CN106947293A - A kind of method of surface treating nano silica - Google Patents

A kind of method of surface treating nano silica Download PDF

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Publication number
CN106947293A
CN106947293A CN201710340377.5A CN201710340377A CN106947293A CN 106947293 A CN106947293 A CN 106947293A CN 201710340377 A CN201710340377 A CN 201710340377A CN 106947293 A CN106947293 A CN 106947293A
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nano
nano silicon
surface treating
silicon dioxide
added
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不公告发明人
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Guangxi Assured Source Biotechnology Co Ltd
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Guangxi Assured Source Biotechnology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Cosmetics (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a kind of method of surface treating nano silica, it is that nano silicon is delivered to surface processing trough, then adds the dispersants of PEG 40 and ethanol, control temperature is at 60 80 DEG C, it is that 100 300r/min stir 20 30min in rotating speed, obtains nano silicon dioxide dispersion;Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, ricinoleate ester sodium sulphate and lauryl sodium sulfate composite modifier is added, temperature be 60 80 DEG C, frequency be ultrasonic 20 40min under 60 80Hz, obtain modified manometer silicon dioxide liquid;Modified manometer silicon dioxide liquid dry, pulverize through filtering again, sieve, that is, complete the modification of nano silicon.Nano silicon after this method surface treatment not only good dispersion, good stability, good with the compatibility of organic matter, moreover it is possible to improve the light resistance and weatherability of silica.

Description

A kind of method of surface treating nano silica
Technical field
The present invention relates to inorganic material-modified technical field, specifically a kind of method of surface treating nano silica.
Background technology
Nano silicon has extensive use in many fields, including filling, increment, thickens and strengthen various organic Material, such as plastics, resin, rubber, oil.There is undersaturated key and various hydroxyl bases in nano-silica surface Group, thus surface is in hydrophily, polarity is strong, easily absorbing water is interconnected to space network, and this space network Intermolecular active force is very strong, so that easily producing agglomeration between silicon dioxide granule, is not easy in organic solvent Disperse with rubber matrix, and because nano-silicon dioxide particle is small, specific surface area big, surface energy is high, it is unstable in energy State, it is easy to flock together and form aggregate, particularly easily reunite in organic polymer, poor compatibility, because This nano silicon needs to be modified it processing.
Many correlative studys have been done how to improve dispersive property of the nano material in organic polymer.Mainly Functional group is introduced on nano-silicon dioxide particle surface, so as to improve the dispersiveness of nano silicon, weatherability and automatically cleaning Property.The method of processing is modified to nano silicon following several:A kind of method is beaten by physical mechanical method The broken scattered nano particle reunited, such as by ultrasonically treated, but such a method effect is extremely limited, inorganic nanoparticles with Interaction between organic polymer is very limited compared with the interaction between inorganic nanoparticles.Another method is Graft Method is chemically bonded, nano grain surface is modified, the interaction between enhancing nano particle and polymer chain subtracts Reunion between few nano particle, promotes nano particle scattered in polymeric matrix, while having good photocatalytic Energy.But the technique of this kind of processing method is more complicated, control process is difficult, and cost is higher, it is difficult to realize industrialized production.
The content of the invention
The problem of present invention exists for the processing of current nano-silica surface there is provided a kind of technique it is simple, be easy to behaviour Nano silicon good dispersion and the good processing method of organic matter compatibility after work, low cost, processing.
In order to realize the above object the technical solution adopted by the present invention is as follows:
A kind of method of surface treating nano silica, comprises the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature exists 60-80 DEG C, it is that 100-300r/min stirs 20-30min in rotating speed, obtains nano silicon dioxide dispersion;
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, ricinoleate ester sodium sulphate and 12 are added Sodium alkyl sulfate composite modifier, temperature be 60-80 DEG C, frequency be ultrasound 20-40min under 60-80KHz, obtain modified Nano Titanium dioxide silicon liquid;
(3)Modified manometer silicon dioxide liquid dry, pulverize through filtering again, sieve, that is, complete the modification of nano silicon.
Further, the addition of the PEG-40 dispersants is the 1-2% of nano silicon weight.
Further, the mass concentration of the nano silicon dioxide dispersion is 15-20%.
Further, the castor oil acid fat sodium sulphate be methyl ricinolcic acid sodium sulphate, castor oil acid ethyl ester sodium sulphate, One kind in castor oil acid butyl ester sodium sulphate.
Further, the ricinoleate ester sodium sulphate and the mass ratio of lauryl sodium sulfate are 2-4:1.
Further, the addition of glycine betaine and the Sodium Polyacrylate composite modifier is nano silicon weight 1.5-3%。
Further, it in temperature is that the moisture content dried at 80-100 DEG C to nano silicon is 8- that the drying, which is, 12%。
Compared with prior art, beneficial effects of the present invention are:
1st, the not only good dispersion, good stability, good with the compatibility of organic matter of the nano silicon after this method surface treatment, The light resistance and weatherability of silica can also be improved.
2nd, the present invention breaks the nano particle of scattered reunion using physical agitation and ultrasonic method, and ultrasonic wave energy is produced Cavitation, makes liquid be in higher-order of oscillation state;It can be in nano-silicon dioxide particle using the effect of ultrasonic wave good Dispersity, mitigate the agglomeration between nano-silicon dioxide particle, while reactant can be accelerated in the mixed of micro-scale Close and react.
3rd, this method technique is simple, easily operated, low cost, production efficiency are high, easily realizes industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in more detail, but is not limited to protection scope of the present invention.
Embodiment 1
A kind of method of surface treating nano silica, comprises the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature is 60 DEG C, it is that 300r/min stirs 30min in rotating speed, obtains the nano silicon dioxide dispersion that mass concentration is 20%;The PEG-40 points The addition of powder is the 1.5% of nano silicon weight
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, methyl ricinolcic acid sodium sulphate and ten are added Sodium dialkyl sulfate composite modifier, temperature be 60 DEG C, frequency be ultrasound 40min under 60KHz, obtain modified manometer silicon dioxide Liquid;The methyl ricinolcic acid sodium sulphate and the mass ratio of lauryl sodium sulfate are 3:1, the addition of modifying agent is nanometer two The 2% of silica weight;
(3)Again by modified manometer silicon dioxide liquid through filtering, it is 12% to be dried at 80 DEG C to the moisture content of nano silicon, Crush, sieving completes the modification of nano silicon.
Embodiment 2
A kind of method of surface treating nano silica, comprises the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature is 70 DEG C, it is that 150r/min stirs 25min in rotating speed, obtains the nano silicon dioxide dispersion that mass concentration is 18%;The PEG-40 points The addition of powder is the 1.0% of nano silicon weight
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, castor oil acid ethyl ester sodium sulphate and ten are added Sodium dialkyl sulfate composite modifier, temperature be 70 DEG C, frequency be ultrasound 30min under 70KHz, obtain modified manometer silicon dioxide Liquid;The castor oil acid ethyl ester sodium sulphate and the mass ratio of lauryl sodium sulfate are 4:1, the addition of modifying agent is nanometer two The 2.5% of silica weight;
(3)Again by modified manometer silicon dioxide liquid through filtering, it is 10% to be dried at 100 DEG C to the moisture content of nano silicon, Crush, sieving completes the modification of nano silicon.
Embodiment 3
A kind of method of surface treating nano silica, comprises the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature is 80 DEG C, it is that 100r/min stirs 30min in rotating speed, obtains the nano silicon dioxide dispersion that mass concentration is 15%;The PEG-40 points The addition of powder is the 2.0% of nano silicon weight
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, castor oil acid butyl ester sodium sulphate and ten are added Sodium dialkyl sulfate composite modifier, temperature be 80 DEG C, frequency be ultrasound 20min under 80KHz, obtain modified manometer silicon dioxide Liquid;The castor oil acid butyl ester sodium sulphate and the mass ratio of lauryl sodium sulfate are 3:1, the addition of modifying agent is nanometer two The 3.0% of silica weight;
(3)Again by modified manometer silicon dioxide liquid through filtering, it is 10% to be dried at 100 DEG C to the moisture content of nano silicon, Crush, sieving completes the modification of nano silicon.
Embodiment 4
A kind of method of surface treating nano silica, comprises the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature is 60 DEG C, it is that 300r/min stirs 20min in rotating speed, obtains the nano silicon dioxide dispersion that mass concentration is 20%;The PEG-40 points The addition of powder is the 1.5% of nano silicon weight
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, castor oil acid ethyl ester sodium sulphate and ten are added Sodium dialkyl sulfate composite modifier, temperature be 60 DEG C, frequency be ultrasound 30min under 60KHz, obtain modified manometer silicon dioxide Liquid;The castor oil acid ethyl ester sodium sulphate and the mass ratio of lauryl sodium sulfate are 3:1, the addition of modifying agent is nanometer two The 3.0% of silica weight;
(3)Again by modified manometer silicon dioxide liquid through filtering, it is 8% to be dried at 100 DEG C to the moisture content of nano silicon, Crush, sieving completes the modification of nano silicon.

Claims (7)

1. a kind of method of surface treating nano silica, it is characterised in that:Comprise the following steps:
(1)Nano silicon is delivered to surface processing trough, PEG-40 dispersants and ethanol is then added, control temperature exists 60-80 DEG C, it is that 100-300r/min stirs 20-30min in rotating speed, obtains nano silicon dioxide dispersion;
(2)Above-mentioned nano silicon dioxide dispersion is added into supersonic generator, ricinoleate ester sodium sulphate and 12 are added Sodium alkyl sulfate composite modifier, temperature be 60-80 DEG C, frequency be ultrasound 20-40min under 60-80KHz, obtain modified Nano Titanium dioxide silicon liquid;
(3)Modified manometer silicon dioxide liquid dry, pulverize through filtering again, sieve, that is, complete the modification of nano silicon.
2. the method for surface treating nano silica according to claim 1, it is characterised in that:The PEG-40 dispersants Addition be nano silicon weight 1-2%.
3. the method for surface treating nano silica according to claim 1, it is characterised in that:The nano silicon The mass concentration of dispersion liquid is 15-20%.
4. the method for surface treating nano silica according to claim 1, it is characterised in that:The castor oil acid fat sulphur Sour sodium is one kind in methyl ricinolcic acid sodium sulphate, castor oil acid ethyl ester sodium sulphate, castor oil acid butyl ester sodium sulphate.
5. the method for surface treating nano silica according to claim 4, it is characterised in that:The ricinoleate ester sulphur Sour sodium and the mass ratio of lauryl sodium sulfate are 2-4:1.
6. the method for surface treating nano silica according to claim 5, it is characterised in that:The glycine betaine and poly- third The addition of olefin(e) acid sodium composite modifier is the 1.5-3% of nano silicon weight.
7. the method for surface treating nano silica according to claim 1, it is characterised in that:The drying is in temperature It is 8-12% for the dry moisture content to nano silicon at 80-100 DEG C.
CN201710340377.5A 2017-05-15 2017-05-15 A kind of method of surface treating nano silica Pending CN106947293A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107455492A (en) * 2017-08-07 2017-12-12 西南林业大学 A kind of method that nano-silicon dioxide modified microcapsule wall material prepares microcapsules
CN110144196A (en) * 2019-06-24 2019-08-20 西南石油大学 A kind of dispersing method of water-base drilling fluid nano silica
CN111826149A (en) * 2020-07-20 2020-10-27 宁波锋成先进能源材料研究院 Modified nano silicon dioxide and preparation method and application thereof

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CN1394918A (en) * 2001-07-06 2003-02-05 韩巍 Nano Water dispersion medium composition, its preparation method and application
CN103194097A (en) * 2013-04-19 2013-07-10 中国民航大学 Method for ultrasonically carrying out surface modification on silicon dioxide
CN104031430A (en) * 2014-05-12 2014-09-10 谷屿 Modified nanometer titanium dioxide with improved dispersibility and preparation method thereof
CN104479266A (en) * 2014-12-26 2015-04-01 天津滨浦生产力促进有限公司 Surface modification method of inorganic nanoparticles as well as polytetrafluoroethylene/inorganic nanoparticle composite material

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US3647495A (en) * 1970-01-29 1972-03-07 Nl Industries Inc Titanium dioxide pigment having improved dispersibility in coating compositions
CN1394918A (en) * 2001-07-06 2003-02-05 韩巍 Nano Water dispersion medium composition, its preparation method and application
CN103194097A (en) * 2013-04-19 2013-07-10 中国民航大学 Method for ultrasonically carrying out surface modification on silicon dioxide
CN104031430A (en) * 2014-05-12 2014-09-10 谷屿 Modified nanometer titanium dioxide with improved dispersibility and preparation method thereof
CN104479266A (en) * 2014-12-26 2015-04-01 天津滨浦生产力促进有限公司 Surface modification method of inorganic nanoparticles as well as polytetrafluoroethylene/inorganic nanoparticle composite material

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107455492A (en) * 2017-08-07 2017-12-12 西南林业大学 A kind of method that nano-silicon dioxide modified microcapsule wall material prepares microcapsules
CN110144196A (en) * 2019-06-24 2019-08-20 西南石油大学 A kind of dispersing method of water-base drilling fluid nano silica
CN111826149A (en) * 2020-07-20 2020-10-27 宁波锋成先进能源材料研究院 Modified nano silicon dioxide and preparation method and application thereof
CN111826149B (en) * 2020-07-20 2023-04-14 宁波锋成先进能源材料研究院 Modified nano silicon dioxide and preparation method and application thereof

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