CN101891205B - Method for preparing nano silica subjected to surface modification by urushiol - Google Patents
Method for preparing nano silica subjected to surface modification by urushiol Download PDFInfo
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- CN101891205B CN101891205B CN2010102130088A CN201010213008A CN101891205B CN 101891205 B CN101891205 B CN 101891205B CN 2010102130088 A CN2010102130088 A CN 2010102130088A CN 201010213008 A CN201010213008 A CN 201010213008A CN 101891205 B CN101891205 B CN 101891205B
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Abstract
The invention relates to a method for preparing nano silica subjected to surface modification by urushiol, which is characterized by comprising the following steps of: premixing silicate ester, absolute ethyl alcohol and distilled water into mixed solution and dropping inorganic acid or alkali solution to obtain silica sol; dropping the urushiol-containing solution of absolute ethyl alcohol into the silica sol for isothermal reaction to obtain urushiol surface-modified nano silica dispersion solution; and centrifugally separating the dispersion solution to obtain modified nano silica, washing for three times, centrifugally precipitating, and performing vacuum drying to obtain the urushiol surface-modified nano silica. The method for preparing the nano silica has the advantages of simple process, low production cost, and suitability for industrialized production, and is applied to the field of nano materials.
Description
Technical field
The present invention relates to a kind of preparation method of nano silicon dioxide of subjected to surface modification by urushiol, belong to technical field of nano material.
Background technology
Nanometer SiO
2It is a kind of pollution-free, nontoxic ceramic;, specific surface area little because of its particle diameter reaches surface hydroxyl greatly and has reactive behavior; And have HS, high rigidity, can absorb characteristics such as ultraviolet ray; Thereby at organic polymer material, be used widely like fields such as rubber, plastics, tamanori, coating with superior stability, reinforcement property, thickening property and thixotropy.In organic polymer material; Give full play to the performance of nano silicon; Must keep the homogeneity and the dispersed uniform property of nano silicon particle diameter, have two critical problems: the one, compatibility problem, the interfacial interaction of promptly inorganic and organic phase; The 2nd, scattering problem, i.e. nano silicon homogeneity and distributivity in polymeric matrix.Nanometer SiO
2Surface energy is big, be easy to reunite, and giving full play to of restriction nano effect is difficult to soak into and disperse in organic phase, with nanometer SiO
2Carrying out surface-treated is a kind of effective means, changes nanometer SiO
2The physico-chemical property on surface improves the consistency and the bonding force of itself and organic molecule.The method of nano-silica surface modification is mainly contained, utilize physical adsorption, the coating modification of Van der Waals force, interaction of hydrogen bond between two components, and utilize the chemical modification of surface-modifying agent and some group generation chemical reactions of particle surface.Chemical modification can make SiO through the covalent linkage effect between properties-correcting agent and the nano silicon
2The surface has the active organic group of particular chemical, thereby improves SiO
2The consistency of particle in organic solvent and polymeric matrix.But the present properties-correcting agent that adopts is main with silane coupling agent, and its price is high.So need a kind of effective, surface-modifying agent wide, that price is low of originating of exploitation.
Summary of the invention
The present invention is directed to the deficiency of prior art, proposed a kind of method for preparing nano silica that nano silicon is carried out finishing through laccol, implementation process comprises:
1 is pre-mixed into mixed solution with silicon ester, absolute ethyl alcohol, zero(ppm) water, is warming up to 60 ℃～80 ℃, under 400～800 rev/mins stir speed (S.S.) in the mixed solution dropping inorganic acid or alkaline solution; Continue to stir; Isothermal reaction 2～8 hours obtains silicon dioxide gel, wherein:
Above-mentioned ratio is the molar weight ratio.
The ethanol solution that 2, will contain laccol splashes in 40～80 ℃ of silicon dioxide gels, and stirs with 400～1400 rev/mins speed simultaneously, and isothermal reaction 0.5～3h obtains the nano silicon dispersion liquid of laccol finishing; The laccol weight ratio accounts for 5%～15% in the ethanol solution, and nano silicon dispersion liquid mesosilicic acid ester is 1: 0.01～0.1 with the molar weight ratio of laccol.
3, dispersion liquid spinning under 6000～12000 rev/mins rotating speed gets modified manometer silicon dioxide; And get absolute ethanol washing in addition three times, supernatant is removed in centrifugation; Throw out obtains the nano silicon of laccol finishing through 60～80 ℃ of vacuum-drying 6～8h.
Described silicon ester is the tetraethyl orthosilicate of making a comment or criticism.
Described mineral acid is meant nitric acid, hydrochloric acid, sulfuric acid or phosphoric acid.
Described alkaline solution is meant strong aqua, sodium hydroxide solution or potassium hydroxide solution.
The present invention has the following advantages:
1. compare with silane coupling agent commonly used, laccol is a natural reproducible resource, and is cheap.
2. can prepare the nano silicon of laccol finishing easily.
3. this modified manometer silicon dioxide particle, the laccol hydroxyl interacts through covalent linkage, contain a large amount of long carbochains at silica sphere, and exist polymerisable carbon-carbon double bond, can with most crosslinked polymers and blend.
Description of drawings
Fig. 1 is the infrared spectrogram of laccol surface finish nano silicon-dioxide.
Fig. 2 be laccol surface finish nano silicon-dioxide the thermogravimetric spectrogram.
Embodiment
The positive tetraethyl orthosilicate, 1.32 gram zero(ppm) water and the 10.00 gram absolute ethyl alcohols that in a there-necked flask, add 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 37% aqueous hydrochloric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s.
Mixed solution is cooled to 40 ℃, under 600 rev/mins stir speed (S.S.), splashes into ethanol solution 31.40 grams of 5% laccol, drip and finish, isothermal reaction 3h, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 2
The positive tetraethyl orthosilicate, 1.32 gram zero(ppm) water and the 9.50 gram absolute ethyl alcohols that in a there-necked flask, add 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 37% aqueous hydrochloric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s.
Mixed solution is cooled to 40 ℃, under 600 rev/mins stir speed (S.S.), splashes into ethanol solution 15.70 grams of 10% laccol, drip and finish, isothermal reaction 3h, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 6000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 3
The positive tetraethyl orthosilicate, 1.32 gram zero(ppm) water and the 11.50 gram absolute ethyl alcohols that in a there-necked flask, add 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 37% aqueous hydrochloric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s.
Mixed solution is warming up to 80 ℃, under 1400 rev/mins stir speed (S.S.), splashes into ethanol solution 10.47 grams of 15% laccol, drip and finish, isothermal reaction 30min, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 12000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 5h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 4
The positive tetraethyl orthosilicate, 1.33 gram zero(ppm) water and the 10.00 gram absolute ethyl alcohols that in a there-necked flask, add 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 63% aqueous nitric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s;
Mixed solution is cooled to 40 ℃, under 600 rev/mins stir speed (S.S.), splashes into ethanol solution 3.14 grams of 5% laccol, drip and finish, isothermal reaction 3h, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 5
The positive tetraethyl orthosilicate, 1.33 gram zero(ppm) water and the 10.00 gram absolute ethyl alcohols that in a there-necked flask, add 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 63% aqueous nitric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s;
Mixed solution is cooled to 40 ℃, under 600 rev/mins stir speed (S.S.), splashes into ethanol solution 1.57 grams of 10% laccol, drip and finish, isothermal reaction 3h, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 6
The positive tetraethyl orthosilicate, 1.33 gram zero(ppm) water and the 10.00 gram absolute ethyl alcohols that in a there-necked flask, add calculated amount 10.41 grams; Be pre-mixed into mixed solution; Be warming up to 60 ℃, restrain 63% aqueous nitric acid, isothermal reaction 8h toward wherein dripping 0.05 400 rev/mins stir speed (S.S.)s;
Mixed solution is warming up to 80 ℃, under 1400 rev/mins stir speed (S.S.), splashes into ethanol solution 1.05 grams of 15% laccol, drip and finish, isothermal reaction 30min, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 7
In a there-necked flask, add positive tetraethyl orthosilicate, 0.89 gram zero(ppm) water and the 11.00 gram absolute ethyl alcohols of 10.41 grams, be pre-mixed into mixed solution, be warming up to 80 ℃, at the past strong aqua that wherein drips 1.42 grams 36% of 800 rev/mins stir speed (S.S.)s, isothermal reaction 2h;
Mixed solution is cooled to 40 ℃, under 600 rev/mins stir speed (S.S.), splashes into ethanol solution 3.14 grams of 5% laccol, drip and finish, isothermal reaction 3h, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 8h of 60 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 8
In a there-necked flask, add positive tetraethyl orthosilicate, 0.89 gram zero(ppm) water and the 10.00 gram absolute ethyl alcohols of 10.41 grams, be pre-mixed into mixed solution, be warming up to 80 ℃, at the past strong aqua that wherein drips 1.42 grams 36% of 800 rev/mins stir speed (S.S.)s, isothermal reaction 8h;
Mixed solution is warming up to 70 ℃, under 1400 rev/mins stir speed (S.S.), splashes into ethanol solution 10.47 gram (or represent with milliliter) of 15% laccol, drip and finish, isothermal reaction 30min, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 9
In a there-necked flask, add the positive tetraethyl orthosilicate and the 10.00 gram absolute ethyl alcohols of 10.41 grams, be pre-mixed into mixed solution, be warming up to 80 ℃, restrain 40% aqueous sodium hydroxide solution, isothermal reaction 8h toward wherein dripping 3.00 800 rev/mins stir speed (S.S.)s;
Mixed solution is cooled to 50 ℃, under 1400 rev/mins stir speed (S.S.), splashes into ethanol solution 31.40 grams of 5% laccol, drip and finish, isothermal reaction 30min, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Embodiment 10
In a there-necked flask, add the positive tetraethyl orthosilicate and the 10.00 gram absolute ethyl alcohols of 10.41 grams, be pre-mixed into mixed solution, be warming up to 80 ℃, restrain 40% aqueous sodium hydroxide solution, isothermal reaction 8h toward wherein dripping 3.00 800 rev/mins stir speed (S.S.)s;
Mixed solution is cooled to 50 ℃, under 1400 rev/mins stir speed (S.S.), splashes into ethanol solution 1.05 grams of 15% laccol, drip and finish, isothermal reaction 30min, the nano silicon dispersion liquid of acquisition laccol finishing.
The spinning under 8000 rev/mins rotating speed of gained dispersion liquid, throw out place the dry 6h of 80 ℃ of vacuum drying ovens behind absolute ethanol washing three times, promptly get laccol surface finish nano silicon-dioxide.
Claims (4)
1. a method for preparing nano silica that utilizes laccol to carry out finishing is characterized in that
1) silicon ester, absolute ethyl alcohol, zero(ppm) water are pre-mixed into mixed solution, are warming up to 60 ℃～80 ℃, under 400～800 rev/mins stir speed (S.S.) in the mixed solution dropping inorganic acid or alkaline solution; Continue to stir; Isothermal reaction 2～8 hours obtains silicon dioxide gel, wherein:
Above-mentioned ratio is the molar weight ratio;
The ethanol solution that 2) will contain laccol splashes in 40～80 ℃ of silicon dioxide gels, and stirs with 400～1400 rev/mins speed simultaneously, and isothermal reaction 0.5～3h obtains the nano silicon dispersion liquid of laccol finishing; The laccol weight ratio accounts for 5%～15% in the ethanol solution, and nano silicon dispersion liquid mesosilicic acid ester is 1: 0.01～0.1 with the molar weight ratio of laccol;
3) dispersion liquid spinning under 6000～12000 rev/mins rotating speed gets modified manometer silicon dioxide; And get absolute ethanol washing in addition three times, supernatant is removed in centrifugation; Throw out obtains the nano silicon of laccol finishing through 60～80 ℃ of vacuum-drying 6～8h.
2. the method for preparing nano silica that utilizes laccol to carry out finishing according to claim 1 is characterized in that described silicon ester is the tetraethyl orthosilicate of making a comment or criticism.
3. the method for preparing nano silica that utilizes laccol to carry out finishing according to claim 1 is characterized in that described mineral acid is meant nitric acid, hydrochloric acid, sulfuric acid or phosphoric acid.
4. the method for preparing nano silica that utilizes laccol to carry out finishing according to claim 1 is characterized in that described alkaline solution is meant strong aqua, sodium hydroxide solution or potassium hydroxide solution.
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| CN108721682B (en) * | 2018-06-20 | 2021-04-27 | 福建师范大学 | Synthesis method and application of urushiol modified mesoporous silica microspheres containing catechol groups |
| CN111218210A (en) * | 2020-01-08 | 2020-06-02 | 闽江学院 | Composite coating, preparation method and application thereof |
| CN113069937B (en) * | 2021-05-06 | 2023-03-31 | 长兴光宏新材料科技有限公司 | Oil-water separation membrane for wastewater treatment and preparation method thereof |
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