritical Fluid Deposition, SFD) technology is a kind of new method for preparing nano composite material of development in recent years, compare with the traditional preparation process method, aspect control particle size, Size Distribution and the content of metal huge advantage is being arranged, be a kind of advanced person's the method for preparing nano composite material, be subjected to increasing attention.Compare with existing nano composite material preparation method, the supercritical fluid deposition method possesses advantages such as zero surface tension, diffusivity is good, solvent removal is easy.
The many employings of preparation composite at present are placed on predecessor, solvent, carrier (base material) in the reactor and adopt and stir so that mix, use such reactor, no matter be normal pressure or operation with high pressure, all have obvious defects: carrier needed post processings such as complex surfaces cleaning after (1) preparation was finished, so that unnecessary solvent, predecessor etc. are removed; (2), must adopt methods such as high-temperature roasting or freeze drying to realize desolventizing for the liquid of small amount of residual in inside, carrier duct is removed fully.Facts have proved that regular meeting produces defective or destructions such as ftractureing, cave in because of the surface tension of liquid and the nano-micro structure that capillarity causes carrier like this, preparation brings serious puzzlement to nano composite material.
Summary of the invention
The purpose of this invention is to provide a kind of supercritical fluid-cosolvent sedimentation and prepare nano composite material reactor, this inside reactor is provided with a special charging basket, be used to hold carrier, isolate carrier and solvent, and play overcritical cosolvent solution to be in contact with one another and do not influence the effect that it freely spreads in the carrier micropore with carrier, this structure of reactor is simple, be convenient to processing and manufacturing, easy accessibility, high pressure sealing is reliable.
In order to achieve the above object, technical scheme of the present invention is as follows:
The supercritical fluid-cosolvent sedimentation prepares nano composite material reactor and mainly is made up of reactor shell 1, carrier charging basket 2, charging basket top cover 3, charging aperture and discharging opening 4, reactor end cap 5 and seal washer 6; At distance reactor bottom 3/7～2/3 height and position place, be provided with the annular platform that is used to place carrier charging basket 2, all offer a plurality of apertures on the bottom support panel of carrier charging basket 2 and the top blind flange, charging basket top cover 3 adopts the cassette quick fixation structure to be connected with basket, and filter paper, absorbent cotton or macromolecule membrane are laid in the charging basket bottom; Be respectively equipped with charging aperture and discharging opening 4 on the two side of reactor shell 1, charging aperture and discharging opening 4 all are positioned at the top of carrier charging basket 2; Reactor bottom is the circular flat structure, and the end of reactor shell 1 is a ring shaped slot shape structure, adopts between reactor end cap 5 and the reactor shell 1 to be threaded; Seal washer 6 is O type circle self-tightening sealing structure between reactor shell 1 and reactor end cap 5.
Above-mentioned reactor shell 1 employing 1Cr18Ni9Ti model stainless steel or 316 model stainless steels or 316L model stainless steel or 304 model stainless steel materials are made; Described reactor end cap 5 is provided with an outer-hexagonal cap; Described seal washer 6 adopts silicon rubber or polytetrafluoroethylmaterial material to make.
Beneficial effect of the present invention is as follows:
1) overcome fundamentally that carrier material is big because of solvent contamination, the solvent residual amount that direct contact solution causes, caused destructions such as structure is caved in, cracking in the dry run;
2) utilize that reactor of the present invention can prepare that particle size is little, narrow size distribution, finely dispersed nano composite material;
3) structure of reactor compactness of the present invention is easy and simple to handle, good seal performance, and control is convenient;
4) carrier is collected convenient, free of losses;
5) low cost of manufacture.
Description of drawings
Fig. 1 is a reactor general assembly drawing of the present invention.
Fig. 2 is the structural representation of reactor shell of the present invention.
Fig. 3 is the partial enlarged drawing of reactor shell hermetically-sealed construction I of the present invention.
Fig. 4 is that the A-A of Fig. 2 is to view.
Fig. 5 is a splendid attire carrier charging basket assembling schematic diagram of the present invention.
Fig. 6 is a charging basket basket bottom structure schematic diagram of the present invention.
Fig. 7 is the front view of charging basket basket structure of the present invention.
Fig. 8 is the vertical view of charging basket basket structure of the present invention.
Among the figure: 1, reactor shell, 2, the carrier charging basket, 3, the charging basket top cover, 4, charging aperture and discharging opening, 5, the reactor end cap, 6, seal washer, 7, basket, 8, the basket base plate.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is done description in further detail:
To shown in Figure 8, supercritical fluid-cosolvent sedimentation of the present invention prepares nano composite material reactor and mainly is made up of reactor shell 1, carrier charging basket 2, charging basket top cover 3, charging aperture and discharging opening 4, reactor end cap 5 and seal washer 6 as Fig. 1; Be respectively equipped with charging aperture and discharging opening 4 on the two side of reactor shell 1; At annular platform of distance reactor bottom 3/7～2/3 above height and position design, in order to place the charging basket 2 of splendid attire carrier; Charging basket 2 is all offered the aperture of some, as the diffusion admittance of supercritical fluid through particular design on bottom support panel and the top blind flange; Charging basket top cover 3 adopts the cassette quick fixation structure to be connected with basket 7; Filter paper, absorbent cotton or macromolecule membrane are laid in the charging basket bottom, in case carrier exposes; Reactor bottom is designed to the circular flat structure, is convenient to magnetic stick and can rotates freely in reactor; Charging aperture and discharging opening 4 all are arranged on the place, top that the high pressure cylinder lateral wall is positioned at charging basket 2; Adopt between reactor head 5 and the cylindrical shell 1 to be threaded, be convenient to dismounting; Seal washer 6 is an O type circle self-tightening sealing structure, and O type circle adopts silicon rubber or polytetrafluoroethylene (PTFE) class material; The stainless steel manufacturing of reactor body material, material can be selected 1Cr18Ni9Ti, 316,316L, 304 etc.; An outer-hexagonal cap is set, so that end cap can be screwed on the reactor end cap 5 with spanner.
During experiment, carrier is put in the charging basket 2, and predecessor is put in reactor bottom, under design temperature, feeds CO by charging aperture
2To a certain pressure, closed reactor by the pressure release of other end discharging opening, took out sample and handles postmenstruation after a period of time, can obtain required nano composite material, this reactor can be under the condition of the highest 200 ℃, 50MPa continuous operation 24 hours at least.
As shown in Figure 1, it is the total structure schematic diagram of reactor of the present invention, and H1=70mm is the charging basket position dimension, in order to be used for supporting the height of charging basket platform on definite reactor wall; H2=90mm is that charging aperture and discharging opening 4 are apart from reactor bottom surface height dimension, in order to the position of determining that feed inlet and outlet is taken over, charging aperture and discharging opening 4 all are arranged on the place, top that the high pressure cylinder lateral wall is positioned at charging basket 2, impact when layout can be avoided charging like this and cause problems such as liquid entrainment during pressure release, in order to seal reliable and easy accessibility, can be designed to conical surface seal, screw connection structure, feed inlet and outlet is taken over and is inserted high pressure cylindrical shell and concordant with internal face, and extension is for taking over end face to cylinder body outer wall face 20mm.H3=150mm defines the real space height after reactor is installed, and is the characteristic size of reactor; L1=20mm stretches out the length dimension of reactor outside wall surface for taking over; L2=30mm * 26mm is the overall size of hexagonal boss on the end cap 5, and its height H 5=15mm is so that can screw end cap with spanner; H4=42mm is the end cap overall height; D2=60mm is the end cap outside diameter, and the internal thread of processing M52 * 1.5 on the inner cylinder face connects; D1=52mm is the cylindrical shell external diameter.
As shown in Figure 2, it is the reactor shell structure diagram.Reactor body material selection stainless steel is made, and material can be selected 1Cr18Ni9Ti, 316,316L, 304 etc.; Reactor bottom is designed to the circular flat structure, and adopts the round-corner transition of r1=2mm, is convenient to magnetic stick and can rotates freely in reactor; Adopt between reactor head and the cylindrical shell to be threaded, be convenient to dismounting, thread size is M1=M52 * 1.5, length H7=18mm; At annular platform of distance reactor bottom H1=70mm place design, in order to place the charging basket of splendid attire carrier; In order to guarantee to cut down finished cost, reduce the influence that stress is concentrated, adopt the round-corner transition of r1=2mm; D4=35mm, d5=30mm, H9=16mm, H10=36mm, C1=1 * 45 ℃, r1=2mm, cylindrical shell height overall H6=110mm; Offer 2 in the hole of d3=8.5mm along 180 ° of directions at the H2=90mm place, and the platform that ream is put down into H11=10mm in the about deeply L3=3mm scope of drum outer wall face, tube base thickness degree H8=8.5mm.
As shown in Figure 3, it is a cylindrical shell hermetically-sealed construction sketch.This hermetically-sealed construction is the high pressure self-fastening sealing structure, its advantage be if with the high pressure end cap fastening after, then the sealing effectiveness of sealing ring is highly stable and the high more effect of pressure is good more; High pressure sealing is an O type circle self-tightening sealing structure, and O type circle adopts silicon rubber or polytetrafluoroethylene (PTFE) class material; Processing diameter d 6=39mm on cylindrical shell, the groove of depth H 12=2mm, the groove bottom roughness is C2=1.6; Screw thread outer rim chamfer dimesion C1=1 * 45 °, groove width L4=4.5mm.
As shown in Figure 4, its be the A-A of Fig. 2 to view, on cylindrical shell, be two planes of processing, H9=16mm to H10=36mm place apart from the cylindrical shell bottom level, make that two plane distances are L5=49mm, being convenient to when fastening can be with spanner or vice class tool holder.
As shown in Figure 5, it is the charging basket assembly drawing, and it act as the splendid attire carrier and the liquid of carrier and reactor bottom is isolated; For this reason, charging basket is all offered the aperture of some, as the diffusion admittance of supercritical fluid through particular design on bottom support panel and the top blind flange; Assembling back height H 14=11mm, external diameter L6=34mm by the stainless steel manufacturing, adopts between the basket end and the basket to be welded to connect, can spot welding also can seal weld; Filter paper, absorbent cotton or macromolecule membrane are laid in the charging basket bottom, in case carrier leaks outside, material is a stainless sheet steel, can prevent that material is contaminated.
As shown in Figure 6, it is a charging basket basket bottom structure sketch.Thickness of slab H13=2mm is covered with diameter 1mm, the aperture of L7=3mm at interval according to equilateral triangle on base plate, be used for the supercritical fluid that distributes.
As shown in Figure 7, it is a charging basket basket sketch.The charging basket top cover adopts the cassette quick fixation structure to be connected with basket, makes height H 15=8mm by the high stainless steel short cylinder of 9mm, base size C1=1 * 45 ° designs fast-assembling cassette physical dimension H17=1mm for convenient with the base plate welding, H16=2mm, d9=30mm, L6=34mm.
As shown in Figure 8, it is the basket vertical view.Process 3 grooves a=25 ° wide at 120 ° of intervals, last outer rim place, guarantee size d8=32mm, be used for opening soon and be connected with charging basket.
Supercritical fluid-cosolvent sedimentation of the present invention prepares nano composite material reactor, on the one hand, can overcome the direct mixing of carrier and predecessor and solvent, makes things convenient for carrier to collect, avoid the carrier secondary pollution; On the other hand, utilize its preparation nano composite material efficient height, solvent adds micro-cosolvent with supercritical carbon dioxide or supercritical carbon dioxide, and surface tension is zero, diffusion property is superior; Can realize separating of solvent and carrier simply by slow step-down, needn't carry out drying again and handle, can not have any impact carrier structure.In addition, condition such as the pressure by the conditioned reaction device, temperature, reaction time, material proportion just can accomplish that the key technical indexes such as pattern, loading of metallic in the composite is optional, controlled.
Claims (4)
1. be used for the reactor that the supercritical fluid-cosolvent sedimentation prepares nano composite material, it is characterized in that this reactor mainly is made up of reactor shell (1), carrier charging basket (2), charging basket top cover (3), charging aperture and discharging opening (4), reactor end cap (5) and seal washer (6); At distance reactor bottom 3/7～2/3 height and position place, be provided with the annular platform that is used to place carrier charging basket (2), all offer a plurality of apertures on the bottom support panel of carrier charging basket (2) and the top blind flange, charging basket top cover (3) adopts the cassette quick fixation structure to be connected with basket, and filter paper, absorbent cotton or macromolecule membrane are laid in the charging basket bottom; Be respectively equipped with charging aperture and discharging opening (4) on the two side of reactor shell (1), charging aperture and discharging opening (4) all are positioned at the top of carrier charging basket (2); Reactor bottom is the circular flat structure, and the end of reactor shell (1) is a ring shaped slot shape structure, adopts between reactor end cap (5) and the reactor shell (1) to be threaded; Seal washer (6) is positioned between reactor shell (1) and the reactor end cap (5), is O type circle self-tightening sealing structure.
2. as claimed in claim 1ly be used for the reactor that the supercritical fluid-cosolvent sedimentation prepares nano composite material, it is characterized in that described reactor shell (1) adopts stainless steel material to make.
3. as claimed in claim 1ly be used for the reactor that the supercritical fluid-cosolvent sedimentation prepares nano composite material, it is characterized in that described reactor end cap (5) is provided with an outer-hexagonal cap.
4. as claimed in claim 1ly be used for the reactor that the supercritical fluid-cosolvent sedimentation prepares nano composite material, it is characterized in that described seal washer (6) adopts silicon rubber or polytetrafluoroethylmaterial material to make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100103712A CN101310846B (en) | 2008-02-03 | 2008-02-03 | supercritical fluid-cosolvent deposition method for preparing nano composite material reactor |
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| CN101310846A CN101310846A (en) | 2008-11-26 |
| CN101310846B true CN101310846B (en) | 2010-12-15 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102764626A (en) * | 2012-08-17 | 2012-11-07 | 上海应用技术学院 | Fastening structure for sealing portion of reaction kettle |
| CN103818918A (en) * | 2014-02-25 | 2014-05-28 | 大连理工大学 | Method for preparing high-dispersion nanocomposite in liquid, supercritical and near-critical CO2 through induction of inorganic acid |
| CN106622355A (en) * | 2017-01-17 | 2017-05-10 | 大连理工大学 | Copper-based nanocomposite controllable preparation method based on fine gradient desorption kinetics |
| CN111569780B (en) * | 2020-05-24 | 2021-12-28 | 西安交通大学 | Internal mixing type supercritical hydrothermal synthesis nano powder reactor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6689700B1 (en) * | 1999-11-02 | 2004-02-10 | University Of Massachusetts | Chemical fluid deposition method for the formation of metal and metal alloy films on patterned and unpatterned substrates |
| CN1763242A (en) * | 2004-10-19 | 2006-04-26 | 东京毅力科创株式会社 | Deposition method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6689700B1 (en) * | 1999-11-02 | 2004-02-10 | University Of Massachusetts | Chemical fluid deposition method for the formation of metal and metal alloy films on patterned and unpatterned substrates |
| CN1763242A (en) * | 2004-10-19 | 2006-04-26 | 东京毅力科创株式会社 | Deposition method |
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Granted publication date: 20101215 Termination date: 20110203 |