CN101099949A - Composite nozzle for preparing supercritical fluid nanometer micrometer materail - Google Patents
Composite nozzle for preparing supercritical fluid nanometer micrometer materail Download PDFInfo
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- CN101099949A CN101099949A CNA2006100452860A CN200610045286A CN101099949A CN 101099949 A CN101099949 A CN 101099949A CN A2006100452860 A CNA2006100452860 A CN A2006100452860A CN 200610045286 A CN200610045286 A CN 200610045286A CN 101099949 A CN101099949 A CN 101099949A
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Abstract
The present invention relates to superfine powder preparing apparatus, and is especially one kind of combined supercritical fluid nozzle for preparing superfine material. The combined supercritical fluid nozzle consists of end caps, moving ring, inner fixed mixing ring, outer fixed mixing ring, crystallizer, and other basic members. It may be assembled into a multichannel internal mixing nozzle, a multichannel external mixing nozzle, a multichannel internal-external mixing nozzle or a fast expanding nozzle for jetting material and mixing materials. The present invention has compact structure, small size, easy manufacture, wide application range and other advantages.
Description
One, technical field
The invention belongs to nano and micro materials or ultrafine powder prepares equipment, specially refer to a kind of composite nozzle for preparing supercritical fluid nanometer micrometer materail.
Two, background technology
At present the supercritical fluid nano and micro materials prepares that nozzle bore mostly is elongated hole greatly in the equipment, is made by methods such as laser borings, guarantees very little aperture thus.But this conventional structure nozzle processing difficulties, the manufacturing cost height; And because material has part to separate out easily at the nozzle bore place, be easy to block, be difficult for mediation; Because nozzle bore is very little, circulation area is very little, although adopts a plurality of nozzles, also is difficult to improve the preparation output of nano and micro materials, production efficiency is low; In addition,, in experiment and production process, be difficult to adapt to the variation of process conditions, particularly need to change circulation area and when reaching corresponding flow regime, can only adopt the nozzle of replacing different size to realize because nozzle bore can not regulate.
China Intellectual Property Office accepts in March, 2005, and application number is CN200510042540.1, and name is called " internal-mixing supercritical fluid nano and micro materials prepares nozzle "; With application number be CN 200510042541.7, name is called " exterior mixing supercritical fluid nano and micro materials prepares nozzle "; Reaching the application number of accepting in May, 2005 is CN200510043476.4, and name is called " the internal and external mixing type and super-critical fluid jetting nano and micro materials prepares nozzle "; Solve present supercritical fluid nano and micro materials preferably and prepared the above problem that exists in the equipment.
The above-mentioned nozzle of applying for is adjustable annular space formula nozzle, is made of awl end cover and nozzle core, awl end cover and awl end cover etc., and superposes, installs and combine according to the requirement of material hybrid mode.
Internal-mixing nozzle is that multiple solution is imported respectively in a plurality of nozzles, the solution of previous nozzle sprays into current nozzle, spray into next nozzle after being mixed together with solution in the current nozzle, with spray into again the next nozzle and the solution rapid mixing of next nozzle again after the solution rapid mixing of next nozzle again, by that analogy, mix the back fully until all solution and spray at a high speed, enter same crystallizer from last nozzle.Multiple solution is by a plurality of annular space formula nozzles, and enters same crystallizer after mixing in nozzle, carries out crystallization and prepares nano and micro materials.
Outer mixed mode nozzle is that multiple solution is imported respectively in a plurality of nozzles, and a plurality of nozzles spray into same injection channel simultaneously with multiple solution, enters same crystallizer after mixing outside nozzle, carries out crystallization and prepares nano and micro materials.
The nozzle of being made up of internal-mixing and two kinds of hybrid modes of exterior mixing is interior outer mixed mode nozzle.
The nozzle that adjustable annular space nozzle has replaced laser boring to make has solved the easy blocking problem of nozzle, has simplified processing technology, has improved the nozzle precision.Utilize two slits between the adjustable taper seat to form nozzle; the ejection material; the nozzle bore structural change that routine is fixing is a ring-type expanding slot structure; can not only finish the particulate preparation of single solute; can also realize the preparation of the synthetic particulate of ultra micro; have wide adaptability, easy to adjust, characteristics such as be easy to accomplish scale production.
Because adjustable annular space nozzle constitutes by boring end cover and nozzle core, awl end cover and awl end cover etc., and requires to superpose, install combination according to the material hybrid mode.When making the nozzle that mixes multiple solution, the stack combinations of nozzle arrangement increases the radial dimension of nozzle, has increased processing, installation difficulty, especially is not suitable for the crystallizer than minor diameter.The annular space adjustment means of this new type nozzle is placed into crystallizer inside, and the adjusting of annular space can be carried out after needing shut-down operation, system's release and pulling down nozzle, and complicated operation, efficient are low.
Three, summary of the invention
The objective of the invention is to overcome the deficiency of foregoing invention, the version of the adjustable annular space formula nozzle radial expansion that constitutes is overlapped etc. in change by awl end cover and nozzle core, awl end cover and awl end, according to processing, manufacturing, easy to assembly, operate, adjust fast and requirement efficiently, design one cover nozzle clearance can be adjusted in the crystallizer random external, the nozzle basic building block that installation dimension is unified, make the nozzle can axial expansion, and can press the mixed form that supercritical fluid nano and micro materials preparation technology needs, the built up nozzle of selecting basic building block to make up, install.
Basic design of the present invention is: by end cap, rotating ring, interior mixed stationary ring, mix basic building blocks such as stationary ring, crystallizer (claiming gatherer again), adjusting nut, spacer sleeve, sealing ring, connector outward and constitute, requirement according to supercritical fluid nano and micro materials preparation technology, select above installation dimension unified basic building block assembling multichannel internal-mixing nozzle, multichannel outer mixed mode nozzle, the inside and outside mix nozzle of multichannel for use, and the rapid expanding nozzle:
The multichannel internal-mixing nozzle is made up of following basic building block: mix stationary ring and at least 2 rotating rings, crystallizer at least in the end cap, 1, be connected and installed to be fixed together by connector and constitute; In the link position of end cap and rotating ring reaches, mix the link position of stationary ring and rotating ring, adjusting nut is installed;
The multichannel outer mixed mode nozzle is made up of following basic building block: end cap, at least 1 be outer to mix stationary ring and at least 2 rotating rings, crystallizer, is connected and installed to be fixed together by connector to constitute; Outside the link position of end cap and rotating ring reaches, mix the link position of stationary ring and rotating ring, adjusting nut is installed;
The inside and outside mix nozzle of multichannel is made up of following basic building block: mix stationary ring and at least 3 rotating rings and at least 1 outer mixed stationary ring in the end cap, at least 1, crystallizer is connected and installed to be fixed together by connector and constitutes; The link position of end cap and rotating ring and in mix stationary ring and rotating ring link position and outside the link position of mixed stationary ring and rotating ring, the installation adjusting nut;
The rapid expanding nozzle is made up of following basic building block: end cap, 1 rotating ring, and crystallizer is connected and installed to be fixed together by connector and constitutes; At the link position of end cap and rotating ring, adjusting nut is installed.
End cap, rotating ring, interior mixed stationary ring, mixing mounting means between the installation position of stationary ring, crystallizer outward, is use the rim of the mouth close fit, adds sealing ring at binding site and seals.The crystallizer installation position is a ring flange, ring flange can be built-in also can external end at crystallizer.
End cap, rotating ring, interior mixed stationary ring, mix the ring flange of stationary ring, crystallizer outward, it all is disc-shape, its connecting portion all has the hole of unified installation connector, in the mode that is slidingly matched spacer sleeve is installed in the hole of installation connector on the rotating ring, the height of spacer sleeve is greater than the thickness of rotating ring, and its difference is the regulated quantity of nozzle clearance; The nozzle that assembles is connected and fixed with connector.
The taper seat that matches between the adjacent rotating ring with it of end cap, the adjacent stationary ring with it of rotating ring forms adjustable annular space, by spacer sleeve and connector it is assembled together between end cap and stationary ring, stationary ring and the stationary ring, pass through adjusting nut, rotating ring is moved up and down along spacer sleeve, regulate annular space and lock by locking member, to reach the requirement of nano and micro materials preparation to nozzle clearance, realize a kind of simple injection of material, two kinds and two or more materials interior mix, mix outward, inside and outside mixing, and the multiple composite injection of rapid expanding.
The present invention, compact conformation, volume is less, processing, manufacturing, easy to assembly; Can realize dynamically adjusting nozzle clearance, operation, adjust quick and efficient, wide accommodation.
Four, description of drawings
Fig. 1 is the end cover structure schematic diagram;
Fig. 2 is interior mixed stationary ring structural representation;
Fig. 3 is the outer stationary ring structural representation that mixes;
Fig. 4 is the rotating ring structural representation;
Fig. 5 is a multichannel internal-mixing nozzle structural representation;
Fig. 6 is a multichannel outer mixed mode nozzle structural representation;
Fig. 7 is an exterior mixing nozzle arrangements schematic diagram in the multichannel;
Fig. 8 is a rapid expanding nozzle arrangements schematic diagram.
Reference numeral:
1 end cap, the 1-1 feeding-passage, the 1-2 connecting pore, 1-3 regulates screw thread, 1-4 cloth annular groove, 1-5 conical boss, 1-6 rim of the mouth, the 2 interior stationary rings that mix, the 2-1 feeding-passage, 2-2 rim of the mouth, 2-3 center of orifices, 2-4 conical boss, 2-5 cloth hole, the 2-6 connecting pore, the 2-7 conical boss, 2-8 regulates screw thread, 3 outer stationary ring, 3-1 feeding-passage, 3-2 rim of the mouth, the 3-3 through holes of mixing, 3-4 cloth annular groove, 3-5 connecting pore, 3-6 conical boss, 3-7 regulates screw thread, 4 rotating rings, 4-1 seal groove, the 4-2 boss, 4-3 connecting pore, 4-4 conical bore, 4-5 regulates screw thread, 5 adjusting nuts, 6 spacer sleeves, 7 sealing rings, 8 connectors, 9 crystallizers.
Five, the specific embodiment
Be described in detail embodiments of the present invention in conjunction with the accompanying drawings:
1, embodiment one: select mix nozzle in triple channel of basic building block assembling for use.
As shown in Figure 5, select for use in the end cap 1, two and mix stationary ring 2 and three rotating rings 4, with 9 assemblings of a crystallizer.Installation process is:
The adjusting screw thread 4-5 of first rotating ring 4 installs adjusting nut 5, adjusting screw thread 1-3 on the adjusting nut 5 upside precession end caps 1, the rotation direction of regulating screw thread 1-3 is opposite with the rotation direction of regulating screw thread 4-5, adjusting nut 5 revolves about being, the upside boss 4-2 of end cap 1 rim of the mouth 1-6 and rotating ring 4 is installed together simultaneously, and sealing ring 7 is installed in the seal groove 4-1; The downside boss 4-2 of rotating ring 4 and first interior upside rim of the mouth 2-2 that mixes stationary ring 2 are installed together, and the center of orifices 2-3 mouth of interior mixed stationary ring 2 is upwards installed sealing ring 7 in the seal groove 4-1 of rotating ring 4, the interior spacer sleeve 6 of installing of connecting pore 4-3;
Mix second adjusting nut 5 of adjusting screw thread 2-8 precession of stationary ring 2 in first, opposite side with the adjusting screw thread 4-5 precession adjusting nut 5 of second rotating ring 4, the rotation direction of regulating screw thread 2-8 is opposite with the rotation direction of regulating screw thread 4-5, adjusting nut 5 revolves screw thread about being, downside rim of the mouth 2-2 of mixed stationary ring 2 and the upside boss 4-2 of second rotating ring 4 are installed together in first simultaneously, sealing ring 7 is installed in the seal groove 4-1, second spacer sleeve 6 is installed in the connecting pore 4-3;
The upside rim of the mouth 2-2 that mixes stationary ring 2 in the downside boss 4-2 of second rotating ring 4 and second is installed together, and sealing ring 7 is installed in the seal groove 4-1 of rotating ring 4, and spacer sleeve 6 is installed in the connecting pore 4-3;
Mix the 3rd adjusting nut 5 of adjusting screw thread 2-8 precession of stationary ring 2 in second, opposite side with the adjusting screw thread 4-5 precession adjusting nut 5 of the 3rd rotating ring 4, the rotation direction of regulating screw thread 2-8 is opposite with the rotation direction of regulating screw thread 4-5, adjusting nut 5 revolves about being, simultaneously mix the downside rim of the mouth 2-2 of stationary ring 2 in second and the upside boss 4-2 of the 3rd rotating ring 4 is installed together, sealing ring 7 is installed in the seal groove 4-1, the 3rd spacer sleeve 6 is installed in the connecting pore 4-3;
The downside boss 4-2 of the 3rd rotating ring 4 and the rim of the mouth of crystallizer 9 are installed together, and sealing ring 7 is installed in the seal groove 4-1;
Because nozzle basic building block installation dimension is unified, the connecting pore of the connecting portion of the end cap of this combination, rotating ring, interior mixed stationary ring and crystallizer ring flange connecting pore all are the circular hole of four circumference uniform distributions, spacer sleeve 6 is installed in each connecting pore 4-3, at this moment four groups of spacer sleeve 6 endoporus are alignd respectively with end cap and stationary ring connecting pore, pierce into screw rod, the pad upper gasket, clamp nut, screw rod, packing ring and nut are formed connector 8, and sub-assembly is fixed together, and mix nozzle has installed in the triple channel.
The conical boss 1-5 of the end cap 1 of mix nozzle and the conical bore 4-4 of first rotating ring 4 in the mounted triple channel, mix the downside conical boss 2-7 and conical bore 4-4 of second rotating ring 4 of stationary ring 2 in first, the downside conical boss 2-7 of mixed stationary ring 2 and the conical bore 4-4 of the 3rd rotating ring 4 have constituted three nozzle clearances in second; Because the height of spacer sleeve is greater than the thickness of rotating ring, its difference is the regulated quantity of nozzle clearance, and the matching relationship of connecting pore 4-3 and spacer sleeve 6 is for being slidingly matched, so, rotating 5, three rotating rings 4 of three adjusting nuts respectively can move up and down along spacer sleeve 6, can adjust three nozzle clearances respectively; Adjust back locking adjusting nut 5.
Mix the method supercritical fluid in the triple channel and prepare the nano and micro materials technical process: carbon dioxide is through common supercritical carbon dioxide production method, promptly earlier carbon dioxide refrigeration is liquefied, reach more than the critical pressure by force (forcing) pump pressurization, enter heater again and the carbon dioxide temperature is brought up to formed supercritical carbon dioxide more than the critical-temperature; If the single material nano and micro materials of preparation is passed into mixed stationary ring feeding-passage 2-1 in first, second with supercritical carbon dioxide; Material is dissolved in the solvent that dissolves each other with supercritical carbon dioxide, throw end cap feeding-passage 1-1 into by force (forcing) pump; Material solution with vaporific from end cap conical boss 1-5 and the conical bore 4-4 of first rotating ring between the annular space nozzle that forms be injected to fast that to mix between stationary ring 2 and end cap 1, first rotating ring 4 formed batch mixing in first indoor, the supercritical carbon dioxide that enters with mixed stationary ring feeding-passage 2-1 in first mixes; Mixing the annular space nozzle that forms between the conical bore 4-4 of the conical boss 2-7 that continues to mix in first stationary ring in the back and second rotating ring, to spray in first, second between the mixed stationary ring 2 and second rotating ring 4 formed batch mixing fast indoor, further mix with the supercritical carbon dioxide that enters from the second interior mixed stationary ring feeding-passage 2-1, the mixing back continues to spray into crystallizer fast from annular space nozzle between the conical bore 4-4 of the conical boss 2-7 of the second interior mixed stationary ring and the 3rd rotating ring, supercritical carbon dioxide is taken away solvent, and material crystallization to be prepared forms nano and micro materials.If the two material nano and micro materials of preparation coat as particulate, then material 1 is dissolved in the solvent that dissolves each other with supercritical carbon dioxide, throw end cap feeding-passage 1-1 into by force (forcing) pump; Material 2 is dissolved in the solvent that dissolves each other with supercritical carbon dioxide, throw into by force (forcing) pump and mix stationary ring feeding-passage 2-1 in first; Material 1 solution with vaporific from end cap conical boss 1-5 and the conical bore 4-4 of first rotating ring between the annular space nozzle spray into fast that to mix between stationary ring 2 and end cap 1, first rotating ring 4 formed batch mixing in first indoor; Mix with material 2 solution that enter from the first interior mixed stationary ring feeding-passage 2-1, form tiny covering liquid pearl; Mixing between the conical bore 4-4 of the conical boss 2-7 that continues to mix in first stationary ring in the back and second rotating ring annular space nozzle, to spray in first, second between the mixed stationary ring 2 and second rotating ring 4 formed batch mixing fast indoor, further mix with the supercritical carbon dioxide that enters from the second interior mixed stationary ring feeding-passage 2-1, the mixing back continues to spray into crystallizer fast from the annular space nozzle that forms between the conical bore 4-4 of the conical boss 2-7 of the second interior mixed stationary ring and the 3rd rotating ring, supercritical carbon dioxide is taken away solvent, and material crystallization to be prepared forms nano and micro materials.If when need regulating nozzle clearance and preparing different nano and micro materials, then before beginning preparation, turn adjusting nut 5 is regulated the screw-in depth of rotating ring, thereby regulates the annular space size.
2, embodiment two: select the outer mix nozzle of four-way of basic building block assembling for use.
As shown in Figure 6, select an end cap 1, three outer stationary ring 3 and four rotating rings 4 of mixing for use, with 9 assemblings of a crystallizer.Installation process is:
Adjusting nut 5 is installed on the adjusting screw thread 4-5 of first rotating ring 4, opposite side with the adjusting screw thread 1-3 precession adjusting nut 5 on the end cap 1, the rotation direction of regulating screw thread 1-3 is opposite with the rotation direction of regulating screw thread 4-5, adjusting nut 5 revolves about being, the upside boss 4-2 of end cap 1 rim of the mouth 1-6 and rotating ring 4 is installed together simultaneously, and sealing ring 7 is installed in the seal groove 4-1; The downside boss 4-2 of rotating ring 4 and first outer upside rim of the mouth 3-2 that mixes stationary ring 3 are installed together, and sealing ring 7 is installed in the seal groove 4-1 of rotating ring 4, and spacer sleeve 6 is installed in the connecting pore 4-3;
First outer second adjusting nut 5 of adjusting screw thread 3-7 precession that mixes stationary ring 3, adjusting screw thread 4-5 precession adjusting nut 5 with second rotating ring 4, the rotation direction of regulating screw thread 3-7 is opposite with the rotation direction of regulating screw thread 4-5, adjusting nut 5 revolves about being, the downside rim of the mouth 3-2 of first outer mixed stationary ring 3 and the upside boss 4-2 of second rotating ring 4 are installed together simultaneously, sealing ring 7 is installed in the seal groove 4-1, spacer sleeve 6 is installed in the connecting pore 4-3;
According to above installation procedure second outer outer stationary ring 3, the 4th rotating ring 4 and crystallizer 9 of mixing of stationary ring 3, the 3rd rotating ring 4, the 3rd that mix fitted together;
Because nozzle basic building block installation dimension is unified, the end cap of this combination, rotating ring, to mix the connecting pore of connecting portion of stationary ring and the ring flange connecting pore of crystallizer outward all be the circular hole of four circumference uniform distributions, spacer sleeve 6 is installed in the connecting pore 4-3, and matching relationship is for being slidingly matched; At this moment four groups of spacer sleeve 6 endoporus are alignd respectively with end cap and stationary ring connecting pore, pierce into screw rod, the pad upper gasket, clamp nut, screw rod, packing ring and nut are formed connector 8, and sub-assembly is fixed together, and the outer mix nozzle of four-way has installed.
The outer mix nozzle built up nozzle of mounted four-way, by the conical boss 1-5 of end cap 1 and the rotating ring 4 conical bore 4-4 that match, and the downside conical boss 3-6 that mixes stationary ring 3 has outward constituted four nozzle clearances with the downside conical boss 3-6 of the outer mixed stationary ring 3 of the continuous rotating ring 4 conical bore 4-4 that adorn, continuous dress and the rotating ring 4 conical bore 4-4 of following continuous dress, because the height of spacer sleeve is greater than the thickness of rotating ring, its difference is the regulated quantity of nozzle clearance, rotate each adjusting nut 5 respectively, each rotating ring 4 can move up and down along spacer sleeve 6, can adjust each nozzle clearance respectively; Adjust back locking adjusting nut 5.
Four-way mixes the method supercritical fluid outward and prepares the nano and micro materials technical process: if the two material nano and micro materials of preparation, then dissolve in two kinds of materials in the solvent that dissolves each other with supercritical carbon dioxide on request respectively, after respectively two kinds of solution being pressurizeed by force (forcing) pump, press technological requirement with supercritical carbon dioxide, 1 feeding-passage 1-1 is covered in the supercritical carbon dioxide inlet side, material 1 solution advances the first outer stationary ring 3 feeding-passage 3-1 of mixing, supercritical carbon dioxide advances the second outer stationary ring 3 feeding-passage 3-1 of mixing, material 2 solution advance the 3rd outer stationary ring 3 feeding-passage 3-1 of mixing, supercritical carbon dioxide advances mixed all round stationary ring 3 feeding-passage 3-1, respectively from the conical boss 1-5 of end cap 1 and the conical bore 4-4 of first rotating ring, the first outer conical boss 3-6 of stationary ring and the conical bore 4-4 of second rotating ring of mixing, the second outer conical bore 4-4 that mixes stationary ring conical boss 3-6 and the 3rd rotating ring, four annular space nozzles spray fast between the conical boss 3-6 of the 3rd outer mixed stationary ring and the conical bore 4-4 of the 4th rotating ring, externally mixed, form the compound micron particles of receiving; If preparation 3 material nano and micro materials, then dissolve in three kinds of materials in the solvent that dissolves each other with supercritical carbon dioxide on request respectively, after respectively three kinds of solution being pressurizeed by force (forcing) pump, press technological requirement with supercritical carbon dioxide, 1 feeding-passage 1-1 is covered in material 1 solution inlet side, supercritical carbon dioxide advances the first outer stationary ring 3 feeding-passage 3-1 of mixing, material 2 solution advance the second outer stationary ring 3 feeding-passage 3-1 of mixing, supercritical carbon dioxide advances the 3rd outer stationary ring 3 feeding-passage 3-1 of mixing, material 3 solution advance mixed all round stationary ring 3 feeding-passage 3-1, respectively from the conical boss 1-5 of end cap 1 and the conical bore 4-4 of first rotating ring, the first outer conical boss 3-6 of stationary ring and the conical bore 4-4 of second rotating ring of mixing, the second outer conical boss 3-6 of stationary ring and the conical bore 4-4 of the 3rd rotating ring of mixing, four annular space nozzles spray fast between the conical boss 3-6 of the 3rd outer mixed stationary ring and the conical bore 4-4 of the 4th rotating ring, externally mixed, form the compound micron particles of receiving.
3, embodiment three: select the inside and outside mix nozzle of four-way of basic building block assembling for use.
As shown in Figure 7, select for use and mix outer stationary ring 3, four rotating rings 4 of mixing of stationary ring 2, two in the end cap 1, one, with 9 assemblings of a crystallizer.Installation process is:
The adjusting screw thread 4-5 of first rotating ring 4 installs adjusting nut 5, the adjusting screw thread 1-3 position of top precession end cap 1, the rotation direction of regulating screw thread 1-3 is opposite with adjusting screw thread 4-5, adjusting nut 5 revolves about being, the upside boss 4-2 of end cap 1 rim of the mouth 1-6 and first rotating ring 4 is installed together simultaneously, and sealing ring 7 is installed in the seal groove 4-1; The upside rim of the mouth 2-2 of the downside boss 4-2 of rotating ring 4 and interior mixed stationary ring 2 is installed together, and the center of orifices 2-3 of interior mixed stationary ring 2 upwards installs sealing ring 7 in the seal groove 4-1 of rotating ring 4, spacer sleeve 6 is installed in the connecting pore 4-3;
Mix second adjusting nut 5 of adjusting screw thread 2-8 precession of stationary ring 2 in being somebody's turn to do, adjusting screw thread 4-5 precession adjusting nut 5 with second rotating ring 4, the rotation direction of regulating screw thread 2-8 is opposite with adjusting screw thread 4-5, adjusting nut 5 revolves about being, the downside rim of the mouth 2-2 of mixed stationary ring 2 and the upside boss 4-3 of second rotating ring 4 are installed together simultaneously, sealing ring 7 is installed in the seal groove 4-1, second spacer sleeve 6 is installed in the connecting pore 4-3;
The downside boss 4-3 of second rotating ring 4 and first outer upside rim of the mouth 3-2 that mixes stationary ring 3 are installed together, and sealing ring 7 is installed in the seal groove 4-1 of rotating ring 4, and spacer sleeve 6 is installed in the connecting pore 4-3;
First outer the 3rd adjusting nut 5 of adjusting screw thread 3-7 precession that mixes stationary ring 3, adjusting screw thread 4-5 precession adjusting nut 5 with the 3rd rotating ring 4, the rotation direction of regulating screw thread 3-7 is opposite with adjusting screw thread 4-5, adjusting nut 5 revolves about being, the downside rim of the mouth 3-2 of first outer mixed stationary ring 3 and the upside boss 4-2 of the 3rd rotating ring 4 are installed together simultaneously, sealing ring 7 is installed in the seal groove 4-1, spacer sleeve 6 is installed in the connecting pore 4-3;
According to above installation procedure second outer stationary ring 3, the 4th rotating ring 4 and crystallizer 9 of mixing fitted together;
Because nozzle basic building block installation dimension is unified, the end cap of this combination, rotating ring, interior mixed stationary ring, to mix the connecting pore of connecting portion of stationary ring and the ring flange connecting pore of crystallizer outward all be the circular hole of four circumference uniform distributions, spacer sleeve 6 is installed in the connecting pore 4-3, and matching relationship is for being slidingly matched; At this moment four groups of spacer sleeve 6 endoporus are alignd respectively with end cap and stationary ring connecting pore, pierce into screw rod, the pad upper gasket, clamp nut, screw rod, packing ring and nut are formed connector 8, and sub-assembly is fixed together, and the inside and outside mix nozzle of four-way has just installed.
The inside and outside mix nozzle built up nozzle of mounted four-way, by the conical boss 1-5 of end cap 1 and first rotating ring 4, and in mix the interior mix nozzle that the conical bore 4-4 of the downside conical boss 2-7 of stationary ring 2 and second rotating ring 4 forms; And two outer outer mix nozzles that mix conical boss 3-8 and the conical bore 4-4 formation of other two rotating rings 4 below the stationary ring 3, constitute the inside and outside mix nozzle of four-way, because the height of spacer sleeve is greater than the thickness of rotating ring, its difference is the regulated quantity of nozzle clearance, the matching relationship of connecting pore 4-3 and spacer sleeve 6 is for being slidingly matched, so, rotate four adjusting nuts 5 respectively, four rotating rings 4 can move up and down along spacer sleeve 6, can adjust four nozzle clearances respectively; Adjust back locking adjusting nut 5.
The inside and outside method supercritical fluid that mixes of four-way prepares the nano and micro materials technical process: if the two material nano and micro materials of preparation, then dissolve in two kinds of materials in the solvent that dissolves each other with supercritical carbon dioxide on request respectively, after respectively two kinds of solution being pressurizeed by force (forcing) pump, press technological requirement with supercritical carbon dioxide, 1 feeding-passage 1-1 is covered in material 1 solution inlet side, material 1 solution with vaporific from end cap conical boss 1-5 and the conical bore 4-4 of first rotating ring between the annular space nozzle be injected to fast and mix stationary ring 2 and end cap 1 in first, formed batch mixing is indoor between first rotating ring 4, mixes with the supercritical carbon dioxide that enters from the first interior mixed stationary ring feeding-passage 2-1; The mixing back continues to spray fast from annular space nozzle between the conical bore 4-4 of the conical boss 2-7 of the first interior mixed stationary ring and second rotating ring, material 2 solution advance the first outer stationary ring 3 feeding-passage 3-1 of mixing, supercritical carbon dioxide advances the second outer stationary ring 3 feeding-passage 3-1 of mixing, outside first, mix the conical boss 3-6 of stationary ring and the conical bore 4-4 of the 3rd rotating ring respectively, two annular space nozzles spray fast between the conical boss 3-6 of the second outer mixed stationary ring and the conical bore 4-4 of the 4th rotating ring, externally mixed, form the compound micron particles of receiving; If preparation 3 material nano and micro materials, then dissolve in three kinds of materials in the solvent that dissolves each other with supercritical carbon dioxide on request respectively, after respectively three kinds of solution being pressurizeed by force (forcing) pump, press technological requirement with supercritical carbon dioxide, 1 feeding-passage 1-1 is covered in material 1 solution inlet side, material 2 solution advance to mix stationary ring 2 feeding-passage 2-1 in first, material 1 solution sprays into fast and mixes the back ejection in material 2 solution, material 3 solution advance the first outer stationary ring 3 feeding-passage 3-1 of mixing, supercritical carbon dioxide advances the second outer stationary ring 3 feeding-passage 3-1 of mixing, material 3 solution and supercritical carbon dioxide spray fast at annular space nozzle separately, and be externally mixed, forms the compound micron particles of receiving.
4, embodiment four: select rapid expanding nozzle of basic building block assembling for use.
As shown in Figure 8, select an end cap 1, rotating ring 4, crystallizer 9 assemblings for use.Installation process is:
The adjusting screw thread 4-5 of rotating ring 4 installs adjusting nut 5, the adjusting screw thread 1-3 of top precession end cap 1, the rotation direction of regulating screw thread 1-3 is opposite with adjusting screw thread 4-5, adjusting nut 5 revolves about being, the upside boss 4-3 of end cap 1 rim of the mouth 1-6 and rotating ring 4 is installed together simultaneously, and sealing ring 7 is installed in the seal groove 4-1; The downside boss 4-3 of rotating ring 4 and the rim of the mouth of crystallizer 9 are installed together, and sealing ring 7 is installed in the seal groove 4-1 of rotating ring 4, and spacer sleeve 6 is installed in the connecting pore 4-3;
Because nozzle basic building block installation dimension is unified, the ring flange connecting pore of the end cap of this combination, the connecting pore of rotating ring and crystallizer all is the circular hole of four circumference uniform distributions, and spacer sleeve 6 is installed in the connecting pore 4-3, and matching relationship is for being slidingly matched; At this moment spacer sleeve 6 endoporus are alignd respectively with end cap and stationary ring connecting pore, pierce into screw rod, the pad upper gasket, clamp nut, screw rod, packing ring and nut are formed connector 8, and sub-assembly is fixed together, and the rapid expanding nozzle has just installed.
Mounted rapid expanding built up nozzle forms the annular space nozzle by the conical boss 1-5 of end cap 1 and the conical bore 4-4 of rotating ring 4; The height of spacer sleeve is greater than the thickness of rotating ring, and its difference is the regulated quantity of nozzle clearance, and the matching relationship of connecting pore 4-3 and spacer sleeve 6 rotates adjusting nut 5 for being slidingly matched, and rotating ring 4 can move up and down along spacer sleeve 6, can adjust nozzle clearance; Adjust back locking adjusting nut 6.
Rapid expanding method supercritical fluid prepares the nano and micro materials technical process: desire is prepared material add the supercritical carbon dioxide dissolution kettle or claim extraction kettle, feed supercritical carbon dioxide, 1 feeding-passage 1-1 is covered in the supercritical carbon dioxide inlet side that is dissolved with material, with vaporific from end cap conical boss 1-5 and the conical bore 4-4 of rotating ring between the annular space nozzle be injected to fast in the crystallizer 9, because the quick reduction of pressure carbon dioxide, the solubility of material in carbon dioxide also sharply descends, finally separate out, form and to receive micron particles with small grains.
Claims (3)
1, composite nozzle for preparing supercritical fluid nanometer micrometer materail, it is characterized by, by end cap, rotating ring, interior mixed stationary ring, mix stationary ring outward, crystallizer claims gatherer, adjusting nut, spacer sleeve, sealing ring, connector basic building block to constitute again, according to supercritical fluid nano and micro materials preparation technology's requirement, select above basic building block assembling multichannel internal-mixing nozzle, multichannel outer mixed mode nozzle, the inside and outside mix nozzle of multichannel, rapid expanding nozzle for use:
The multichannel internal-mixing nozzle is made up of following basic building block; Mix stationary ring and at least 2 rotating rings, crystallizer at least in the end cap, 1, be connected and installed to be fixed together by connector and constitute; In the link position of end cap and rotating ring reaches, mix the link position of stationary ring and rotating ring, adjusting nut is installed;
The multichannel outer mixed mode nozzle is made up of following basic building block: end cap, at least 1 be outer to mix stationary ring and at least 2 rotating rings, crystallizer, is connected and installed to be fixed together by connector to constitute; Outside the link position of end cap and rotating ring reaches, mix the link position of stationary ring and rotating ring, adjusting nut is installed;
The inside and outside mix nozzle of multichannel is made up of following basic building block: mix stationary ring and at least 3 rotating rings and at least 1 outer mixed stationary ring, crystallizer at least in the end cap, 1, be connected and installed to be fixed together by connector and constitute; The link position of end cap and rotating ring and in mix stationary ring and rotating ring link position and outside the link position of mixed stationary ring and rotating ring, the installation adjusting nut;
The rapid expanding nozzle is made up of following basic building block: end cap, 1 rotating ring, crystallizer are connected and installed to be fixed together by connector and constitute; At the link position of end cap and rotating ring, adjusting nut is installed.
2, according to claims 1 described composite nozzle for preparing supercritical fluid nanometer micrometer materail, the mounting means that it is characterized by described end cap, rotating ring, interior mixed stationary ring, mixes between the installation position of stationary ring, crystallizer outward is use the rim of the mouth close fit, adds sealing ring at binding site and seals.
3, according to claims 1 described composite nozzle for preparing supercritical fluid nanometer micrometer materail, it is characterized by described end cap, rotating ring, interior mixed stationary ring, mix the ring flange of stationary ring, crystallizer outward, it all is disc-shape, its connecting portion all has the hole of unified installation connector, with the fit system that is slidingly matched spacer sleeve is installed in the hole of installation connector on the rotating ring, the height of spacer sleeve is greater than the thickness of rotating ring, and its difference is the regulated quantity of nozzle clearance; The nozzle that assembles is connected and fixed with connector.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610045286A CN100594070C (en) | 2006-07-05 | 2006-07-05 | Composite nozzle for preparing supercritical fluid nanometer micrometer materail |
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| CN200610045286A CN100594070C (en) | 2006-07-05 | 2006-07-05 | Composite nozzle for preparing supercritical fluid nanometer micrometer materail |
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| CN101099949A true CN101099949A (en) | 2008-01-09 |
| CN100594070C CN100594070C (en) | 2010-03-17 |
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| CN200610045286A Expired - Fee Related CN100594070C (en) | 2006-07-05 | 2006-07-05 | Composite nozzle for preparing supercritical fluid nanometer micrometer materail |
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| CN102019241A (en) * | 2010-10-22 | 2011-04-20 | 山东大学 | Combined nozzle for preparing supercritical fluid nano-micron materials |
| CN102133558A (en) * | 2010-12-10 | 2011-07-27 | 山东大学 | Accurate adjusting annular gap combined nozzle for preparing supercritical fluid nano/micron material |
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- 2006-07-05 CN CN200610045286A patent/CN100594070C/en not_active Expired - Fee Related
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| CN102019241A (en) * | 2010-10-22 | 2011-04-20 | 山东大学 | Combined nozzle for preparing supercritical fluid nano-micron materials |
| CN102019241B (en) * | 2010-10-22 | 2012-08-01 | 山东大学 | Combined nozzle for preparing supercritical fluid nano-micron materials |
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| CN108499486B (en) * | 2018-05-23 | 2023-10-17 | 山东大学 | Equipment for preparing superfine powder by supercritical fluid rapid expansion method |
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| CN109730929B (en) * | 2019-03-11 | 2024-05-28 | 塔尔普(北京)制药技术有限公司 | Combined spray nozzle for drug nano-granulation |
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