CN2503978Y - Super crisis CO2 solvent resistant appts. for making nano material - Google Patents
Super crisis CO2 solvent resistant appts. for making nano material Download PDFInfo
- Publication number
- CN2503978Y CN2503978Y CN 01201289 CN01201289U CN2503978Y CN 2503978 Y CN2503978 Y CN 2503978Y CN 01201289 CN01201289 CN 01201289 CN 01201289 U CN01201289 U CN 01201289U CN 2503978 Y CN2503978 Y CN 2503978Y
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- Prior art keywords
- nozzle
- supercritical
- solvent
- utility
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- 239000002904 solvent Substances 0.000 title claims description 19
- 239000002086 nanomaterial Substances 0.000 title abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000005755 formation reaction Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 239000012296 anti-solvent Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000013557 residual solvent Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract 3
- 238000000889 atomisation Methods 0.000 abstract 2
- 239000003595 mist Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000001046 rapid expansion of supercritical solution Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010253 intravenous injection Methods 0.000 description 1
- 238000001725 laser pyrolysis Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
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Abstract
The utility model relates to a supercritical CO <2> anti-solvent device for manufacturing the nanomaterial, and the utility model comprises a multi-nozzle spraying nozzle, an atomization crystallization cauldron, a collector, a separation cauldron, a feeding system and a CO <2> circulating system. When the feed liquid and the supercritical CO <2> are mixed for an instant and perform a mist spraying through a spraying nozzle, the oversaturated product is deposited in the atomization crystallization cauldron, and the nanomaterial is obtained through the continuous collection of the collector. A plurality of nanometer particles is manufactured with the device. The device has the advantages that the structure is compact, the operation is safe and stable, the device can be continuously produced and the products can flow freely; and the utility model has no residual solvent. The CO <2> is friendly to the human body and the environment, and the utility model has no three wastes, thereby belonging to a high technology facility of the sustainable development.
Description
The utility model relates to a kind of device of making the nanometer new material, particularly a kind of supercritical CO of making nano material
2Solvent-resistant device.
The method of making nano material has multiple: a class is mechanical milling method, laser pyrolysis processes and ultrasonic method, and these class methods are unsuitable for heat-sensitive materials because of producing heat; Two classes are chemical vapour deposition technique, alkoxide hydrolysis and vapour phase oxidation process, and this class methods size distribution is wide, dissolvent residual is difficult to eliminate; Three classes are supercritical fluid manufactured nano materials, as supercritical solvent rapid expanding method (RESS), and gas anti-solvent method (GAS) and supercritical CO
2Anti-solvent method (Supercritical Anti Solvent, SAS).The advantage of these methods is that product cut size is little, narrow particle size distribution, and temperature is low, is suitable for biochemical substances.1, in the RESS method, require solute to be dissolved in supercritical CO
2In the fluid, generate particulate through the nozzle rapid expanding again, because of many polar substances at supercritical CO
2Middle solubility is little, so energy consumption is big, productive rate is low, has limited range of application.2, in the GAS method, must make homogeneous phase solution earlier, selected solvent must not only dissolve solute but also with CO
2Dissolve each other, this method mostly is intermittently operated greatly, and product and difficult solvent recovery are unsuitable for producing in batches.3, in the SAS method, be with supercritical CO
2Be anti-solvent, selected solvent is solubilized solute but also dissolve in anti-solvent not only, and this characteristics of promptly utilizing solute to be insoluble to anti-solvent and anti-solvent and solvent dissolve each other are worked as supercritical CO
2Mix with solution moment, the solvent volume rapid expanding makes solution moment produce high degree of supersaturation and separate out solute, controls solute concentration in flow velocity, nozzle diameter size and the solution of anti-solvent, controls particle diameter, shape and the size distribution of particulate.The particle diameter of SAS manufactured can be made into sustained-release microparticle to 10nm for a short time, satisfies the needs of aerosol, intravenous injection and change gene DNA, and is easy to realize serialization, the industrialization of particulate production.Satisfy the needs of " no medicine is particulate not, and no medicine is slowly-releasing not ".
But the instrument and equipment that said method is used mostly is on a small scale instrument of development, oneself assembling, laboratory, is characterized in intermittently operated, CO
2Solvent does not reclaim, and output is little.Have only milligram to the gram level, Shang Weijian has relatively large continuous process units report.
The purpose of this utility model provides a kind of continuous supercritical CO
2Solvent-resistant device is used to make multiple nano material.This SAS device is made of nozzle cluster, spray crystallization still, product gatherer etc., can produce continuously.Innovative point of the present utility model is, the one, and a plurality of concentric tube nozzle shower nozzles are applicable to the multiple product manufacturing, and output is increased.The 2nd, a plurality of product gatherers, changeable continuous collection also can dry up product, produces continuously.
Embodiment of the present utility model is as follows:
One, a kind of supercritical CO
2Solvent-resistant device, as shown in Figure 1, by CO
2Pump, solvent pump, a plurality of concentric tube nozzle shower nozzle, spray crystallization still, product gatherer, separator, CO
2Reclaiming circulation and Control System of Microcomputer constitutes.Its nozzle arrangements as shown in Figure 2, form by the concentric tube that internal diameter is different: stainless steel capillary (5), external diameter 0.5-0.95mm locates to weld a segment length 2-6mm at outer tube spout (7), internal diameter 0.1-0.2mm stainless steel capillary, formation moment solution and anti-solvent district.Form by stainless steel cutting ferrule (4) seal combination.The SAS stream is supercritical CO
2Walk interior road through (2), solution is walked from outside by (1), also can be opposite, i.e. and supercritical CO
2Walk from outsidely, solution is walked interior road, and simultaneously and flow the high velocity stream delivery nozzle and atomize, the product deposition is separated out.The condition of work of SAS is: 25-60 ℃, make multiple nano material under the 7-30MPa condition.
Two, SAS operating characteristics:
1, starts crystallization kettle (12), gatherer (13), separating still (17) and printhead heater (11) and reach design temperature, start compressor by CO
2Source (23) is to CO
2Basin (22) topping up.Start CO
2Pump (1), heater via (2) heating, valve (3) regulation and control flow velocity is sprayed to crystallization kettle (12) through interior pipe (2), arrives gatherer (13) through valve (V1) again, and valve (16) is stable to setting pressure.
2, when system stability behind the temperature of setting, pressure, flow velocity, start solution pump (4) solution in the solution (5) is sucked, heater via (7) heating, reset valve (8) regulation and control flow velocity, introduce by outer pipeline Fig. 2 (1), at the preceding and supercritical CO of jet expansion Fig. 2 (7)
2Moment mixes, and by spout ejection atomizing, product is deposited in the crystallization kettle (12), flows into and collects CO in the gatherer (13)
2With solvent through counterbalance valve (16) step-down, in cyclone separator (17), stay solvent, gas CO2 passes through filter (18), buffer (19), compressor (20), condenser (21) again, with liquid CO
2Compress into CO
2Recycling in the basin (22).
3, after product is collected certain hour, close V1 and open V2, V5, switch to gatherer (14) and continue to collect product.Open V7 simultaneously, use CO
2Purging, dry products remove residual solvent.After purging certain hour, close V4, V7, open V10, make gatherer (13) connect atmosphere after, uncap and take out free flowable powder product.
4, after gatherer (14) is collected certain hour, switch to another gatherer (15).The rest may be inferred, produces continuously.
Advantage of the present utility model:
1, utilize the stainless steel capillary of special different inner diameters to be assembled into the bushing type atomizer, compact conformation, easily processing and fabricating can satisfy the needs of producing different product by changing the different inner diameters nozzle.
2, by the counterbalance valve controlled pressure, reset valve control flow, microcomputer control heating and valve, the temperature of system, pressure, stability of flow, favorable reproducibility.
3, because nozzle is adjustable, and optional solvent is more, this device purposes is wider, can flow freely particulate, the product no solvent residue as bioengineering, medicine, inorganic salts etc.
4, used anti-solvent C O
2To human body, environmental friendliness, cheap, three-waste free discharge, the new and high technology device of genus sustainable development.
Claims (3)
1, a kind of supercritical CO
2Solvent-resistant device is characterized in that: this device is mainly by nozzle cluster, atomizing crystallization autoclave, gatherer and separating still, charging, CO
2Formations such as circulation, microcomputer control.
2, supercritical CO according to claim 1
2Solvent-resistant device is characterized in that: nozzle is made up of the different concentric tube of internal diameter, stainless steel capillary 5, external diameter 0.5～0.95mm, internal diameter 0.05～0.3mm, outer tube 6 external diameters 2.0～3.0mm, internal diameter 0.55～0.95mm, concentric tube combines nozzle by 4 sealings of stainless steel cutting ferrule.
3, supercritical CO according to claim 1
2Solvent-resistant device is characterized in that: the nozzle shower nozzle is made up of three or more nozzle, and each nozzle inner and outer pipes is received the main entrance pipe through multiple-connector, and its stream is: supercritical CO
2Walk interior road through 2, solution is walked from outside by 1, also can be opposite, i.e. and supercritical CO
2Walk from outsidely, solution is walked interior road, simultaneously and stream, give mix the place and mix moment after, high velocity stream delivery nozzle and atomizing, product is separated out in the crystallization kettle deposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01201289 CN2503978Y (en) | 2001-02-12 | 2001-02-12 | Super crisis CO2 solvent resistant appts. for making nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01201289 CN2503978Y (en) | 2001-02-12 | 2001-02-12 | Super crisis CO2 solvent resistant appts. for making nano material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2503978Y true CN2503978Y (en) | 2002-08-07 |
Family
ID=33623377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01201289 Expired - Fee Related CN2503978Y (en) | 2001-02-12 | 2001-02-12 | Super crisis CO2 solvent resistant appts. for making nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2503978Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
| CN115253893A (en) * | 2022-07-25 | 2022-11-01 | 安徽科幂仪器有限公司 | Supercritical carbon dioxide preparation device and method for small amount of nano polar particles |
-
2001
- 2001-02-12 CN CN 01201289 patent/CN2503978Y/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108310797A (en) * | 2018-04-09 | 2018-07-24 | 南通市华安超临界萃取有限公司 | A kind of supercritical fluid recrystallization device |
| CN115253893A (en) * | 2022-07-25 | 2022-11-01 | 安徽科幂仪器有限公司 | Supercritical carbon dioxide preparation device and method for small amount of nano polar particles |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: 100083 DONGSHENG PARK DISTRICT, WUDAOKOU, HAIDIAN Free format text: FORMER NAME OR ADDRESS: 34, 10/F, NO. 61, ZHICHUN ROAD, HAIDIAN DISTRICT, BEIJING CITY, 100080 |
|
| CP03 | Change of name, title or address |
Patentee address after: 100083 6-3-203, Dongsheng garden area, Haidian District, Beijing, Wudaokou Patentee address before: 100080, Haidian District, Zhichun Road, No. 61, 10, 34, boxes |
|
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |