CN109369842A - A kind of preparation method of compound acrylic ester lotion - Google Patents
A kind of preparation method of compound acrylic ester lotion Download PDFInfo
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- CN109369842A CN109369842A CN201811156419.0A CN201811156419A CN109369842A CN 109369842 A CN109369842 A CN 109369842A CN 201811156419 A CN201811156419 A CN 201811156419A CN 109369842 A CN109369842 A CN 109369842A
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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
- C08K3/32—Phosphorus-containing compounds
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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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- 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Cosmetics (AREA)
Abstract
The present invention discloses a kind of preparation method of compound acrylic ester lotion, polyoxethylene octylphenyl phenol ether -10 is added in emulsifying kettle, lauryl sodium sulfate, ammonium persulfate, then deionized water is added, stirring and dissolving, butyl acrylate is sequentially added in pre-emulsification kettle, methyl methacrylate, methacrylic acid, stirring and emulsifying obtains the pre-emulsion of monomer, sodium bicarbonate and deionized water are sequentially added in polymeric kettle, start stirring be allowed to dissolution be placed in 50 DEG C of water-baths, then constant pressure funnel is installed, it weighs 5 parts of the monomer pre-emulsion made and is added in polymeric kettle, modifted-nano-hydroxyapatite material is added, weigh ammonium persulfate and soluble in water, it is slowly added into polymeric kettle, adjusting bath temperature simultaneously is 82 DEG C of slowly heatings, after temperature is upgraded to 82 DEG C, monomer pre-emulsion is slowly added dropwise, it drips off Water rinses pre-emulsification kettle and is added dropwise in polymeric kettle afterwards, is 8 with ammonium hydroxide tune pH value, obtains composite Nano acrylic acid ester emulsion.
Description
Technical field
The present invention relates to a kind of preparation methods of compound acrylic ester lotion.
Background technique
Polyacrylate dispersion with its excellent performance paint, coating, adhesive, fabric finishing agent, leather finish and
The industries such as ink obtain very extensive application.But most of polyacrylate dispersion is ordinary emulsion, partial size is larger,
Majority is White-opalescent low viscosity colloidal dispersion of the partial size at 0.1~1 μm.
The properties such as skin effect, small-size effect, quantum size effect due to nano material, so nanometer polymer grain
Son has high surface energy amount and low film-forming temperature with nanoparticle, and higher glass can be obtained under same film-forming temperature
Change the paint film of temperature, to have better weatherability and anti-fouling performance.The colloid diameter of general polymerization object lotion is greater than
100nm, and partial size can directly be prepared in the nano grade polymer micelle of 10-50nm by rising micro-emulsion polymerization the beginning of the eighties,
This kind of nano rubber latex can effectively improve the properties such as filming performance, film consistency, the finish of lotion.With miniemulsion polymerization
For the perfect of technology, have become possibility with this kind of nanometer polymer latex to prepare water paint.
Summary of the invention
The invention discloses a kind of preparation method of compound acrylic ester lotion, the acrylic acid ester emulsion of preparation has excellent
Physical property.
A kind of preparation method of compound acrylic ester lotion, emulsifying kettle is interior to be added 0.30 part of polyoxethylene octylphenyl phenol ether-
10, then 0.3 part of lauryl sodium sulfate, 0.15 part of ammonium persulfate are added 20 parts of deionized water, start stirring and be allowed to all
Dissolution, sequentially adds butyl acrylate, methyl methacrylate, methacrylic acid, stirring and emulsifying 15min in pre-emulsification kettle
The pre-emulsion of monomer is obtained, sequentially add 0.2 part of sodium bicarbonate in the polymeric kettle equipped with stirring, reflux condensing tube and is gone
30 parts of ionized water, start stirring be allowed to dissolution be placed in 50 DEG C of water-baths,
Then constant pressure funnel is installed, 5 parts of the monomer pre-emulsion made is weighed and is added in polymeric kettle, is added 0.3 part
Modifted-nano-hydroxyapatite material weighs 0.3 part of ammonium persulfate and is dissolved in 5 parts of water, is slowly added into polymeric kettle, simultaneously
Adjusting bath temperature is 82 DEG C of slowly heatings, and after temperature is upgraded to 82 DEG C, monomer pre-emulsion is slowly added dropwise, and 2h or so is dripped off,
After take 5 parts of water to rinse pre-emulsification kettles and be added dropwise in polymeric kettle, be 8 with ammonium hydroxide tune pH value, obtain composite Nano propylene
Acid esters lotion.
The preparation of modifted-nano-hydroxyapatite material is as follows: 20 parts of diameter 40nm nanometer hydroxyapatite powder are distributed to
In 200 parts of water, with salt acid for adjusting pH to 5, then 5 parts of epoxychloropropane (mass concentration 99%, commercially available analysis are pure) are added drop-wise to
In above-mentioned solution, 25 DEG C of reaction 6h are filtered to remove the epoxychloropropane for having neither part nor lot in reaction, obtain epoxychloropropane modified nanometer hydroxyl
Base apatite；4wt% over-branched polyamidoamine (2 parts) acid solution is added to epoxychloropropane modified nanometer hydroxyapatite
In (20 parts), 4%NaOH solution (200 parts) then are added, then 40 DEG C of stirring 2h filter nanometer hydroxyapatite, wash
It is put into drying in oven to neutrality, obtains modified ultra-branching polyamide nano hydroxyapatite.
The utility model has the advantages that the oxygen atom on the carbonyl of nanometer hydroxyapatite surface can be with the carboxyl or hydroxyl of monomer pre-emulsion
Base junction closes to form hydrogen bond, and forms a polymeric layer in microsphere surface, reduces nano-substance agglomeration, enhances lotion stream
Denaturation, the nanometer hydroxyapatite after modified ultra-branching polyamide have small-size effect, can be filled into lotion overlay film,
Effectively enhance the physical isolation effect of emulsion coating.In addition, nanometer hydroxyapatite in situ Polymerization generates polyamide,
It is added in lotion, improves the mechanical performance of coating, the ultrabranching polyamide in its duct extends at aperture and matrix
Latex generates new keys, increases the crosslink density of system, and then the tensile strength of film and elongation at break is made to be multiplied.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1
0.30 part of polyoxethylene octylphenyl phenol ether -10 is added in a kind of preparation method of compound acrylic ester lotion in emulsifying kettle
, 0.3 part of lauryl sodium sulfate, 0.15 part of ammonium persulfate, then be added 20 parts of deionized water, start stirring be allowed to all it is molten
Solution, sequentially adds 15 parts of butyl acrylates, 20 parts of methyl methacrylates, 2 parts of methacrylic acids in pre-emulsification kettle, stirs
Emulsification 15min obtains the pre-emulsion of monomer, sequentially adds sodium bicarbonate in the polymeric kettle equipped with stirring, reflux condensing tube
0.2 part and 30 parts of deionized water, start stirring and are allowed to dissolution and be placed in 50 DEG C of water-baths,
Then constant pressure funnel is installed, 5 parts of the monomer pre-emulsion made is weighed and is added in polymeric kettle, is added 0.3 part
Modifted-nano-hydroxyapatite material weighs 0.3 part of ammonium persulfate and is dissolved in 5 parts of water, is slowly added into polymeric kettle, simultaneously
Adjusting bath temperature is 82 DEG C of slowly heatings, and after temperature is upgraded to 82 DEG C, monomer pre-emulsion is slowly added dropwise, 5m parts are taken after dripping off
Water rinses pre-emulsification kettle and is added dropwise in polymeric kettle, is 8 with ammonium hydroxide tune pH value, obtains composite Nano acrylic acid ester emulsion.
The preparation of modifted-nano-hydroxyapatite material is as follows: 20 parts of diameter 40nm nanometer hydroxyapatite powder are distributed to
In 200 parts of water, with salt acid for adjusting pH to 5, then 5 parts of epoxychloropropane (mass concentration 99%, commercially available analysis are pure) are added drop-wise to
In above-mentioned solution, 25 DEG C of reaction 6h are filtered to remove the epoxychloropropane for having neither part nor lot in reaction, obtain epoxychloropropane modified nanometer hydroxyl
Base apatite；4wt% over-branched polyamidoamine (2 parts) acid solution is added to epoxychloropropane modified nanometer hydroxyapatite
In (20 parts), 4%NaOH solution (200 parts) then are added, then 40 DEG C of stirring 2h filter nanometer hydroxyapatite, wash
It is put into drying in oven to neutrality, obtains modified ultra-branching polyamide nano hydroxyapatite.
Embodiment 2
It is with 1 difference of embodiment,
20 parts of butyl acrylates, 15 parts of methyl methacrylates, 2 parts of methacrylic acids, remaining is all the same.
Embodiment 3
It is with 1 difference of embodiment,
15 parts of butyl acrylates, 15 parts of methyl methacrylates, 1 part of methacrylic acid, remaining is all the same.
Comparative example 1
It is with 1 difference of embodiment,
It is added without modifted-nano-hydroxyapatite material.
Comparative example 2
It is with 1 difference of embodiment,
Nanometer hydroxyapatite powder is common hydroxyapatite material without modification.
Comparative example 3
It is with 1 difference of embodiment,
Modifted-nano-hydroxyapatite material is epoxychloropropane modified nanometer hydroxyapatite rather than modified ultra-branching polyamides
Amine nanometer hydroxyapatite.
The test data explanation of mechanical mechanics property and water resistance in following table after each embodiment and comparative example emulsion film forming
The test display embodiment of the present invention has excellent mechanical mechanics property and water resistance.
Claims (2)
1. a kind of preparation method of compound acrylic ester lotion, which is characterized in that 0.30 part of polyoxyethylene is added in emulsifying kettle
Then octyl phenol ether -10,0.3 part of lauryl sodium sulfate, 0.15 part of ammonium persulfate are added 20 parts of deionized water, start and stir
It mixes and is allowed to whole dissolutions, butyl acrylate, methyl methacrylate, methacrylic acid are sequentially added in pre-emulsification kettle, stir
Emulsification 15min obtains the pre-emulsion of monomer,
0.2 part of sodium bicarbonate and 30 parts of deionized water are sequentially added in the polymeric kettle equipped with stirring, reflux condensing tube, starts and stirs
It mixes to be allowed to dissolve and be placed in 50 DEG C of water-baths,
Then constant pressure funnel is installed, 5 parts of the monomer pre-emulsion made is weighed and is added in polymeric kettle, is added 0.3 part
Modifted-nano-hydroxyapatite material weighs 0.3 part of ammonium persulfate and is dissolved in 5 parts of water, is slowly added into polymeric kettle, simultaneously
Adjusting bath temperature is 82 DEG C of slowly heatings, and after temperature is upgraded to 82 DEG C, monomer pre-emulsion is slowly added dropwise, 5 parts are taken after dripping off
Water rinses pre-emulsification kettle and is added dropwise in polymeric kettle, is 8 with ammonium hydroxide tune pH value, obtains composite Nano acrylic acid ester emulsion.
2. a kind of preparation method of compound acrylic ester lotion according to claim 1, which is characterized in that modified Nano hydroxyl
Base Apatite materials use hydrochloric acid the preparation method is as follows: 20 parts of diameter 40nm nanometer hydroxyapatite powder are distributed in 200 parts of water
PH to 5 is adjusted, then 5 parts of epoxychloropropane are added drop-wise in above-mentioned solution, 25 DEG C of reaction 6h are filtered to remove and have neither part nor lot in reaction
Epoxychloropropane obtains epoxychloropropane modified nanometer hydroxyapatite；2 parts of 4wt% over-branched polyamidoamine acidity is molten
Liquid is added in 20 parts of epoxychloropropane modified nanometer hydroxyapatite, 200 parts of 4%NaOH solution is then added, 40 DEG C are stirred
2h is mixed, then filters nanometer hydroxyapatite, neutrality is washed to and is put into drying in oven, modified ultra-branching polyamide is obtained and receives
Rice hydroxyapatite.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811156419.0A CN109369842B (en) | 2018-09-30 | 2018-09-30 | Preparation method of composite acrylate emulsion |
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| CN201811156419.0A CN109369842B (en) | 2018-09-30 | 2018-09-30 | Preparation method of composite acrylate emulsion |
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| CN109369842A true CN109369842A (en) | 2019-02-22 |
| CN109369842B CN109369842B (en) | 2021-03-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663327A (en) * | 2020-06-05 | 2020-09-15 | 西安工程大学 | Preparation method of polyacrylic acid based graphene core-shell structure composite fiber |
| CN112251097A (en) * | 2020-10-20 | 2021-01-22 | 汤普勒新材料嘉兴有限公司 | Multifunctional polyacrylate nano composite coating agent and preparation method thereof |
| CN115926566A (en) * | 2022-11-21 | 2023-04-07 | 南昌大学 | Temporary protective coating for surface of nuclear fuel rod and preparation method thereof |
| CN117004281A (en) * | 2023-08-04 | 2023-11-07 | 南昌大学 | Preparation method of temporary coating and application of temporary coating on surface of zirconium alloy cladding |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663327A (en) * | 2020-06-05 | 2020-09-15 | 西安工程大学 | Preparation method of polyacrylic acid based graphene core-shell structure composite fiber |
| CN112251097A (en) * | 2020-10-20 | 2021-01-22 | 汤普勒新材料嘉兴有限公司 | Multifunctional polyacrylate nano composite coating agent and preparation method thereof |
| CN115926566A (en) * | 2022-11-21 | 2023-04-07 | 南昌大学 | Temporary protective coating for surface of nuclear fuel rod and preparation method thereof |
| CN117004281A (en) * | 2023-08-04 | 2023-11-07 | 南昌大学 | Preparation method of temporary coating and application of temporary coating on surface of zirconium alloy cladding |
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| CN109369842B (en) | 2021-03-23 |
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