CN108238603A - Using rice biolobic material as the SiO of raw material2Nano-fluid preparation process - Google Patents

Using rice biolobic material as the SiO of raw material2Nano-fluid preparation process Download PDF

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Publication number
CN108238603A
CN108238603A CN201810220708.6A CN201810220708A CN108238603A CN 108238603 A CN108238603 A CN 108238603A CN 201810220708 A CN201810220708 A CN 201810220708A CN 108238603 A CN108238603 A CN 108238603A
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CN
China
Prior art keywords
rice
sio
nano
biolobic
biolobic material
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Pending
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CN201810220708.6A
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Chinese (zh)
Inventor
郭文文
李国能
郑友取
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Zhejiang Lover Health Science and Technology Development Co Ltd
Zhejiang University of Science and Technology ZUST
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Zhejiang Lover Health Science and Technology Development Co Ltd
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Priority to CN201810220708.6A priority Critical patent/CN108238603A/en
Publication of CN108238603A publication Critical patent/CN108238603A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/32Thermal properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention discloses a kind of using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, including step:Rice biolobic material is crushed to the first predetermined size;Broken rice biolobic material particle is carried out, except alkali, drying and heat treatment, to obtain the preliminary silica product for meeting default purity and the second predetermined size;Preliminary silica product is added in be stirred in deionized water or ethylene glycol until the volumetric concentration of silica reaches preset value;The solution stirred to get is subjected to ultrasonic disruption, obtains final silica nanometer fluid.Nano-fluid is made by raw material of renewable bioenergy in this method, at low cost and can substantially reduce pollution to environment for the preparation of existing chemical precipitation method.

Description

Using rice biolobic material as the SiO of raw material2Nano-fluid preparation process
Technical field
The present invention relates to nano-fluid medium manufacturing fields more particularly to a kind of SiO2 using rice biolobic material as raw material to receive Rice fluid preparation technique.
Background technology
Nano-fluid can be used as heat transferring medium, for heat transmission equipment augmentation of heat transfer, reduce the volume of heat transmission equipment, in energy The fields such as source, chemical industry, automobile, building, microelectronics, information have huge potential application foreground.
The SiO of the prior art2The raw material SiO of nano-fluid2It is generally prepared using chemical precipitation method, by sodium metasilicate and acidification Precipitation reaction occurs under certain conditions for agent, after be dried after separation to dioxy Si powder.Common acidulant is hydrochloric acid, sulphur Acid, sulphur nitre etc..Industrial manufacturing processes include productions, the transport of raw material, the synthesis of silica such as production, the sulfuric acid of waterglass, And prepared by nano-fluid.This preparation method needs to use a large amount of sodium metasilicate and acidulant, and cost of material is high, generates simultaneously A large amount of waste liquid, easily causes environmental pollution.
Therefore, it is necessary to a kind of low cost and the silica nanometer fluid preparation techniques of of low pollution.
Invention content
It is of the existing technology in order to solve the problems, such as, a kind of SiO using rice biolobic material as raw material is now provided2Nano-fluid Preparation process.
The technical solution that the present invention takes is as follows:
It is a kind of using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, including step:
Rice biolobic material is crushed to the first predetermined size;
Broken rice biolobic material particle is carried out, except alkali, drying and heat treatment, obtaining meeting default purity and second The preliminary silica product of predetermined size;
Preliminary silica product is added in be stirred in deionized water or ethylene glycol until the volume of silica Concentration reaches preset value;
The solution stirred to get is subjected to ultrasonic disruption, obtains final silica nanometer fluid.
First predetermined size refers to that rice biolobic material crushes rear average grain diameter.Second predetermined size refers to preliminary dioxy The average grain diameter of SiClx product.
Nano-fluid is made for raw material with renewable bioenergy (rice biolobic material) in this method, relative to existingization It learns for prepared by the precipitation method, it is at low cost and pollution to environment can be substantially reduced.
In a wherein embodiment of the invention, the rice biolobic material is rice husk or straw.
In a wherein embodiment of the invention, first predetermined size is 200~500 μm.
In a wherein embodiment of the invention, except alkali includes the following steps:
The rice biolobic material particle of first predetermined size is impregnated 12~24 hours in water;
Rice biolobic material particle after immersion is subjected to pickling with acid solution, is filtered after pickling.
" impregnating the rice biolobic material particle of the first presetting granularity in water 12~24 hours ", can remove rice husk in this way Middle major part alkali and alkaline earth metal ions;" the rice biolobic material particle after immersion is subjected to pickling with acid solution, is carried out after pickling Filtering " can remove alkali and alkaline earth metal ions completely after operating in this way.
In a wherein embodiment of the invention, acid concentration range is 4~10wt% used by pickling, acidleach temperature range It is 95~120 DEG C, leaching time ranging from 1~4 hour, and the ratio of rice biolobic material particle and acid is 1:6~1:12g:ml.
In a wherein embodiment of the invention, acid pickling is hydrochloric acid or nitric acid.
In a wherein embodiment of the invention, the heat treatment carried out to removing the product obtained after alkali, drying is to use atmosphere furnace Heated, wherein atmosphere furnace be heat-treated used in gas for air, single O2、N2With reference to O2Or CO2With reference to O2.When Atmosphere furnace be heat-treated used in gas be single O2, the temperature range of hot atmosphere is 650 DEG C, and the time being heat-treated is long Spend is 3 hours.Gas used in being heat-treated when atmosphere furnace is N2With reference to O2, hot atmosphere process is:
First in N2It is lower to carry out 400 DEG C of hot atmospheres 0.5 hour, after in O2Lower 600 DEG C of progress hot atmosphere 1.5 hours;Or
First in N2It is lower to carry out 500 DEG C of hot atmospheres 0.5 hour, after in O2Lower 600 DEG C of progress hot atmosphere 1 hour.
Gas used in being heat-treated when atmosphere furnace is CO2With reference to O2, hot atmosphere process is:First in CO2Lower progress 400 DEG C of hot atmospheres 0.5 hour, after in O2Lower 600 DEG C of progress hot atmosphere 1.5 hours.
In a wherein embodiment of the invention, the default purity is 89.0~99.9wt%, second predetermined size For 8~20nm.
In a wherein embodiment of the invention, the stirring is carried out using magnetic stirring apparatus, and mixing time is small for 1~4 When, silica volume concentration need to reach in obtained solution values are stirred in 0.5~1.0vol%.
The beneficial effects of the invention are as follows:Nanometer is made for raw material with renewable bioenergy (rice biolobic material) in this method Fluid, it is at low cost and pollution to environment can be substantially reduced for the preparation of existing chemical precipitation method.
Specific embodiment
With reference to embodiment, further explanation explanation is subject to the present invention.
It is a kind of using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, including step:
Rice biolobic material is crushed to by the first predetermined size by crusher;
Broken rice biolobic material particle is carried out, except alkali, drying and heat treatment, obtaining meeting default purity and second The preliminary silica product of predetermined size;
Preliminary silica product is added in base fluid (deionized water or ethylene glycol) and is stirred up to silica Volumetric concentration reaches preset value;
The solution stirred to get is subjected to ultrasonic disruption, obtains final silica nanometer fluid.
First predetermined size refers to that rice biolobic material crushes rear average grain diameter.Second predetermined size refers to preliminary dioxy The average grain diameter of SiClx product.
In this present embodiment, the rice biolobic material is rice husk or straw.
In this present embodiment, first predetermined size is 200~500 μm.
In this present embodiment, except alkali includes the following steps:
The rice biolobic material particle of first predetermined size is impregnated 12~24 hours in water;
Rice biolobic material particle after immersion is subjected to pickling with acid solution, is filtered after pickling.
" impregnating the rice biolobic material particle of the first presetting granularity in water 12~24 hours ", can remove rice husk in this way Middle major part alkali and alkaline earth metal ions;" the rice biolobic material particle after immersion is subjected to pickling with acid solution, is carried out after pickling Filtering " can remove alkali and alkaline earth metal ions completely after operating in this way.
In this present embodiment, acid concentration range is 4~10wt% used by pickling, and acidleach temperature range is 95~120 DEG C, leaching time ranging from 1~4 hour, and the ratio of rice biolobic material particle and acid is 1:6~1:12g:ml.
In this present embodiment, acid pickling is hydrochloric acid or nitric acid.
In this present embodiment, the heat treatment carried out to removing the product obtained after alkali, drying is to be heated with atmosphere furnace, Middle atmosphere furnace be heat-treated used in gas for air, single O2、N2With reference to O2Or CO2With reference to O2
In this present embodiment, the default purity is 89.0~99.9wt%, and second predetermined size is 8~20nm.
In this present embodiment, the stirring is carried out using magnetic stirring apparatus, and mixing time is 1~4 hour, stirring gained To solution in the values that need to reach of silica volume concentration in 0.5~1.0vol%.
In the lab, 1-10g rice husks are taken, SiO is prepared using the method for the present embodiment2Nano-fluid, specific data It is as shown in table 1 below, wherein, acid is nitric acid, and ultrasonic power is 100~500W used by ultrasonic disruption, and ultrasonic wave is broken The broken time is 1~6 hour, finally from SiO obtained2Volume 100ml is extracted in nano-fluid, is received using transient hot wire technique measurement Rice flow thermal conductivity coefficient.
Table 1
As seen from the above table, heat conduction can be made for raw material with renewable bioenergy (rice biolobic material) by this method The higher nano-fluid of coefficient, this method are at low cost and can substantially reduce for the preparation of existing chemical precipitation method Pollution to environment.
The foregoing is merely the preferred embodiment of the present invention, not thereby limit the scope of patent protection of the present invention, all It is the equivalent structure transformation made with present specification, is directly or indirectly used in other related technical areas, Similarly include within the scope of the present invention.

Claims (9)

  1. It is 1. a kind of using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that including step:
    Rice biolobic material is crushed to the first predetermined size;
    Broken rice biolobic material particle is carried out except alkali, drying and heat treatment, obtains meeting default purity and second default The preliminary silica product of grain size;
    Preliminary silica product is added in be stirred in deionized water or ethylene glycol until the volumetric concentration of silica Reach preset value;
    The solution stirred to get is subjected to ultrasonic disruption, obtains final silica nanometer fluid.
  2. 2. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that described Rice biolobic material is rice husk or straw.
  3. 3. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that described First predetermined size is 200~500 μm.
  4. 4. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that except alkali Include the following steps:
    The rice biolobic material particle of first predetermined size is impregnated 12~24 hours in water;
    Rice biolobic material particle after immersion is subjected to pickling with acid solution, is filtered after pickling.
  5. 5. as claimed in claim 4 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that pickling Used acid concentration range is 4~10wt%, and acidleach temperature range is 95~120 DEG C, leaching time ranging from 1~4 hour, And the ratio of rice biolobic material particle and acid is 1:6~1:12g:ml.
  6. 6. as claimed in claim 5 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that pickling Acid used is hydrochloric acid or nitric acid.
  7. 7. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that removing To be heated with atmosphere furnace, wherein atmosphere furnace, which is heat-treated, is used for the heat treatment that the product obtained after alkali, drying carries out Gas for air, single O2、N2With reference to O2Or CO2With reference to O2
  8. 8. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that described Default purity is 89.0~99.9wt%, and second predetermined size is 8~20nm.
  9. 9. as described in claim 1 using rice biolobic material as the SiO of raw material2Nano-fluid preparation process, which is characterized in that described Stirring is carried out using magnetic stirring apparatus, and mixing time is 1~4 hour, and it is dense to stir silica volume in obtained solution The values that need to reach are spent in 0.5~1.0vol%.
CN201810220708.6A 2018-03-16 2018-03-16 Using rice biolobic material as the SiO of raw material2Nano-fluid preparation process Pending CN108238603A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1449996A (en) * 2003-05-20 2003-10-22 吉林大学 Process for preparing high-purity nano silicon dioxide from rice husk
CN101920966A (en) * 2010-07-21 2010-12-22 化工部长沙设计研究院 Method for producing porous nano silica and active carbon by utilizing rice hull ash
CN103045180A (en) * 2012-12-26 2013-04-17 青岛科技大学 Low-conductivity nanofluid and preparation method thereof
CN103360801A (en) * 2013-07-22 2013-10-23 华南理工大学 Novel nano-fluid and its preparation method and application thereof
CN104671247A (en) * 2015-02-11 2015-06-03 武汉科技大学 Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof
CN104692387A (en) * 2015-02-11 2015-06-10 武汉科技大学 Method for preparing nanometer silicon carbide by using silicon-containing biomass as raw material at low temperature and prepared nanometer silicon carbide
CN106634861A (en) * 2016-10-12 2017-05-10 哈尔滨工业大学 Preparation method of low-concentration silicon dioxide nano fluid based on water/ethylene glycol
CN107365571A (en) * 2017-06-09 2017-11-21 内蒙古工业大学 The preparation technology and microchannel heat-transfer working medium of carbon pipe nano-fluid

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1449996A (en) * 2003-05-20 2003-10-22 吉林大学 Process for preparing high-purity nano silicon dioxide from rice husk
CN101920966A (en) * 2010-07-21 2010-12-22 化工部长沙设计研究院 Method for producing porous nano silica and active carbon by utilizing rice hull ash
CN103045180A (en) * 2012-12-26 2013-04-17 青岛科技大学 Low-conductivity nanofluid and preparation method thereof
CN103360801A (en) * 2013-07-22 2013-10-23 华南理工大学 Novel nano-fluid and its preparation method and application thereof
CN104671247A (en) * 2015-02-11 2015-06-03 武汉科技大学 Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof
CN104692387A (en) * 2015-02-11 2015-06-10 武汉科技大学 Method for preparing nanometer silicon carbide by using silicon-containing biomass as raw material at low temperature and prepared nanometer silicon carbide
CN106634861A (en) * 2016-10-12 2017-05-10 哈尔滨工业大学 Preparation method of low-concentration silicon dioxide nano fluid based on water/ethylene glycol
CN107365571A (en) * 2017-06-09 2017-11-21 内蒙古工业大学 The preparation technology and microchannel heat-transfer working medium of carbon pipe nano-fluid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周显青: "《稻谷加工工艺与设备》", 30 September 2011 *

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