CN107474180A - A kind of preparation method of silicon dioxide polyester emulsion - Google Patents
A kind of preparation method of silicon dioxide polyester emulsion Download PDFInfo
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- CN107474180A CN107474180A CN201710793783.7A CN201710793783A CN107474180A CN 107474180 A CN107474180 A CN 107474180A CN 201710793783 A CN201710793783 A CN 201710793783A CN 107474180 A CN107474180 A CN 107474180A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of preparation method of silicon dioxide polyester emulsion, the present invention is first using tetraethyl orthosilicate as presoma, obtained silica is organised, it is subsequently dispersed in deionized water, participate in again in the polymerisation of methyl methacrylate, silica is effectively distributed in polyester liquid, effectively reduces reunion, improves the uniform and stable property of finished emulsion.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of silicon dioxide polyester emulsion.
Background technology
Polymethyl methacrylate, acrylics are referred to as with the polymer obtained by acrylicacidandesters Type of Collective,
Corresponding plastics are referred to as polyacrylic plastics, wherein most widely used with polymethyl ester methyl ester.Poly-methyl methacrylate
Ester abbreviation code name be PMMA, also known as does acryl or lucite, the referred to as A Jiali glue more than Hong Kong, has the high grade of transparency, low
Price, be easy to machining the advantages that, be so far synthesize transparent material in quality it is most excellent, price again than convenient product
Kind.PMMA is dissolved in organic solvent, such as phenol, methyl phenyl ethers anisole etc., and good film can be formed by spin coating, has good dielectric
Performance, organic field-effect tube can be used as（OFET, also known as OTFT）Dielectric layer.
Application number：201510728207.5 disclosing a kind of polyester fiber and preparation method thereof, the polyester fiber includes such as
The raw material components of lower parts by weight：Polyethylene terephthalate 60-80 parts, polyoxyethylene 6-20 parts, nano silicon 10-12
Part, rare-earth coupling agent 2-4 parts, chain branching agent 2-4 parts.The present invention is by the way that polyoxyethylene, nano silicon and rare earth are coupled
It is incorporated into after agent and chain branching agent heating in polyethylene terephthalate, forms poly- polyester composition；Again by the poly- polyester
Composition carries out melt spinning after drying, and is spun into polyester fiber.Polyester fiber provided by the invention have excellent physics and
Chemical property, there is important application value.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of system of silicon dioxide polyester emulsion
Preparation Method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of silicon dioxide polyester emulsion, comprises the following steps：
（1）The tetraethyl orthosilicate of 20-30 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, is dripped
Add 10-12% ammoniacal liquor, regulation pH is 10-11, stirring reaction 2-3 hours, adds the p-methyl benzenesulfonic acid of 0.8-2 parts by weight, rises
High-temperature is 60-70 DEG C, insulated and stirred 40-50 minutes, filtering, precipitation is washed, and 1-2 hours are dried at 90-100 DEG C of vacuum,
Normal temperature is cooled to, obtains carboxylated silica；
（2）The magnesium stearate mixing of the 8-hydroxyquinoline, 2-3 parts by weight of 0.7-1 parts by weight is taken, is added to compound weight 5-9
In pentaerythrite again, stir, obtain alcohol dispersion liquid；
（3）The glyceryl tristearate of 1-2 parts by weight is taken, is added in the nylon acid methyl esters of 4-5 times of its weight, stirs,
The tert-butyl group of 0.3-0.5 parts by weight is added to biphenol, the insulated and stirred 10-20 minutes at 60-65 DEG C, is disperseed with above-mentioned alcohol
Liquid, the mixing of carboxylated silica, insulated and stirred 1-2 hours, are cooled to normal temperature at 90-95 DEG C, obtain titanium dioxide estersil and disperse
Liquid；
（4）The allylthiourea of 1-2 parts by weight is taken, is added in the tetrahydrofuran of 6-10 times of its weight, stirs, in addition
Titanium dioxide estersil dispersion liquid is stated, is stirred, adds the dimethyl suflfate of 1-2 parts by weight, rise temperature is 40-50 DEG C, is added
The lithium hydroxide of 0.1-0.2 parts by weight, insulated and stirred 3-4 hours, filtering, precipitation is washed, air drying, must methylate dioxy
SiClx；
（5）Above-mentioned methylated silicon dioxide is taken, is added in the deionized water of 60-73 times of its weight, stirs, adds 4-6
The allyl polyglycol of parts by weight, ultrasonic 4-10 minutes, obtain silica dispersions；
（6）The ammonium persulfate of 0.7-1 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs, must be drawn
Send out agent solution；
（7）The acrylic acid mixing of the methyl methacrylate, 2-3 parts by weight of 50-60 parts by weight is taken, is added to above-mentioned silica
In dispersion liquid, stir, be sent in reactor, be passed through nitrogen, rise temperature is 60-70 DEG C, and it is molten that above-mentioned initiator is added dropwise
Liquid, rear insulated and stirred 2-3 hours are added dropwise, discharging cooling, produce the silicon dioxide polyester emulsion.
Advantages of the present invention：
The present invention is hydrolyzed under ammoniacal liquor effect using tetraethyl orthosilicate as presoma, is then handled, obtained using p-methyl benzenesulfonic acid
Carboxylated silica, is then mixed with pentaerythrite, is esterified under high temperature, titanium dioxide estersil dispersion liquid is obtained, then with sulfuric acid two
Methyl esters is methylating reagent, and tetrahydrofuran is solvent, and lithium hydroxide is catalyst, methylated silicon dioxide is obtained, then with over cure
Sour ammonium is initiator, and methyl methacrylate is monomer, is polymerize by solvent of silica dispersions, obtains silica
Polyester emulsion；
Obtained silica is organised first using tetraethyl orthosilicate as presoma, is subsequently dispersed deionized water by the present invention
In, then participate in the polymerisation of methyl methacrylate, silica is effectively distributed in polyester liquid, effectively
Reduce and reunite, improve the uniform and stable property of finished emulsion.
Embodiment
Embodiment 1
A kind of preparation method of silicon dioxide polyester emulsion, comprises the following steps：
（1）The tetraethyl orthosilicate of 20 parts by weight is taken, is added in the deionized water of 30 times of its weight, is stirred, be added dropwise 10%
Ammoniacal liquor, regulation pH are 10, stirring reaction 2 hours, add the p-methyl benzenesulfonic acid of 0.8 parts by weight, and rise temperature is 60 DEG C, insulation
Stirring 40 minutes, filtering, precipitation is washed, dried 1 hour at 90 DEG C of vacuum, be cooled to normal temperature, obtain carboxylated silica；
（2）The magnesium stearate mixing of the 8-hydroxyquinoline, 2 parts by weight of 0.7 parts by weight is taken, is added to the season of 5 times of compound weight
In penta tetrol, stir, obtain alcohol dispersion liquid；
（3）The glyceryl tristearate of 1 parts by weight is taken, is added in the nylon acid methyl esters of 4 times of its weight, stirs, is added
The tert-butyl group of 0.3 parts by weight is to biphenol, insulated and stirred 10 minutes at 60 DEG C, with above-mentioned alcohol dispersion liquid, carboxylated titanium dioxide
Silicon mixes, and insulated and stirred 1 hour, is cooled to normal temperature at 90 DEG C, obtains titanium dioxide estersil dispersion liquid；
（4）The allylthiourea of 1 parts by weight is taken, is added in the tetrahydrofuran of 6 times of its weight, stirs, adds above-mentioned two
Estersil dispersion liquid is aoxidized, is stirred, adds the dimethyl suflfate of 1 parts by weight, rise temperature is 40 DEG C, adds 0.1 parts by weight
Lithium hydroxide, insulated and stirred 3 hours, filtering, will precipitation washing, air drying, obtain methylated silicon dioxide；
（5）Above-mentioned methylated silicon dioxide is taken, is added in the deionized water of 60 times of its weight, stirs, adds 4 parts by weight
Allyl polyglycol, ultrasound 4 minutes, obtain silica dispersions；
（6）The ammonium persulfate of 0.7 parts by weight is taken, is added in the deionized water of 20 times of its weight, is stirred, it is molten to obtain initiator
Liquid；
（7）The acrylic acid mixing of the methyl methacrylate, 2 parts by weight of 50 parts by weight is taken, above-mentioned silica is added to and disperses
In liquid, stir, be sent in reactor, be passed through nitrogen, rise temperature is 60 DEG C, and above-mentioned initiator solution is added dropwise, and is added dropwise
After insulated and stirred 2 hours, discharging cooling, produce the silicon dioxide polyester emulsion.
Claims (1)
1. a kind of preparation method of silicon dioxide polyester emulsion, it is characterised in that comprise the following steps：
（1）The tetraethyl orthosilicate of 20-30 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, is dripped
Add 10-12% ammoniacal liquor, regulation pH is 10-11, stirring reaction 2-3 hours, adds the p-methyl benzenesulfonic acid of 0.8-2 parts by weight, rises
High-temperature is 60-70 DEG C, insulated and stirred 40-50 minutes, filtering, precipitation is washed, and 1-2 hours are dried at 90-100 DEG C of vacuum,
Normal temperature is cooled to, obtains carboxylated silica；
（2）The magnesium stearate mixing of the 8-hydroxyquinoline, 2-3 parts by weight of 0.7-1 parts by weight is taken, is added to compound weight 5-9
In pentaerythrite again, stir, obtain alcohol dispersion liquid；
（3）The glyceryl tristearate of 1-2 parts by weight is taken, is added in the nylon acid methyl esters of 4-5 times of its weight, stirs,
The tert-butyl group of 0.3-0.5 parts by weight is added to biphenol, the insulated and stirred 10-20 minutes at 60-65 DEG C, is disperseed with above-mentioned alcohol
Liquid, the mixing of carboxylated silica, insulated and stirred 1-2 hours, are cooled to normal temperature at 90-95 DEG C, obtain titanium dioxide estersil and disperse
Liquid；
（4）The allylthiourea of 1-2 parts by weight is taken, is added in the tetrahydrofuran of 6-10 times of its weight, stirs, in addition
Titanium dioxide estersil dispersion liquid is stated, is stirred, adds the dimethyl suflfate of 1-2 parts by weight, rise temperature is 40-50 DEG C, is added
The lithium hydroxide of 0.1-0.2 parts by weight, insulated and stirred 3-4 hours, filtering, precipitation is washed, air drying, must methylate dioxy
SiClx；
（5）Above-mentioned methylated silicon dioxide is taken, is added in the deionized water of 60-73 times of its weight, stirs, adds 4-6
The allyl polyglycol of parts by weight, ultrasonic 4-10 minutes, obtain silica dispersions；
（6）The ammonium persulfate of 0.7-1 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs, must be drawn
Send out agent solution；
（7）The acrylic acid mixing of the methyl methacrylate, 2-3 parts by weight of 50-60 parts by weight is taken, is added to above-mentioned silica
In dispersion liquid, stir, be sent in reactor, be passed through nitrogen, rise temperature is 60-70 DEG C, and it is molten that above-mentioned initiator is added dropwise
Liquid, rear insulated and stirred 2-3 hours are added dropwise, discharging cooling, produce the silicon dioxide polyester emulsion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710793783.7A CN107474180A (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of silicon dioxide polyester emulsion |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710793783.7A CN107474180A (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of silicon dioxide polyester emulsion |
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| CN107474180A true CN107474180A (en) | 2017-12-15 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908022A (en) * | 2006-08-11 | 2007-02-07 | 中山耐乐生物科技有限公司 | Process for preparing room temperature self-crosslinking acrylic ester emulsion modified by inorganic nano particle |
| CN101638464A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing polyurethane-polyacrylic ester microemulsion |
| CN106380761A (en) * | 2016-08-30 | 2017-02-08 | 宁波通冠电气自动化设备有限公司 | Impact-resistant waterproof film and preparation method thereof |
| CN106497293A (en) * | 2016-12-09 | 2017-03-15 | 陕西高新实业有限公司 | Silicon dioxide, the preparation method of poly acrylate composite emulsion |
-
2017
- 2017-09-06 CN CN201710793783.7A patent/CN107474180A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908022A (en) * | 2006-08-11 | 2007-02-07 | 中山耐乐生物科技有限公司 | Process for preparing room temperature self-crosslinking acrylic ester emulsion modified by inorganic nano particle |
| CN101638464A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing polyurethane-polyacrylic ester microemulsion |
| CN106380761A (en) * | 2016-08-30 | 2017-02-08 | 宁波通冠电气自动化设备有限公司 | Impact-resistant waterproof film and preparation method thereof |
| CN106497293A (en) * | 2016-12-09 | 2017-03-15 | 陕西高新实业有限公司 | Silicon dioxide, the preparation method of poly acrylate composite emulsion |
Non-Patent Citations (1)
| Title |
|---|
| 赵存挺等: ""单分散纳米二氧化硅微球的制备及羧基化改性"", 《功能材料》 * |
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Application publication date: 20171215 |
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