CN107138738A - A kind of method and device of Fast back-projection algorithm silver nano-grain - Google Patents

A kind of method and device of Fast back-projection algorithm silver nano-grain Download PDF

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Publication number
CN107138738A
CN107138738A CN201710387563.4A CN201710387563A CN107138738A CN 107138738 A CN107138738 A CN 107138738A CN 201710387563 A CN201710387563 A CN 201710387563A CN 107138738 A CN107138738 A CN 107138738A
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China
Prior art keywords
reactor
cavitation
silver
belgaum
reaction solution
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CN201710387563.4A
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刘宏宇
程媛媛
张环
王捷
魏俊富
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention is intended to provide the present invention is intended to provide a kind of can aid in belgaum walnut leaf Aqueous extracts come the method for quick continuous preparing silver nano granules by reducing and regulation and control grain diameter in Hydrodynamic cavitation reactor using cavitation.Hydrodynamic cavitation reactor is fabricated, reaction unit as shown in Figure 1 is built, the temperature of reactor is regulated and controled by heater, keep it in 30~90 DEG C.Take the belgaum walnut leaf Aqueous extracts and silver-colored presoma (AgNO of certain volume3Solution) it is configured to reaction solution and is put into accumulator tank, reaction solution liquid is continually fed into cavitation reactor with certain flow rate (1~3L/min) by vavuum pump, reaction solution is collected in reactor outlet with pipeline to be back in reactive tank, circulate operation, gained reaction solution is nano silver colloidal sol in reactive tank after a period of time.Present invention process is simple, easy to operate, is swift in response, environment-friendly, and energy consumption is relatively low, and due to using continuous preparation technology, reaction is easily achieved scale amplification, carries out industrialized production.

Description

A kind of method and device of Fast back-projection algorithm silver nano-grain
Technical field
The present invention relates to a kind of method of green continuity Fast back-projection algorithm Nano silver grain, i.e., used in cavitation reactor The method that candlenut tree leaf extract quickly continuously prepares Nano Silver.
Background technology
Silver nano-grain as a kind of emerging function nano material (Chem.Mater., 19 (2007) 1231-1238), Had a wide range of applications in biomedical sector.Utilize the surface plasma optical characteristics of silver nano-grain, it is possible to achieve right The high-sensitivity detection of biomolecule.And the characteristics of there is correlation with medium refraction index by plasma resonance wavelength, Using the silver nano-grain of functionalization the protein of specific binding can be observed under dark field microscope.
The traditional preparation method of nanometer-level silver material (Toxicol in Vitro, 35 (2016) 43-54) mainly has physics Method, including vacuum vapour deposition, plasma sputtering etc. and chemical method, including chemical reduction method (Sensor. Actuat.B- Cheml., 137 (2009) 768-773), microemulsion method etc..Can although Physical can obtain high-purity, polymolecularity, granularity The silver nano-grain of control, but its equipment investment is fairly expensive, and the controllable silver nano-grain of high-purity granularity is being made in chemical method Simultaneously as the substantial amounts of pollution for introducing chemical reagent and being easily caused environment.Some green lifes relatively are also occurred in that at present Thing method prepares the method (Talanta, 146 (2016) 237-243) of silver nano-grain, but these existing researchs are only rested on Simple interval preparatory phase, due to the mass transfer and heat-transfer effect of liquid in reactor it is poor, it is necessary to reaction time all compare Long (several to dozens of hour), and with the increase of reactor volume, the homogeneity of temperature in the kettle and concentration is more difficult to Realize, this just brings difficulty for amplification production.
Hydrodynamic cavitation is microcosmic, instantaneous, random, multiphase complex process, substantial amounts of energy can be produced, in cavitation energy Using aspect, the research and application being concentrated mainly on to ultrasonic cavitation are upper, are such as induced using cavitation or acceleration chemical reaction, ultrasound Cleaning, sewage disposal, augmentation of heat transfer etc. (Ultrasonics Sonochemistry, 34 (2017) 51-59).
The present invention continuously prepares the plant biomass reduction that Hydrodynamic cavitation reactor is applied to silver nano-grain, not only may be used To solve the shortcoming of interval preparation process, and it is simple to operate, and the reaction time, short (1~5 minute) was environment-friendly, and energy consumption is relatively low.
The content of the invention
The present invention is intended to provide one kind can aid in belgaum walnut leaf Aqueous extracts come quick in Hydrodynamic cavitation reactor using cavitation The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter.It is in mainly using the silver nano-grain obtained by this method Spherical, average grain diameter is located at 1~30nm, and particle dispersion is good.
Utilization Hydrodynamic cavitation reactor auxiliary biomass reduction involved in the present invention prepares the main dress of silver nano-grain Put is to consist of the following components:(1) vavuum pump (2) Hydrodynamic cavitation reactor, (3) product collecting tank.(specific device is shown in attached Fig. 1)
Selection processing and manufacturing Hydrodynamic cavitation reactor, builds reaction unit as shown in Figure 1, reactor is placed in sweet first In oil bath heater, the temperature in reactor is regulated and controled by heater, raw material flow velocity is adjusted by vavuum pump, then set Technological parameter:Reaction temperature (30~90 DEG C), the flow rate (1~3L/min) of material liquid.Concrete operation step is as follows:
(1) 1g candlenut tree leaf dried powders are weighed, 100ml deionized water is added, is placed in shaking table (30 DEG C, 150rpm) and shakes 12h is swung, is filtered with double-layer filter paper, gained filtrate is the Aqueous extracts that concentration is 10g/L;
(2) 2mmol/L silver-colored presoma (AgNO is prepared3Solution)
(3) regulate and control the temperature of reactor by heater, keep it in 30~90 DEG C.Take the silver-colored forerunner of certain volume Body (AgNO3Solution) and belgaum walnut leaf Aqueous extracts be configured to reaction solution and be put into accumulator tank, by vavuum pump by reaction solution with certain Flow rate (1~3L/min) is continually fed into cavitation reactor, and collecting reaction solution with pipeline in reactor outlet is back to reaction In groove, circulate operation, gained reaction solution is nano silver colloidal sol in reactive tank after a period of time.Utilize F30 transmission electron microscopes (TEM) pattern and particle diameter of the silver nano-grain of gained are observed and utilizes particle diameter statistical software Sigmascan pro4 couple Resulting electron microscope carries out particle diameter statistics.
Present invention process is simple, easy to operate, is swift in response, environment-friendly, and energy consumption is relatively low, due to preparing work using continuous Skill, reaction is easily achieved scale amplification, carries out industrialized production.
Brief description of the drawings
The reaction unit flow chart that Fig. 1 uses for the present invention.
Fig. 2 schemes for the TEM of the real silver nano-grain prepared of the present invention.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1:
Belgaum walnut leaf after drying, which is crushed, is made candlenut tree dry powder, 10g/L Aqueous extracts is obtained by preceding method, by same volume Long-pending belgaum walnut leaf Aqueous extracts and the silver-colored presoma (AgNO of 2mmol/L3Solution) it is well mixed, with vavuum pump by mixed liquor with 1L/min Flow rate be continuously supplied to throat's internal diameter for 0.8mm, in supervisor's internal diameter 6mm Hydrodynamic cavitation reaction tube, set reaction temperature as Room temperature (30 DEG C).The silver nano-grain of gained be it is subsphaeroidal, it is uniform in size, grain diameter footpath is mainly distributed on 2.4 ± 4.2nm。
Embodiment 2:
The volume flow rate of reaction solution in embodiment 1 is set as 1.5L/min, keeps other reaction conditions constant, gained Nano particle be subsphaeroidal, particle diameter is mainly distributed on 3.7 ± 4.8nm.
Embodiment 3:
The volume flow rate of reaction solution in embodiment 1 is set as 2L/min, keeps other reaction conditions constant, gained Nano particle is subsphaeroidal, and particle diameter is mainly distributed on 4.7 ± 6.3nm.
Embodiment 4:
The volume flow rate of reaction solution in embodiment 1 is set as 2.5L/min, keeps other reaction conditions constant, gained Nano particle be subsphaeroidal, particle diameter is mainly distributed on 5.5 ± 6.9nm.
Embodiment 5:
The volume flow rate of reaction solution in embodiment 1 is set as 3L/min, keeps other reaction conditions constant, gained Nano particle is subsphaeroidal, and particle diameter is mainly distributed on 6.6 ± 8.2nm.
Embodiment 6:
The pH of reaction solution is adjusted to 8.4, by the belgaum walnut leaf Aqueous extracts of same volume and the silver-colored presoma (AgNO of 2mmol/L3 Solution) it is well mixed, mixed liquor using 1L/min flow rate are continuously supplied to throat's internal diameter as 0.8mm with vavuum pump, in supervisor In footpath 6mm Hydrodynamic cavitation reaction tube, reaction temperature is set as room temperature (30 DEG C).The silver nano-grain of gained be it is subsphaeroidal, Uniform in size, grain diameter footpath is mainly distributed on 1.2 ± 3.2nm.
Embodiment 7:
Reaction temperature in embodiment 6 is set as 90 DEG C, keeps other reaction conditions constant, the nano particle of gained It is subsphaeroidal, particle diameter is mainly distributed on 3.3 ± 4.6nm.
Embodiment 8:
The pH of reaction solution in embodiment 6 is adjusted to 9.4, keeps other reaction conditions constant, the nano particle of gained It is subsphaeroidal, particle diameter is mainly distributed on 2.1 ± 3.6nm.
Embodiment 9:
The pH of reaction solution in embodiment 6 is adjusted to 10.4, keeps other reaction conditions constant, the nano particle of gained It is subsphaeroidal, particle diameter is mainly distributed on 1.5 ± 2.8nm.
Embodiment 10:
The pH of reaction solution in embodiment 6 is adjusted to 11.4, keeps other reaction conditions constant, the nano particle of gained It is subsphaeroidal, particle diameter is mainly distributed on 1.0 ± 1.8nm.

Claims (6)

1. the cavitation that a kind of utilization Hydrodynamic cavitation reactor is produced can aid in the quick continuous reduction preparation of silver of belgaum walnut leaf Aqueous extracts to receive The method of rice grain and regulation and control grain diameter, it is characterised in that its step is:The cavitation reactor of certain size is processed, by adding Hot device regulates and controls the temperature of reactor, keeps it in 30~90 DEG C.Take the silver-colored presoma (AgNO of certain volume3Solution) and stone Li Ye Aqueous extracts are configured to reaction solution and are put into accumulator tank, are held reaction solution with certain flow rate (1~3L/min) by vavuum pump It is continuous to be passed into cavitation reactor, collect reaction solution with pipeline in reactor outlet and be back in reactive tank, circulate operation, one section Gained reaction solution is nano silver colloidal sol in reactive tank after time.
2. the cavitation that a kind of utilization Hydrodynamic cavitation reactor as claimed in claim 1 is produced can aid in belgaum walnut leaf Aqueous extracts quick The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter, it is characterised in that silver nano-grain is anti-in Hydrodynamic cavitation Answer what is continuously synthesized in device, the Hydrodynamic cavitation reactor is made up of polytetrafluoroethylene (PTFE) and stainless steel, and throat diameter is 0.5~1.2mm.
3. the cavitation that a kind of utilization Hydrodynamic cavitation reactor as claimed in claim 1 is produced can aid in belgaum walnut leaf Aqueous extracts quick The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter, it is characterised in that the pH value of the silver-colored presoma of regulation is 8.3 To 11.4.
4. the cavitation that a kind of utilization Hydrodynamic cavitation reactor as claimed in claim 1 is produced can aid in belgaum walnut leaf Aqueous extracts quick The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter, it is characterised in that the silver-colored presoma used is AgNO3 Solution, its concentration is 2mmol/L.
5. the cavitation that a kind of utilization Hydrodynamic cavitation reactor as claimed in claim 1 is produced can aid in belgaum walnut leaf Aqueous extracts quick The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter, it is characterised in that the conveying flow rate of material liquid is 1~3L/ min。
6. the cavitation that a kind of utilization Hydrodynamic cavitation reactor as claimed in claim 1 is produced can aid in belgaum walnut leaf Aqueous extracts quick The method of continuous preparing silver nano granules by reducing and regulation and control grain diameter, it is characterised in that reaction temperature is 30~90 DEG C.
CN201710387563.4A 2017-05-23 2017-05-23 A kind of method and device of Fast back-projection algorithm silver nano-grain Pending CN107138738A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108837777A (en) * 2018-07-10 2018-11-20 军事科学院系统工程研究院卫勤保障技术研究所 A kind of nanoparticulate dispersion and preparation method thereof
CN117469719A (en) * 2023-12-27 2024-01-30 沈阳菱太技研新工业技术有限公司 Axial flow cavitation pump for heating system
CN118204506A (en) * 2024-03-19 2024-06-18 无锡晶睿光电新材料有限公司 Method and device for preparing metal powder by using high-dispersion synthesis reactor

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CN101342600A (en) * 2008-08-15 2009-01-14 厦门大学 Continuous preparing apparatus for nano-silver and continuous preparing method for nano-silver and
CN102423807A (en) * 2011-12-01 2012-04-25 厦门大学 Method for continuously synthesizing platinum nanometer particle
RU2448810C1 (en) * 2011-04-05 2012-04-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет" (ГОУ ВПО БашГУ) Method of producing silver nanoparticles
CN102773496A (en) * 2012-08-22 2012-11-14 厦门大学 Method for preparing gold-silver alloy nano particle by continuous reaction kettle
CN103449527A (en) * 2013-08-09 2013-12-18 华南理工大学 Method for preparing ferrate through hydraulic power cavitation and activation
CN104043382A (en) * 2014-06-23 2014-09-17 清华大学 Hydrodynamic cavitation generating device
CN104136151A (en) * 2012-02-13 2014-11-05 同和电子科技有限公司 Spherical silver powder and method for producing same
CN205295102U (en) * 2015-12-11 2016-06-08 黑龙江省科学院高技术研究院 Water conservancy cavitation reactor

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Publication number Priority date Publication date Assignee Title
CN101342600A (en) * 2008-08-15 2009-01-14 厦门大学 Continuous preparing apparatus for nano-silver and continuous preparing method for nano-silver and
RU2448810C1 (en) * 2011-04-05 2012-04-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет" (ГОУ ВПО БашГУ) Method of producing silver nanoparticles
CN102423807A (en) * 2011-12-01 2012-04-25 厦门大学 Method for continuously synthesizing platinum nanometer particle
CN104136151A (en) * 2012-02-13 2014-11-05 同和电子科技有限公司 Spherical silver powder and method for producing same
CN102773496A (en) * 2012-08-22 2012-11-14 厦门大学 Method for preparing gold-silver alloy nano particle by continuous reaction kettle
CN103449527A (en) * 2013-08-09 2013-12-18 华南理工大学 Method for preparing ferrate through hydraulic power cavitation and activation
CN104043382A (en) * 2014-06-23 2014-09-17 清华大学 Hydrodynamic cavitation generating device
CN205295102U (en) * 2015-12-11 2016-06-08 黑龙江省科学院高技术研究院 Water conservancy cavitation reactor

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108837777A (en) * 2018-07-10 2018-11-20 军事科学院系统工程研究院卫勤保障技术研究所 A kind of nanoparticulate dispersion and preparation method thereof
CN117469719A (en) * 2023-12-27 2024-01-30 沈阳菱太技研新工业技术有限公司 Axial flow cavitation pump for heating system
CN117469719B (en) * 2023-12-27 2024-02-23 沈阳菱太技研新工业技术有限公司 Axial flow cavitation pump for heating system
CN118204506A (en) * 2024-03-19 2024-06-18 无锡晶睿光电新材料有限公司 Method and device for preparing metal powder by using high-dispersion synthesis reactor

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Application publication date: 20170908