CN109160971A - A kind of phenylpropyl alcohol water-proof emulsion and preparation method thereof - Google Patents
A kind of phenylpropyl alcohol water-proof emulsion and preparation method thereof Download PDFInfo
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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
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- 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
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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Abstract
The invention discloses a kind of phenylpropyl alcohol water-proof emulsion and preparation method thereof, which includes the raw material of following parts by weight: 20-30 parts of styrene, 10-18 parts of methyl methacrylate, 12-20 parts of methyl acrylate, 40-50 parts of butyl acrylate, 0.2-0.8 parts of acrylic acid, 1.0-2.0 parts of acrylamide, 1-3 parts of emulsifier, 0.5-1.5 parts of initiator, 0.2-0.8 parts of buffer.The cohesion rate of water-proof emulsion of the invention is low, consistency is moderate, efficiently solves the compatibility issue of the powders such as phenylpropyl alcohol water-proof emulsion and cement, the poor compatibility after solving the problems, such as polymeric and cement film forming；Lotion flexibility with super strength, tensile strength and elongation at break are much higher than requirements of the national standard and are better than the water-proof emulsion of better performances on the market, stable product quality, in practical applications, guarantee that the adhesion strength of film and basal plane is high, water resistance, alkali resistance, weather resistance are good.
Description
Technical field
The invention belongs to the technical fields of construction material, and in particular to a kind of phenylpropyl alcohol water-proof emulsion and preparation method thereof.
Technical background
JS water-repellent paint is combined by organic material and inorganic material, has had both that organic material is flexible and inorganic material
The strong advantage of rigidity has the characteristics that big elastic height, elongation percentage, durability and water-tolerant.Since coating resin lotion is
Water-based system, product is nontoxic and pollution-free, clean and environmental protection, and transport and construction safety have compared with other waterproof materials without comparable
Quasi- advantage.
Currently, common JS water-repellent paint resin emulsion mainly has polyacrylate dispersion, polyvinyl acetate in the market
Ester-vac emulsion and Polystyrene-acrylate lotion, in addition there are the lotions such as the styrene-butadiene latex being just eliminated, polychloroprene latex.
Polyvinyl acetate-ethylene lotion contains the ester group of a large amount of hydrolyzables due to polymer molecule segment, in strong basicity after film forming
It is easily hydrolyzed under environment, to influence the water resistance of entire coating.And compared with pure acrylate copolymer, styrene with
The copolymer of acrylate monomer has more excellent water resistance, alkali resistance, and its sexual valence is relatively high, styrene-acrylic latex grain film forming
The flexible polymer network formed afterwards can fill up the pore that cement is formed in hydration process, bridge microcrack, be promoted whole
The cohesive force of a concrete structure, unique performance are particularly suitable in JS water-repellent paint.And traditional styrene-acrylic emulsion is anti-
α-H group during answering due to styrene segment is very active, easily occurs with acrylate monomer when dosage is more quick-fried
It is poly-, so that polymerization reaction kettle inner wall and agitating shaft is generated a large amount of structural gels, the MFFT of product emulsion is caused to increase, latex film
Water resistance decline.More seriously, the generation of a large amount of condensation products keeps raw material availability low in process of production, and production cost increases
Height, while also carrying out inconvenience to the cleaning tape of reaction kettle, increase unnecessary post-processing expense.Therefore, develop it is a
The phenylpropyl alcohol water-proof emulsion that there is polymerization stage lower condensation product to generate, is all very necessary in terms of economic and technical.
By the research and development and improvement of many years, although achieve in properties of product and quality can for polymer cement waterproof paint
The achievement of happiness, but there are still much can improvements.Not environmentally such as emulsion polymer, it with cement poor compatibility, is stirred with cement
It mixes rear dispersibility difference and is easy sedimentation；Polymer and cement compatibility are bad, occur organic inorganic phase separation after curing of coating, deposit
In microstructural flaws.Meanwhile the polymer cement ratio of commercially available polymer cement waterproof paint recommendation is excessive, cause cost compared with
Height, and it is difficult to the relationship of balanced stretch intensity and elongation at break.Therefore, a kind of environmentally friendly high performance polymer is studied
Cement waterproof paint lotion has very great economic benefit and social benefit.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of economic and environment-friendly, while the phenylpropyl alcohol of excellent combination property
Water-proof emulsion and preparation method thereof.
The technical scheme adopted by the invention is that:
A kind of phenylpropyl alcohol water-proof emulsion, which is characterized in that the lotion includes the raw material of following parts by weight: 20-30 parts of styrene,
10-18 parts of methyl methacrylate, 12-20 parts of methyl acrylate, 40-50 parts of butyl acrylate, 0.2-0.8 parts of acrylic acid, third
1.0-2.0 parts of acrylamide, 1-3 parts of emulsifier, 0.5-1.5 parts of initiator, 0.2-0.8 parts of buffer.
The present invention using styrene, methyl methacrylate, methyl acrylate, butyl acrylate as main monomer, with acrylic acid,
Acrylamide is function monomer, and main monomer, function monomer and other raw materials act synergistically, and obtains a kind of preventing for excellent combination property
Aqueous emulsion.
Further, the emulsifier is lauryl sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate salt, alkyl phenol gather
One of ethylene oxide ether.The emulsifier is anionic emulsifier, and the hydrophilic radical of anionic emulsifier is anion,
Using anion emulsifier, monomer droplet surface can take one layer of negative electrical charge, since there are electrostatic repulsions between monomer droplet
Power, therefore be difficult to hit the big droplet of synthesis between small droplet, stable emulsion system can be formed, is closed using anionic emulsifier
At water-proof emulsion and cement compatibility it is good, application performance is excellent in water-repellent paint.
Further, the initiator is one of sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) emulsifier, deionized water are uniformly mixed at room temperature, styrene, the first of above-mentioned parts by weight is then added
Base methyl acrylate, methyl acrylate, butyl acrylate, acrylic acid, total amount 60-70% acrylamide, while opening stirring
Device is stirred, and obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 75-85 DEG C, and total amount 10- is then added
The pre-emulsion that 15% the step of (1) obtains, after temperature plateau in reaction kettle, the initiator for adding total amount 20-30% is molten
Liquid carries out emulsion polymerization 40-60min, obtains seed emulsion；
(3) 75-85 DEG C of temperature in reaction kettle is kept, the pre-emulsion that remaining step (1) obtains is added dropwise to reaction kettle,
And the initiator solution of total amount 55-65% is added dropwise simultaneously, time for adding control starts in 3-4h when half is added dropwise in pre-emulsion
Remaining acrylamide is added dropwise；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 75-85 DEG C, and remaining initiation is added
Agent solution is added dropwise to complete in 15-30min, drips off subsequent continuous insulation reaction 1-2h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 50-60 DEG C, then stirring heat preservation 10-20min, will react
Temperature in kettle is down to room temperature, and the water-proof emulsion is obtained after strainer filtering.
The present invention forms cross-linked structure by the improvement to monomer addition technique, and synthesis obtains the anti-of excellent combination property
Aqueous emulsion, function monomer acrylamide can make it effectively react generation one with acrylic acid using adding manner stage by stage
Fixed crosslink density forms the structure of micro- crosslinking, has the tensile strength of water-repellent paint and elongation at break a degree of
It improves, effectively promotes application performance of the water-proof emulsion in water-repellent paint.Water-proof emulsion simple process, green is synthesized by the method
Color is pollution-free, monomer conversion is high, quality of the emulsion is stable, cohesion rate is low, consistency is moderate, economic and environment-friendly.
Wherein, in step (3), the acrylamide of dropwise addition is the acrylamide aqueous solution of mass fraction 10-20%.
In step (3), the time difference that acrylamide and pre-emulsion are added dropwise is within ± 5min.
In step (5), the mesh number of strainer is 300 mesh.
Dropwise addition in above-mentioned steps is at the uniform velocity to be added dropwise, and the speed of stirring is 200-260rpm.
The invention has the following beneficial effects:
(1) the cohesion rate of water-proof emulsion of the invention is low, consistency is moderate, efficiently solves phenylpropyl alcohol water-proof emulsion and cement etc.
The compatibility issue of powder, the poor compatibility after solving the problems, such as polymeric and cement film forming；
(2) water-proof emulsion of the invention flexibility with super strength, tensile strength and elongation at break are much higher than country
Standard requirements and the water-proof emulsion for being better than better performances on the market, stable product quality guarantee film and base in practical applications
The adhesion strength in face is high, and water resistance, alkali resistance, weather resistance are good；
(3) preparation process of the invention is simple, emulsion coagulation rate is low, monomer conversion is high, green non-pollution, economic ring
It protects, be conducive to construction.The polymer cement waterproof paint tensile strength made from the water-proof emulsion and elongation at break are much higher than
Requirements of the national standard and the water-proof emulsion for being better than better performances on the market, flexibility with super strength, stable product quality are conducive to
Construction, has a extensive future.
Specific embodiment
The invention will be further described combined with specific embodiments below.
In following embodiments, if not otherwise indicated, agents useful for same and material are that conventional commercial can obtain.
Embodiment 1
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 25 parts of styrene, 15 parts of methyl methacrylate, third
15 parts of e pioic acid methyl ester, 45 parts of butyl acrylate, 0.6 part of acrylic acid, 1.5 parts of acrylamide, 2 parts of lauryl sodium sulfate, over cure
1.0 parts of sour sodium, 0.5 part of buffer sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) lauryl sodium sulfate, deionized water are uniformly mixed under 250rpm speed under room temperature (25 DEG C), so
Styrene, methyl methacrylate, methyl acrylate, butyl acrylate, the acrylic acid, total amount 65% of above-mentioned parts by weight are added afterwards
Acrylamide, while turn on agitator is stirred under 250rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 80 DEG C, and the step of total amount 15% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the sodium peroxydisulfate solution for adding total amount 25% carries out lotion
Polymerization reaction 50min, obtains seed emulsion；The sodium peroxydisulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the sodium peroxydisulfate solution of score 25%；
(3) the pre- cream that the step of keeping 80 DEG C of temperature in reaction kettle, residue 85% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the sodium peroxydisulfate solution of total amount 65% is at the uniform velocity added dropwise simultaneously, time for adding control is added dropwise one in 3.5h, in pre-emulsion
The acrylamide of residue 35% (is configured to the third of mass fraction 15% by the acrylamide for starting at the uniform velocity to be added dropwise residue 35% when half
Acrylamide aqueous solution is added dropwise)；Acrylamide is dripped with pre-emulsion with pre-emulsion simultaneously；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 80 DEG C, and the over cure of residue 10% is added
Acid sodium solution is added dropwise to complete in 20min, drips off subsequent continuous insulation reaction 1.5h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 60 DEG C, then stirring heat preservation 15min under 250rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.In above-mentioned steps,
The conversion ratio of monomer is 99.9%.
Embodiment 2
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 30 parts of styrene, 18 parts of methyl methacrylate, third
20 parts of e pioic acid methyl ester, 50 parts of butyl acrylate, 0.8 part of acrylic acid, 2.0 parts of acrylamide, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate
3 parts of salt, 1.5 parts of potassium peroxydisulfate, 0.8 part of buffer sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate salt, deionized water are stirred under 260rpm speed under room temperature (25 DEG C)
It is uniformly mixed, styrene, methyl methacrylate, methyl acrylate, butyl acrylate, the propylene of above-mentioned parts by weight is then added
The acrylamide of acid, total amount 70%, while turn on agitator is stirred under 260rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 85 DEG C, and the step of total amount 15% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the potassium persulfate solution for adding total amount 30% carries out lotion
Polymerization reaction 60min, obtains seed emulsion；The potassium peroxydisulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the potassium persulfate solution of score 25%；
(3) the pre- cream that the step of keeping 85 DEG C of temperature in reaction kettle, residue 85% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the potassium persulfate solution of total amount 65% is at the uniform velocity added dropwise simultaneously, half is added dropwise in 4h, in pre-emulsion in time for adding control
When start at the uniform velocity to be added dropwise the acrylamide of residue 30% and (acrylamide of residue 30% be configured to the propylene of mass fraction 20%
Amide aqueous solution is added dropwise)；Pre-emulsion is later than acrylamide 1min and is added dropwise；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 85 DEG C, and the over cure of residue 5% is added
Sour potassium solution, is added dropwise to complete in 30min, drips off subsequent continuous insulation reaction 2h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 60 DEG C, then stirring heat preservation 20min under 260rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.In above-mentioned steps,
The conversion ratio of monomer is 99.8%.
Embodiment 3
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 20 parts of styrene, 10 parts of methyl methacrylate, third
12 parts of e pioic acid methyl ester, 40 parts of butyl acrylate, 0.2 part of acrylic acid, 1.0 parts of acrylamide, 1.0 parts of alkyl phenol polyoxyethylene ether,
0.5 part of ammonium persulfate, 0.2 part of buffer sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) alkyl phenol polyoxyethylene ether, deionized water are uniformly mixed under 200rpm speed under room temperature (25 DEG C),
Then styrene, methyl methacrylate, methyl acrylate, butyl acrylate, the acrylic acid, total amount of above-mentioned parts by weight is added
60% acrylamide, while turn on agitator is stirred under 200rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 75 DEG C, and the step of total amount 10% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the ammonium persulfate solution for adding total amount 20% carries out lotion
Polymerization reaction 40min, obtains seed emulsion；The ammonium persulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the ammonium persulfate solution of score 25%；
(3) the pre- cream that the step of keeping 75 DEG C of temperature in reaction kettle, residue 90% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the ammonium persulfate solution of total amount 55% is at the uniform velocity added dropwise simultaneously, half is added dropwise in 3h, in pre-emulsion in time for adding control
When start at the uniform velocity to be added dropwise the acrylamide of residue 40% and (acrylamide of residue 40% be configured to the propylene of mass fraction 10%
Amide aqueous solution is added dropwise)；Acrylamide is later than pre-emulsion 2min and is added dropwise；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 75 DEG C, and the over cure of residue 25% is added
Acid ammonium solution is added dropwise to complete in 15min, drips off subsequent continuous insulation reaction 1h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 50 DEG C, then stirring heat preservation 10min under 200rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.In above-mentioned steps,
The conversion ratio of monomer is 99.8%.
Comparative example 1
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 25 parts of styrene, 15 parts of methyl methacrylate, third
15 parts of e pioic acid methyl ester, 45 parts of butyl acrylate, 0.6 part of acrylic acid, 2 parts of lauryl sodium sulfate, 1.0 parts of sodium peroxydisulfate, buffering
0.5 part of agent sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) lauryl sodium sulfate, deionized water are uniformly mixed under 250rpm speed under room temperature (25 DEG C), so
Styrene, methyl methacrylate, methyl acrylate, butyl acrylate, the acrylic acid of above-mentioned parts by weight are added afterwards, opens simultaneously
Blender is stirred under 250rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 80 DEG C, and the step of total amount 15% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the sodium peroxydisulfate solution for adding total amount 25% carries out lotion
Polymerization reaction 50min, obtains seed emulsion；The sodium peroxydisulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the sodium peroxydisulfate solution of score 25%；
(3) the pre- cream that the step of keeping 80 DEG C of temperature in reaction kettle, residue 85% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the sodium peroxydisulfate solution of total amount 65% is at the uniform velocity added dropwise simultaneously, time for adding is controlled in 3.5h；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 80 DEG C, and the over cure of residue 10% is added
Acid sodium solution is added dropwise to complete in 20min, drips off subsequent continuous insulation reaction 1.5h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 60 DEG C, then stirring heat preservation 15min under 250rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.
Comparative example 2
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 25 parts of styrene, 15 parts of methyl methacrylate, third
15 parts of e pioic acid methyl ester, 1.5 parts of acrylamide, 2 parts of lauryl sodium sulfate, 1.0 parts of sodium peroxydisulfate, delays 45 parts of butyl acrylate
0.5 part of electuary sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) lauryl sodium sulfate, deionized water are uniformly mixed under 250rpm speed under room temperature (25 DEG C), so
Be added afterwards the styrene of above-mentioned parts by weight, methyl methacrylate, methyl acrylate, butyl acrylate, total amount 65% propylene
Amide, while turn on agitator is stirred under 250rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 80 DEG C, and the step of total amount 15% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the sodium peroxydisulfate solution for adding total amount 25% carries out lotion
Polymerization reaction 50min, obtains seed emulsion；The sodium peroxydisulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the sodium peroxydisulfate solution of score 25%；
(3) the pre- cream that the step of keeping 80 DEG C of temperature in reaction kettle, residue 85% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the sodium peroxydisulfate solution of total amount 65% is at the uniform velocity added dropwise simultaneously, time for adding control is added dropwise one in 3.5h, in pre-emulsion
The acrylamide of residue 35% (is configured to the third of mass fraction 15% by the acrylamide for starting at the uniform velocity to be added dropwise residue 35% when half
Acrylamide aqueous solution is added dropwise)；Acrylamide is dripped with pre-emulsion with pre-emulsion simultaneously；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 80 DEG C, and the over cure of residue 10% is added
Acid sodium solution is added dropwise to complete in 20min, drips off subsequent continuous insulation reaction 1.5h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 60 DEG C, then stirring heat preservation 15min under 250rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.
Comparative example 3
A kind of phenylpropyl alcohol water-proof emulsion includes the raw material of following parts by weight: 25 parts of styrene, 15 parts of methyl methacrylate, third
15 parts of e pioic acid methyl ester, 45 parts of butyl acrylate, 0.6 part of acrylic acid, 2.5 parts of acrylamide, 2 parts of lauryl sodium sulfate, over cure
1.0 parts of sour sodium, 0.5 part of buffer sodium bicarbonate.
The preparation method of the phenylpropyl alcohol water-proof emulsion the following steps are included:
(1) lauryl sodium sulfate, deionized water are uniformly mixed under 250rpm speed under room temperature (25 DEG C), so
Styrene, methyl methacrylate, methyl acrylate, butyl acrylate, the acrylic acid, total amount 65% of above-mentioned parts by weight are added afterwards
Acrylamide, while turn on agitator is stirred under 250rpm speed, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 80 DEG C, and the step of total amount 15% is then added
Suddenly the pre-emulsion that (1) obtains, after temperature plateau in reaction kettle, the sodium peroxydisulfate solution for adding total amount 25% carries out lotion
Polymerization reaction 50min, obtains seed emulsion；The sodium peroxydisulfate of above-mentioned parts by weight is added in deionized water in advance, is configured to matter
Measure the sodium peroxydisulfate solution of score 25%；
(3) the pre- cream that the step of keeping 80 DEG C of temperature in reaction kettle, residue 85% is at the uniform velocity added dropwise to reaction kettle (1) obtains
Change liquid, and the sodium peroxydisulfate solution of total amount 65% is at the uniform velocity added dropwise simultaneously, time for adding control is added dropwise one in 3.5h, in pre-emulsion
The acrylamide of residue 35% (is configured to the third of mass fraction 15% by the acrylamide for starting at the uniform velocity to be added dropwise residue 35% when half
Acrylamide aqueous solution is added dropwise)；Acrylamide is dripped with pre-emulsion with pre-emulsion simultaneously；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 80 DEG C, and the over cure of residue 10% is added
Acid sodium solution is added dropwise to complete in 20min, drips off subsequent continuous insulation reaction 1.5h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 60 DEG C, then stirring heat preservation 15min under 250rpm speed,
Temperature in reaction kettle is down to room temperature, obtains the water-proof emulsion after strainer (mesh number is 300 mesh) filtering.
The phenylpropyl alcohol water-proof emulsion that 1-3 of the embodiment of the present invention is obtained is detected through profession, and all technical is as shown in table 1.
As shown in Table 1, there is no acrylamide in the raw material of 1 water-proof emulsion of comparative example, in the raw material of 2 water-proof emulsion of comparative example
There is no acrylic acid, the amount of acrylamide is excessive in the raw material of 3 water-proof emulsion of comparative example, the water-proof emulsion of obtained water-proof emulsion
Viscosity, partial size, cohesion rate etc. are higher.The cohesion rate of the application water-proof emulsion is low, consistency is moderate, in conjunction with table 2 as a result, the application
Water-proof emulsion flexibility with super strength, tensile strength and elongation at break.
Using the S400F of the commodity water-proof emulsion BASF of better performances on the market as comparative example 4, by 1-3 of the embodiment of the present invention
It is applied to 4 gained water-proof emulsion of comparative example in polymer cement waterproof paint, referring to GB/T23445-2009 " polymer cement
Water-repellent paint " in technical requirements, concrete outcome is as shown in table 2.
Table 1
| Technical indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Ion characteristic | Anionic | Anionic | Anionic | Anionic | Anionic | Anionic |
| Emulsion appearance | White emulsion | White emulsion | White emulsion | White emulsion | White emulsion | White emulsion |
| Solid content | 56% | 57% | 55% | 46% | 48% | 42% |
| Viscosity (mPa/s) | 500 | 600 | 400 | 200 | 200 | 900 |
| Partial size (μm) | 0.2 | 0.3 | 0.2 | 0.5 | 0.6 | 0.5 |
| pH | 6.8 | 6.85 | 6.8 | 7.2 | 7.5 | 6.9 |
| Glass transition temperature (DEG C) | -12 | -12 | -12 | -13 | -14 | -15 |
| Minimum film formation temperature (DEG C) | 0 | 0 | 0 | 2 | 2 | 3 |
| Cohesion rate (ppm) | 18 | 17 | 17 | 38 | 45 | 40 |
Table 2
Phenylpropyl alcohol water-proof emulsion provided by the present invention and preparation method thereof is described in detail above.It is used herein
A specific example illustrates the principle and implementation of the invention, and the above embodiments are only used to help understand
Method and its core concept of the invention.It should be pointed out that for those skilled in the art, not departing from this
, can be with several improvements and modifications are made to the present invention under the premise of inventive principle, these improvement and modification also fall into the present invention
In scope of protection of the claims.
Claims (8)
1. a kind of phenylpropyl alcohol water-proof emulsion, which is characterized in that the lotion includes the raw material of following parts by weight: 20-30 parts of styrene, first
10-18 parts of base methyl acrylate, 12-20 parts of methyl acrylate, 40-50 parts of butyl acrylate, 0.2-0.8 parts of acrylic acid, propylene
1.0-2.0 parts of amide, 1-3 parts of emulsifier, 0.5-1.5 parts of initiator, 0.2-0.8 parts of buffer.
2. phenylpropyl alcohol water-proof emulsion according to claim 1, which is characterized in that the emulsifier be lauryl sodium sulfate,
One of disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate salt, alkyl phenol polyoxyethylene ether.
3. phenylpropyl alcohol water-proof emulsion according to claim 1, which is characterized in that the initiator is sodium peroxydisulfate, persulfuric acid
One of potassium, ammonium persulfate.
4. a kind of preparation method for preparing the described in any item phenylpropyl alcohol water-proof emulsions of claim 1-3, which is characterized in that this method
The following steps are included:
(1) emulsifier, deionized water are uniformly mixed at room temperature, styrene, the methyl-prop of above-mentioned parts by weight is then added
E pioic acid methyl ester, methyl acrylate, butyl acrylate, acrylic acid, total amount 60-70% acrylamide, while turn on agitator into
Row stirring, obtains pre-emulsion；
(2) buffer and deionized water are added in a kettle, stirring is warming up to 75-85 DEG C, is then added total amount 10-15%'s
The pre-emulsion that step (1) obtains, after temperature plateau in reaction kettle, the initiator solution for adding total amount 20-30% is carried out
Emulsion polymerization 40-60min, obtains seed emulsion；
(3) 75-85 DEG C of temperature in reaction kettle is kept, the pre-emulsion that remaining step (1) obtains is added dropwise to reaction kettle, and same
When the initiator solution of total amount 55-65% is added dropwise, time for adding control starts to be added dropwise in 3-4h when half is added dropwise in pre-emulsion
Remaining acrylamide；
(4) after the completion of pre-emulsification monomer dropping, keeping the temperature in reaction kettle is 75-85 DEG C, and it is molten that remaining initiator is added
Liquid is added dropwise to complete in 15-30min, drips off subsequent continuous insulation reaction 1-2h；
(5) after the completion of keeping the temperature, the temperature in reaction kettle is down to 50-60 DEG C, then stirring heat preservation 10-20min, it will be in reaction kettle
Temperature be down to room temperature, the water-proof emulsion is obtained after strainer filtering.
5. the preparation method of phenylpropyl alcohol water-proof emulsion according to claim 4, which is characterized in that in step (3), the third of dropwise addition
Acrylamide is the acrylamide aqueous solution of mass fraction 10-20%.
6. the preparation method of phenylpropyl alcohol water-proof emulsion according to claim 4, which is characterized in that in step (3), acrylamide
The time difference being added dropwise with pre-emulsion is within ± 5min.
7. the preparation method of phenylpropyl alcohol water-proof emulsion according to claim 4, which is characterized in that in step (5), the mesh of strainer
Number is 300 mesh.
8. the preparation method of phenylpropyl alcohol water-proof emulsion according to claim 4, which is characterized in that the dropwise addition in above-mentioned steps is equal
To be at the uniform velocity added dropwise, the speed of stirring is 200-260rpm.
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