CN108586812A - A kind of preparation method and applications of sol dispersion - Google Patents
A kind of preparation method and applications of sol dispersion Download PDFInfo
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- CN108586812A CN108586812A CN201810408412.7A CN201810408412A CN108586812A CN 108586812 A CN108586812 A CN 108586812A CN 201810408412 A CN201810408412 A CN 201810408412A CN 108586812 A CN108586812 A CN 108586812A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0039—Post treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/02—Polyamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
Abstract
The invention belongs to Ludox technical fields, and in particular to a kind of preparation method and applications of sol dispersion.Preparation process is：1）Zinc ricinate is taken, is added in absolute ethyl alcohol, is stirred evenly, silane coupling agent kh560 is added, insulated and stirred obtains epoxy silane alcoholic solution；2）Ammonium polyphosphate is taken, is add to deionized water, propylgallate is added, stirs evenly, obtains aqueous dispersions；3）Ethyl orthosilicate is taken, is added in above-mentioned aqueous dispersions, stirs evenly, mixes, is stirred to react with epoxy silane alcoholic solution, ethyl alcohol is distilled off to get the sol dispersion.In the sol dispersion of the present invention, using silane coupling agent kh560 as epoxy silane, using ethyl orthosilicate as presoma, using ammonium polyphosphate aqueous solution as dispersion liquid, by by teos hydrolysis, obtained colloidal sol being modified using epoxy silane, obtains epoxy-modified colloidal sol, by the modification, the reactivity of sol surface can effectively improve.
Description
Technical field
The invention belongs to Ludox technical fields, and in particular to a kind of preparation method and applications of sol dispersion.
Background technology
Ludox is grain size in point of the nanometer silicon dioxide particle in water or other organic solvents of 1-100 nanometer ranges
Dispersion liquid, it is excellent to have that particle is uniform, nontoxic and pollution-free, large specific surface area, reactivity are high, adsorption capacity and adhesive property are strong etc.
Point is widely used in all conglomeraties such as building coating, hot investment casting, fireproof coating.Silicon dioxide granule is because with height in Ludox
Intensity, high rigidity can absorb the advantageous properties such as ultraviolet light, nontoxic, be increasingly becoming the hot spot of material science research field.But because of tool
There are the properties such as hydrophily, large specific surface area and surface energy height so that silicon dioxide granule and polymer compatibility and dispersibility are all
It is poor.
Invention content
It is an object of the present invention in view of the drawbacks of the prior art and insufficient, a kind of preparation of sol dispersion is provided
Method.
It is an object of the present invention to provide a kind of applications of sol dispersion
For realization said one purpose, the technical solution adopted by the present invention is：It is prepared by a kind of preparation method of sol dispersion
Step is：
1）Zinc ricinate is taken, is added in the absolute ethyl alcohol of 10-15 times of its weight, stirs evenly, silane coupling agent is added
Kh560, it is 50-55 DEG C to increase temperature, and insulated and stirred 1-2 hours obtains epoxy silane alcoholic solution；
2）Ammonium polyphosphate is taken, is added in the deionized water of 20-30 times of its weight, propylgallate is added, stirs evenly, obtains
Aqueous dispersions；
3）Ethyl orthosilicate is taken, is added in above-mentioned aqueous dispersions, stirs evenly, mixes, stirs with above-mentioned epoxy silane alcoholic solution
Reaction 3-4 hours is mixed, ethyl alcohol is distilled off to get the sol dispersion.
Preferably, the preparation of sol dispersion of the present invention, is counted in parts by weight, and each raw material is：Gallic acid third
0.3-1 parts of ester, 40-50 parts of ethyl orthosilicate, 0.1-0.3 parts of zinc ricinate, 1-2 parts of ammonium polyphosphate, silane coupling agent kh560
1-2 parts.
For another above-mentioned purpose of realization, the technical solution adopted by the present invention is：A kind of application of sol dispersion, is answered
In preparation for colloidal sol polyaniline film.
The preparation of colloidal sol polyaniline film of the present invention, specific preparation method are：1）By polyaniline solutions, colloidal sol point
Dispersion liquid mixes, and stirs evenly, and Sucrose acetoisobutyrate is added, and it is 100-110 DEG C to increase temperature, and insulated and stirred 1-2 hours is taken out
Filter, filter cake is washed, air drying, obtains sol-gel modified polyaniline；2）Sol-gel modified polyaniline is taken, its weight 10-18 is added to
In dimethylformamide again, stir evenly, spin-coating film is to get the colloidal sol polyaniline film.
Preferably, polyaniline solutions of the present invention are made by following steps：
1）The preparation of chloroformic solution
8-hydroxyquinoline, thiol-butyl tin mixing are taken, is added in the chloroform of 2-4 times of mixture weight, it is 10-20 minutes ultrasonic,
Obtain chloroformic solution；
2）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, obtain ammonium persulfate aqueous solution；
3）The preparation of polyaniline solutions
Sym-closene is taken, is mixed with aniline, is added in the deionized water of 10-15 times of mixture weight, stirs evenly, send
Enter into reaction kettle, be passed through nitrogen, it is 60-70 DEG C to adjust temperature of reaction kettle, and ammonium persulfate aqueous solution, insulated and stirred 3-4 is added
Hour, above-mentioned chloroformic solution is added, is stirred to react 1-2 hours, discharging cooling obtains polyaniline solutions.
Preferably, it counts in parts by weight, each raw material of the present invention is：140-160 parts of aniline, 60-70 parts of sol dispersion, second
1-2 parts of sour isobutyric acid sucrose ester, 0.1-0.4 parts of thiol-butyl tin, 1-2 parts of 8-hydroxyquinoline, 3-5 parts of sym-closene, mistake
4-5 parts of ammonium sulfate.
Advantages of the present invention：
In the sol dispersion of the present invention, using silane coupling agent kh560 as epoxy silane, using ethyl orthosilicate as presoma, with
Ammonium polyphosphate aqueous solution is dispersion liquid, by by teos hydrolysis, obtained colloidal sol being modified using epoxy silane, is obtained
Epoxy-modified colloidal sol can effectively improve the reactivity of sol surface by the modification.
The present invention handles aniline monomer using sym-closene, then polymerize under initiator effect, by acid doping,
Be effectively improved the conductive stability of polyaniline, the present invention by the polymer of acid doping and epoxy-modified colloidal sol blending reaction,
Realize that dispersion of the colloidal sol between polymer is compatible, to improve the mechanical strength and comprehensive performance of finished films.
Specific implementation mode
The present invention is further described through with reference to embodiment.
Embodiment 1
The preparation of sol dispersion of the embodiment of the present invention, preparation method include the following steps：
（1）0.3 part of zinc ricinate is taken, is added in the absolute ethyl alcohol of 15 times of its weight, stirs evenly, silane coupling agent is added
2 parts of kh560, it is 55 DEG C to increase temperature, and insulated and stirred 2 hours obtains epoxy silane alcoholic solution；
（2）2 parts of ammonium polyphosphate is taken, is added in the deionized water of 30 times of its weight, 1 part of propylgallate is added, stirring is equal
It is even, obtain aqueous dispersions；
（3）50 parts of ethyl orthosilicate is taken, is added in above-mentioned aqueous dispersions, stirs evenly, it is mixed with above-mentioned epoxy silane alcoholic solution
It closes, is stirred to react 4 hours, ethyl alcohol is distilled off to get the sol dispersion.
Embodiment 2
The preparation of sol dispersion of the embodiment of the present invention, preparation method include the following steps：
（1）0.1 part of zinc ricinate is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, silane coupling agent is added
1 part of kh560, it is 50 DEG C to increase temperature, and insulated and stirred 1 hour obtains epoxy silane alcoholic solution；
（2）1 part of ammonium polyphosphate is taken, is added in the deionized water of 20 times of its weight, 0.3 part of propylgallate, stirring is added
Uniformly, aqueous dispersions are obtained；
（3）40 parts of ethyl orthosilicate is taken, is added in above-mentioned aqueous dispersions, stirs evenly, it is mixed with above-mentioned epoxy silane alcoholic solution
It closes, is stirred to react 3 hours, ethyl alcohol is distilled off to get the sol dispersion.
Embodiment 3
The preparation of colloidal sol polyaniline film of the embodiment of the present invention, preparation method include the following steps：
（1）0.4 part of 2 parts of 8-hydroxyquinoline, thiol-butyl tin mixing are taken, is added in the chloroform of 4 times of mixture weight, ultrasound 20
Minute, obtain chloroformic solution；
（2）5 parts of ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, is stirred evenly, obtain ammonium persulfate aqueous solution；
（3）5 parts of sym-closene is taken, is mixed for 160 parts with aniline, is added in the deionized water of 15 times of mixture weight, stirs
It mixes uniformly, is sent in reaction kettle, be passed through nitrogen, it is 70 DEG C to adjust temperature of reaction kettle, and ammonium persulfate aqueous solution is added, and heat preservation is stirred
It mixes 4 hours, above-mentioned chloroformic solution is added, be stirred to react 2 hours, discharging cooling obtains polyaniline solutions；
（4）70 parts of mixing of sol dispersion made from above-mentioned polyaniline solutions, embodiment 1 are taken, stirs evenly, Sucrose Acetate is added
2 parts of sour sucrose ester, it is 110 DEG C to increase temperature, and insulated and stirred 2 hours filters, filter cake washed, air drying, obtained sol-gel modified
Polyaniline；
（5）Take above-mentioned sol-gel modified polyaniline, be added in the dimethylformamide of 18 times of its weight, stir evenly, spin coating at
Film is to get the colloidal sol polyaniline film.
Embodiment 4
The preparation of colloidal sol polyaniline film of the embodiment of the present invention, preparation method include the following steps：
（1）0.1 part of 1 part of 8-hydroxyquinoline, thiol-butyl tin mixing are taken, is added in the chloroform of 2-4 times of mixture weight, ultrasound
10 minutes, obtain chloroformic solution；
（2）4 parts of ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, is stirred evenly, obtain ammonium persulfate aqueous solution；
（3）3 parts of sym-closene is taken, is mixed for 140 parts with aniline, is added in the deionized water of 10 times of mixture weight, stirs
It mixes uniformly, is sent in reaction kettle, be passed through nitrogen, it is 60 DEG C to adjust temperature of reaction kettle, and ammonium persulfate aqueous solution is added, and heat preservation is stirred
It mixes 3 hours, above-mentioned chloroformic solution is added, be stirred to react 1 hour, discharging cooling obtains polyaniline solutions；
（4）60 parts of mixing of sol dispersion made from above-mentioned polyaniline solutions, embodiment 2 are taken, stirs evenly, Sucrose Acetate is added
1 part of sour sucrose ester, it is 100 DEG C to increase temperature, and insulated and stirred 1 hour filters, filter cake washed, air drying, obtained sol-gel modified
Polyaniline；
（5）Take above-mentioned sol-gel modified polyaniline, be added in the dimethylformamide of 10 times of its weight, stir evenly, spin coating at
Film is to get the colloidal sol polyaniline film.
Performance test：
The colloidal sol polyaniline film of embodiment 3：
Thickness 2.3mm；
Tensile strength 13.7Mpa；
Conductivity is tested using four probe method, result 0.93S/cm；
The colloidal sol polyaniline film of embodiment 4：
Thickness 2.5mm；
Tensile strength 14.0Mpa；
Conductivity is tested using four probe method, result 0.90S/cm.
Claims (6)
1. a kind of preparation method of sol dispersion, it is characterised in that：Preparation process is：
1）Zinc ricinate is taken, is added in the absolute ethyl alcohol of 10-15 times of its weight, stirs evenly, silane coupling agent is added
Kh560, it is 50-55 DEG C to increase temperature, and insulated and stirred 1-2 hours obtains epoxy silane alcoholic solution；
2）Ammonium polyphosphate is taken, is added in the deionized water of 20-30 times of its weight, propylgallate is added, stirs evenly, obtains
Aqueous dispersions；
3）Ethyl orthosilicate is taken, is added in above-mentioned aqueous dispersions, stirs evenly, mixes, stirs with above-mentioned epoxy silane alcoholic solution
Reaction 3-4 hours is mixed, ethyl alcohol is distilled off to get the sol dispersion.
2. a kind of preparation method of sol dispersion according to claim 1, it is characterised in that：The colloidal dispersion
The preparation of liquid, is counted in parts by weight, and each raw material is：0.3-1 parts of propylgallate, 40-50 parts of ethyl orthosilicate, ricinoleic acid
0.1-0.3 parts of zinc, 1-2 parts of ammonium polyphosphate, 1-2 parts of silane coupling agent kh560.
3. a kind of application of sol dispersion, it is characterised in that：In preparation applied to colloidal sol polyaniline film.
4. a kind of application of sol dispersion according to claim 3, it is characterised in that：The colloidal sol polyaniline film
Preparation, preparation method is：1）Polyaniline solutions, sol dispersion are mixed, stirred evenly, Sucrose Acetate acid sucrose is added
Ester, it is 100-110 DEG C to increase temperature, and insulated and stirred 1-2 hours is filtered, filter cake washed, air drying, is obtained sol-gel modified poly-
Aniline；2）Take sol-gel modified polyaniline, be added in the dimethylformamide of 10-18 times of its weight, stir evenly, spin coating at
Film is to get the colloidal sol polyaniline film.
5. a kind of application of sol dispersion according to claim 4, it is characterised in that：The polyaniline solutions by
Following steps are made：
1）The preparation of chloroformic solution
8-hydroxyquinoline, thiol-butyl tin mixing are taken, is added in the chloroform of 2-4 times of mixture weight, it is 10-20 minutes ultrasonic,
Obtain chloroformic solution；
2）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, obtain ammonium persulfate aqueous solution；
3）The preparation of polyaniline solutions
Sym-closene is taken, is mixed with aniline, is added in the deionized water of 10-15 times of mixture weight, stirs evenly, send
Enter into reaction kettle, be passed through nitrogen, it is 60-70 DEG C to adjust temperature of reaction kettle, and ammonium persulfate aqueous solution, insulated and stirred 3-4 is added
Hour, above-mentioned chloroformic solution is added, is stirred to react 1-2 hours, discharging cooling obtains polyaniline solutions.
6. a kind of application of sol dispersion according to claim 5, it is characterised in that：It counts in parts by weight, each raw material
For：140-160 parts of aniline, 60-70 parts of sol dispersion, 1-2 parts of Sucrose acetoisobutyrate, 0.1-0.4 parts of thiol-butyl tin,
1-2 parts of 8-hydroxyquinoline, 3-5 parts of sym-closene, 4-5 parts of ammonium persulfate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810408412.7A CN108586812A (en) | 2018-05-02 | 2018-05-02 | A kind of preparation method and applications of sol dispersion |
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| CN201810408412.7A CN108586812A (en) | 2018-05-02 | 2018-05-02 | A kind of preparation method and applications of sol dispersion |
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| CN104893170A (en) * | 2015-06-16 | 2015-09-09 | 合肥吉科新材料有限公司 | Composite silanized plastic |
| CN105175769A (en) * | 2015-09-21 | 2015-12-23 | 常州大学 | Preparing method for silicon-containing optical anti-reflection polyester film |
| CN105754337A (en) * | 2016-04-06 | 2016-07-13 | 汤卓群 | Nanocomposite film material used for capacitor and preparation method thereof |
| CN106012568A (en) * | 2016-08-03 | 2016-10-12 | 浙江汇锋新材料股份有限公司 | Tent cloth with anti-ultraviolet function and processing method thereof |
| CN106749856A (en) * | 2016-12-23 | 2017-05-31 | 上海正欧实业有限公司 | Ludox and preparation method thereof, acrylic resin, acrylic acid double-component polyurethane coating |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
| CN107880458A (en) * | 2017-12-06 | 2018-04-06 | 安徽鸿宾医药包装有限公司 | A kind of antibacterial medical package film of Ludox and preparation method thereof |
-
2018
- 2018-05-02 CN CN201810408412.7A patent/CN108586812A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434709A (en) * | 2008-12-09 | 2009-05-20 | 西安交通大学 | Preparation of silastic surface hydrophobic coating |
| CN104893170A (en) * | 2015-06-16 | 2015-09-09 | 合肥吉科新材料有限公司 | Composite silanized plastic |
| CN105175769A (en) * | 2015-09-21 | 2015-12-23 | 常州大学 | Preparing method for silicon-containing optical anti-reflection polyester film |
| CN105754337A (en) * | 2016-04-06 | 2016-07-13 | 汤卓群 | Nanocomposite film material used for capacitor and preparation method thereof |
| CN106012568A (en) * | 2016-08-03 | 2016-10-12 | 浙江汇锋新材料股份有限公司 | Tent cloth with anti-ultraviolet function and processing method thereof |
| CN106749856A (en) * | 2016-12-23 | 2017-05-31 | 上海正欧实业有限公司 | Ludox and preparation method thereof, acrylic resin, acrylic acid double-component polyurethane coating |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
| CN107880458A (en) * | 2017-12-06 | 2018-04-06 | 安徽鸿宾医药包装有限公司 | A kind of antibacterial medical package film of Ludox and preparation method thereof |
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Application publication date: 20180928 |