CN107176612A - A kind of preparation method of light silicon dioxide nanoparticle - Google Patents
A kind of preparation method of light silicon dioxide nanoparticle Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of light silicon dioxide nanoparticle, it is related to silicon material technology field, the present invention is using convenient source sodium metasilicate, sulfuric acid as raw material, and prepare light silicon dioxide nanoparticle under n-hexane, NPE, the assistance of trimethoxysilane, the use of wherein dispersing aid helps speed up reaction process, so that particle diameter distribution is made in 50 100nm, apparent density in 0.05g/cm3, specific surface area is in 1200m2/ more than g, average pore size 10 15nm light silicon dioxide nanoparticle, with applied to heat-insulated, catalysis and the field such as chromatographic isolation.
Description
Technical field：
The present invention relates to silicon material technology field, and in particular to a kind of preparation method of light silicon dioxide nanoparticle.
Background technology：
Nanometer light silica is also known as aerosil, is a kind of mutually to assemble composition with nanometer scale particle
Nanoporous network structure, and a kind of high dispersive solid-state material full of gaseous state decentralized medium in space.Because it has nanometer
The features such as loose structure, low-density, low-k, low thermal conductivity, high porosity, high-specific surface area, mechanics, acoustics,
The aspects such as calorifics, optics show peculiar property, in space flight, military affairs, oil, chemical industry, mineral products, communication, medical, building materials, electricity
The various fields such as son, metallurgy have extensive and huge application value.
Preparing spherical SiO 2 aeroge microparticle has a well-regulated shape, the powder aerogel material being made from it have compared with
High apparent density and preferable mobility, is conducive to its application in terms of heat-insulated, chromatographic isolation and catalysis.At present, ball
The shortcomings of technology of preparing of shape aerosil microparticle still has complex process, time-consuming, cost is high, continues to study
A kind of cost is low, technique is simple, the preparing spherical SiO 2 aeroge microparticle technology of preparing of large-scale production can be achieved with developing
Be of great practical significance.
The content of the invention：
The technical problems to be solved by the invention are to provide that a kind of preparation manipulation is simple, specific surface area is big, particle diameter and hole
Footpath is distributed in the preparation method of the light silicon dioxide nanoparticle of Nano grade.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of preparation method of light silicon dioxide nanoparticle, mainly comprises the following steps：
(1) deionized water and dispersing aid are added into reactor, stirring stands 10- after making dispersing aid dissolving completely
15min, is then slowly added dropwise 35wt% sodium silicate aqueous solutions with stirring, and rate of addition is controlled in 5-10mL/min, treats silicic acid
The mixed solution of 10wt% dilute sulfuric acids and n-hexane is added dropwise after sodium water solution completion of dropwise addition again, rate of addition is controlled in 1-5mL/
NPE is added after min, completion of dropwise addition, gained mixed liquor forms breast in stirring under 300-500rpm rotating speeds
Liquid；
(2) added into above-mentioned gained emulsion and 35-40 DEG C of insulation reaction is warming up under trimethoxysilane, stirring
3-5h, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
The deionized water, dispersing aid, 35wt% sodium silicate aqueous solutions, 10wt% dilution heat of sulfuric acid, n-hexane, nonyl
Phenol polyethenoxy ether, the mass ratio of trimethoxysilane are 0.5-1:0.01-0.05:1:1.5-2:3-5:0.1-0.3:
0.5-1。
The dispersing aid is made up of the raw material of following parts by weight：Poloxamer/5-10 parts of alanine, poly dimethyl two
1-2 parts of allyl ammonium chloride, 0.5-1 parts of PVP, 0.1-0.5 parts of rilanit special, 0.01-0.02 parts of ferrocene, it is prepared
Method is：Rilanit special and ferrocene are added into poloxamer/alanine, 120-125 DEG C of insulation grinding 15- is warming up to
30min, adds PDDA, continues in 120-125 DEG C of insulation grinding 10-15min, and be transferred to 0-5
Sealing and standing 1-2h in DEG C environment, then adds PVP, and 120-125 DEG C of insulation grinding 5-10min, i.e. score are warming up to again
Dissipate auxiliary agent.
The preparation method of the poloxamer/alanine is：To PLURONICS F87 and the mixed-powder of alanine under grinding
It is middle that deionized water is added dropwise until being completely dissolved, and in microwave reflow treatment 5- under microwave frequency 2450MHz, power output 700W
10min, stands and continues microwave reflow treatment 5-10min after 10-15min, add N hydroxymethyl acrylamide and caseinic acid
Sodium, microwave reflow treatment 5-10min again after being sufficiently mixed, gained mixture naturally cools to room temperature, and finally feeding freezing is dry
In dry machine, dry gained solid and micro mist is made through micronizer, produce poloxamer/alanine.
The PLURONICS F87, alanine, the mass ratio of N hydroxymethyl acrylamide and casein sodium are 10:1:
0.05:0.05。
The beneficial effects of the invention are as follows：The present invention is using convenient source sodium metasilicate, sulfuric acid as raw material, and in n-hexane, nonyl
Light silicon dioxide nanoparticle, wherein dispersing aid are prepared under phenol polyethenoxy ether, the assistance of trimethoxysilane
Use help speed up reaction process so that be made particle diameter distribution in 50-100nm, apparent density in 0.05g/cm3, compare table
Area is in 1200m2/ more than g, average pore size 10-15nm light silicon dioxide nanoparticle, with applied to it is heat-insulated, catalysis
With the field such as chromatographic isolation.
Embodiment：
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
(1) 0.5kg deionized waters and 0.03kg dispersing aiies are added into reactor, stirring makes dispersing aid dissolving complete
After stand 10min, be then slowly added dropwise 1kg 35wt% sodium silicate aqueous solutions with stirring, rate of addition is controlled in 5-10mL/
Min, after the mixed solution that 1.5kg 10wt% dilute sulfuric acids and 3kg n-hexanes is added dropwise after sodium silicate aqueous solution completion of dropwise addition again, drop
Acceleration Control adds 0.2kg NPEs after 1-5mL/min, completion of dropwise addition, and gained mixed liquor is in 300-
Stirring forms emulsion under 500rpm rotating speeds；
(2) 0.5kg trimethoxysilanes are added into above-mentioned gained emulsion, 35-40 DEG C of guarantor is warming up under stirring
Temperature reaction 3h, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
The preparation of dispersing aid：0.5g rilanit specials and 0.02g ferrocene are added into 10g poloxamers/alanine,
120-125 DEG C of insulation grinding 30min is warming up to, 2g PDDAs is added, continues in 120-125 DEG C of guarantor
Temperature grinding 15min, and sealing and standing 2h in 0-5 DEG C of environment is transferred to, 0.5g PVPs are then added, 120-125 is warming up to again
DEG C insulation grinding 10min, produce dispersing aid.
The preparation of poloxamer/alanine：Dripped under grinding into the mixed-powder of 10g PLURONICS F87s and 1g alanine
It is quiet plus deionized water is up to being completely dissolved, and in microwave reflow treatment 10min under microwave frequency 2450MHz, power output 700W
Continuation microwave reflow treatment 5min after 10min is put, 0.05g N hydroxymethyl acrylamides and 0.05g casein sodiums is added,
Microwave reflow treatment 10min again after being sufficiently mixed, gained mixture naturally cools to room temperature, finally sends into freeze drier
In, dry gained solid and micro mist is made through micronizer, produce poloxamer/alanine.
Embodiment 2
(1) 0.5kg deionized waters and 0.05kg dispersing aiies are added into reactor, stirring makes dispersing aid dissolving complete
After stand 10min, be then slowly added dropwise 1kg 35wt% sodium silicate aqueous solutions with stirring, rate of addition is controlled in 5-10mL/
Min, after the mixed solution that 2kg 10wt% dilute sulfuric acids and 5kg n-hexanes is added dropwise after sodium silicate aqueous solution completion of dropwise addition again, is added dropwise
Speed control adds 0.3kg NPEs after 1-5mL/min, completion of dropwise addition, and gained mixed liquor is in 300-
Stirring forms emulsion under 500rpm rotating speeds；
(2) 1kg trimethoxysilanes are added into above-mentioned gained emulsion, 35-40 DEG C of insulation is warming up under stirring
4h is reacted, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
The preparation of dispersing aid：0.2g rilanit specials and 0.01g ferrocene are added into 5g poloxamers/alanine,
120-125 DEG C of insulation grinding 30min is warming up to, 1g PDDAs is added, continues in 120-125 DEG C of guarantor
Temperature grinding 10min, and sealing and standing 2h in 0-5 DEG C of environment is transferred to, 0.5g PVPs are then added, 120-125 is warming up to again
DEG C insulation grinding 5min, produce dispersing aid.
The preparation of poloxamer/alanine：Dripped under grinding into the mixed-powder of 10g PLURONICS F87s and 1g alanine
It is quiet plus deionized water is up to being completely dissolved, and in microwave reflow treatment 10min under microwave frequency 2450MHz, power output 700W
Continuation microwave reflow treatment 5min after 10min is put, 0.05g N hydroxymethyl acrylamides and 0.05g casein sodiums is added,
Microwave reflow treatment 10min again after being sufficiently mixed, gained mixture naturally cools to room temperature, finally sends into freeze drier
In, dry gained solid and micro mist is made through micronizer, produce poloxamer/alanine.
Reference examples 1
(1) 0.5kg deionized waters and 0.05kg dispersing aiies are added into reactor, stirring makes dispersing aid dissolving complete
After stand 10min, be then slowly added dropwise 1kg 35wt% sodium silicate aqueous solutions with stirring, rate of addition is controlled in 5-10mL/
Min, after the mixed solution that 2kg 10wt% dilute sulfuric acids and 5kg n-hexanes is added dropwise after sodium silicate aqueous solution completion of dropwise addition again, is added dropwise
Speed control adds 0.3kg NPEs after 1-5mL/min, completion of dropwise addition, and gained mixed liquor is in 300-
Stirring forms emulsion under 500rpm rotating speeds；
(2) 1kg trimethoxysilanes are added into above-mentioned gained emulsion, 35-40 DEG C of insulation is warming up under stirring
4h is reacted, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
The preparation of dispersing aid：0.2g rilanit specials and 0.01g ferrocene are added into 5g poloxamers/alanine,
120-125 DEG C of insulation grinding 30min is warming up to, 1g PDDAs is added, continues in 120-125 DEG C of guarantor
Temperature grinding 10min, and sealing and standing 2h in 0-5 DEG C of environment is transferred to, 0.5g PVPs are then added, 120-125 is warming up to again
DEG C insulation grinding 5min, produce dispersing aid.
The preparation of poloxamer/alanine：Dripped under grinding into the mixed-powder of 10g PLURONICS F87s and 1g alanine
It is quiet plus deionized water is up to being completely dissolved, and in microwave reflow treatment 10min under microwave frequency 2450MHz, power output 700W
Continuation microwave reflow treatment 5min after 10min is put, gained mixture naturally cools to room temperature, finally sends into freeze drier,
Dry gained solid and micro mist is made through micronizer, produce poloxamer/alanine.
Reference examples 2
(1) 0.5kg deionized waters and 0.05kg dispersing aiies are added into reactor, stirring makes dispersing aid dissolving complete
After stand 10min, be then slowly added dropwise 1kg 35wt% sodium silicate aqueous solutions with stirring, rate of addition is controlled in 5-10mL/
Min, after the mixed solution that 2kg 10wt% dilute sulfuric acids and 5kg n-hexanes is added dropwise after sodium silicate aqueous solution completion of dropwise addition again, is added dropwise
Speed control adds 0.3kg NPEs after 1-5mL/min, completion of dropwise addition, and gained mixed liquor is in 300-
Stirring forms emulsion under 500rpm rotating speeds；
(2) 1kg trimethoxysilanes are added into above-mentioned gained emulsion, 35-40 DEG C of insulation is warming up under stirring
4h is reacted, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
The preparation of dispersing aid：0.2g rilanit specials are added into the 5g mixed-powders of PLURONICS F87 and alanine
With 0.01g ferrocene, 120-125 DEG C of insulation grinding 30min is warming up to, 1g PDDAs are added, after
Continue in 120-125 DEG C of insulation grinding 10min, and be transferred to sealing and standing 2h in 0-5 DEG C of environment, then add 0.5g PVPs, then
It is secondary to be warming up to 120-125 DEG C of insulation grinding 5min, produce dispersing aid.Wherein, PLURONICS F87 and alanine mass ratio 10:
1。
Reference examples 3
(1) 0.5kg deionized waters are added into reactor, 1kg 35wt% sodium metasilicate water is then slowly added dropwise with stirring
Solution, rate of addition control is in 5-10mL/min, after 2kg 10wt% dilute sulfuric acids are added dropwise after sodium silicate aqueous solution completion of dropwise addition again
With the mixed solution of 5kg n-hexanes, rate of addition control adds 0.3kg polyoxyethylene nonyl phenyls after 1-5mL/min, completion of dropwise addition
Vinethene, gained mixed liquor forms emulsion in stirring under 300-500rpm rotating speeds；
(2) 1kg trimethoxysilanes are added into above-mentioned gained emulsion, 35-40 DEG C of insulation is warming up under stirring
4h is reacted, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, i.e.,
Obtain light silicon dioxide nanoparticle.
Embodiment 3
Respectively to embodiment 1, embodiment 2, reference examples 1, reference examples 2, the made light silicon dioxide nanoparticle of reference examples 3
Character test is carried out, test result is as shown in table 1.
The character of the made light silicon dioxide nanoparticle of the invention of table 1
| Test event | Embodiment 1 | Embodiment 2 | Reference examples 1 | Reference examples 2 | Reference examples 3 |
| Particle diameter nm | 50-100 | 50-100 | 100-150 | 100-150 | 200-300 |
| Apparent density g/cm3 | 0.05 | 0.05 | 0.08 | 0.12 | 0.15 |
| Specific surface area m2/g | 1300 | 1250 | 1200 | 1000 | 800 |
| Average pore size nm | 10-15 | 10-15 | 15-20 | 25-35 | 40-50 |
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (5)
1. a kind of preparation method of light silicon dioxide nanoparticle, it is characterised in that：Mainly comprise the following steps：
(1) deionized water and dispersing aid are added into reactor, stirring stands 10-15min after making dispersing aid dissolving completely,
Then 35wt% sodium silicate aqueous solutions are slowly added dropwise with stirring, rate of addition is controlled in 5-10mL/min, treats that sodium metasilicate is water-soluble
The mixed solution of 10wt% dilute sulfuric acids and n-hexane is added dropwise after liquid completion of dropwise addition again, rate of addition control is added dropwise in 1-5mL/min
NPE is added after end, gained mixed liquor forms emulsion in stirring under 300-500rpm rotating speeds；
(2) added into above-mentioned gained emulsion and 35-40 DEG C of insulation reaction 3- is warming up under trimethoxysilane, stirring
5h, reaction is stood after terminating, and filtering obtains white depositions；
(3) white depositions are washed using n-hexane, until pH value reaches 7-8, most after being dried at 125-130 DEG C, produced light
Matter silicon dioxide nanosphere.
2. the preparation method of light silicon dioxide nanoparticle according to claim 1, it is characterised in that：The deionization
Water, dispersing aid, 35wt% sodium silicate aqueous solutions, 10wt% dilution heat of sulfuric acid, n-hexane, NPE, isobutyl
The mass ratio of base trimethoxy silane is 0.5-1:0.01-0.05:1:1.5-2:3-5:0.1-0.3:0.5-1.
3. the preparation method of light silicon dioxide nanoparticle according to claim 1, it is characterised in that：It is described to disperse to help
Agent is made up of the raw material of following parts by weight：Poloxamer/5-10 parts of alanine, 1-2 parts of PDDA,
0.5-1 parts of PVP, 0.1-0.5 parts of rilanit special, 0.01-0.02 parts of ferrocene, its preparation method is：To poloxamer/
Rilanit special and ferrocene are added in alanine, 120-125 DEG C of insulation grinding 15-30min is warming up to, adds poly dimethyl
Diallyl ammonium chloride, continues in 120-125 DEG C of insulation grinding 10-15min, and is transferred to sealing and standing 1-2h in 0-5 DEG C of environment,
Then PVP is added, 120-125 DEG C of insulation grinding 5-10min is warming up to again, dispersing aid is produced.
4. the preparation method of light silicon dioxide nanoparticle according to claim 3, it is characterised in that：The pool Lip river is husky
The preparation method of nurse/alanine is：Under grinding into the mixed-powder of PLURONICS F87 and alanine be added dropwise deionized water until
It is completely dissolved, and in microwave reflow treatment 5-10min under microwave frequency 2450MHz, power output 700W, stands after 10-15min
Continue microwave reflow treatment 5-10min, add N hydroxymethyl acrylamide and casein sodium, microwave again after being sufficiently mixed
Reflow treatment 5-10min, gained mixture naturally cools to room temperature, finally sends into freeze drier, dries gained solid warp
Micro mist is made in micronizer, produces poloxamer/alanine.
5. the preparation method of light silicon dioxide nanoparticle according to claim 4, it is characterised in that：The pool Lip river is husky
Nurse 188, alanine, the mass ratio of N hydroxymethyl acrylamide and casein sodium are 10:1:0.05:0.05.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115652649A (en) * | 2022-11-15 | 2023-01-31 | 福建佳来户外服装有限公司 | Preparation method of water pressure resistant down jacket fabric |
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