CN109651551A - A kind of dope for inner wall of architecture acrylic acid ester emulsion and preparation method thereof and coating - Google Patents
A kind of dope for inner wall of architecture acrylic acid ester emulsion and preparation method thereof and coating Download PDFInfo
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- CN109651551A CN109651551A CN201811587993.1A CN201811587993A CN109651551A CN 109651551 A CN109651551 A CN 109651551A CN 201811587993 A CN201811587993 A CN 201811587993A CN 109651551 A CN109651551 A CN 109651551A
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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
- C08F212/00—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 an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- 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
- C09D125/00—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 an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/08—Copolymers of styrene
- C09D125/14—Copolymers of styrene with unsaturated esters
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Abstract
The present invention proposes a kind of dope for inner wall of architecture acrylic acid ester emulsion and preparation method thereof and coating, belong to building coating technical field, the lotion is by including that following parts by weight raw material is prepared: 6-20 parts of butyl acrylate, 15.5-26 parts of styrene, 6-20 parts of Isooctyl acrylate monomer, 0.11-0.55 parts of self-cross linking monomer, 0.15-1.3 parts of acrylamide, 0.2-3 parts of carboxylic monomer, 0.015-0.12 parts of silane coupling agent, 0.21-0.81 parts of response type anion emulsifier, 0.21-0.81 parts of response type nonionic emulsifier, 0.1-2 parts of polyethyleneimine, 0.1-0.2 parts of adipic acid dihydrazide, 0.12-0.45 parts of persulfate, 0.2-2 parts of ammonium hydroxide, 30-60 parts of water.Lotion of the present invention is mainly used for dope for inner wall of architecture, can have lower MFFT without adding coalescing agent in lotion, and with its coating obtained with excellent scrub resistance and freeze-thaw stability, VOC content is low, and the feature of environmental protection is good.
Description
Technical field
The present invention relates to a kind of building coating technical field more particularly to a kind of dope for inner wall of architecture acrylic acid ester emulsions
And preparation method thereof and coating.
Background technique
Water-and acrylate lotion is since its feature of environmental protection is good, at low cost, performance is excellent, it has also become dope for inner wall of architecture resin
Mainstream.For dope for inner wall of architecture, scrub resistance, freeze-thaw stability etc. are its important performance indicators, and influence this
A little most important factors of index are selected lotions.Conventional method is often added in lotion to improve the freeze-thaw stability of coating
The higher nonionic surfactant of ethoxy radix, but its scrub resistance can be reduced.
In addition, the minimum film formation temperature (MFFT) of coating lotion is also to consider the important indicator of emulsion property, in order to drop
The MFFT of low lotion can generally add coalescing agent in lotion.However, coalescing agent use not only will increase formula at
This, and the content of volatile organic compounds in coating (VOC) can be improved.Therefore, a kind of ring with lower MFFT is developed
Guarantor's type lotion, while coating made from it has that scrub resistance is good, freeze-thaw stability is good etc. has great importance.
Summary of the invention
The present invention is directed to propose a kind of dope for inner wall of architecture acrylic acid ester emulsion and preparation method thereof and coating, in lotion
There can be lower MFFT without adding coalescing agent, and have excellent scrub resistance and freeze thawing steady with its coating obtained
Qualitative, VOC content is low, and the feature of environmental protection is good.
The present invention proposes a kind of dope for inner wall of architecture acrylic acid ester emulsion, by include following parts by weight raw material preparation and
At:
6-20 parts of butyl acrylate, 15.5-26 parts of styrene, 6-20 parts of Isooctyl acrylate monomer, self-cross linking monomer 0.11-
0.55 part, 0.15-1.3 parts of acrylamide, 0.2-3 parts of carboxylic monomer, 0.015-0.12 parts of silane coupling agent, response type anion
0.21-0.81 parts of emulsifier, 0.21-0.81 parts of response type nonionic emulsifier, 0.1-2 parts of polyethyleneimine, two acyl of hexanedioic acid
0.1-0.2 parts of hydrazine, 0.12-0.45 parts of persulfate, 0.2-2 parts of ammonium hydroxide, 30-60 parts of water.
Further, the self-cross linking monomer is Diacetone Acrylamide, one in acetoacetoxyethyl methacrylate
Kind is two or more.
Further, the silane coupling agent is vinyltrimethoxysilane, γ-methacryloxypropyl front three
It is one or more kinds of in oxysilane.
Further, the carboxylic monomer be acrylic acid, methacrylic acid, it is one or more kinds of in itaconic acid；It is described
Polyethyleneimine be Lupasol G20, Lupasol G35, it is one or more kinds of in Lupasol G100.
Further, the response type anion emulsifier is at least one of SR-10 and SR-20；The reaction
Type nonionic emulsifier is one or more kinds of in ER-10 and ER-20.
Further, the persulfate is one or more kinds of in ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate.
The present invention also proposes the preparation method of above-mentioned acrylic acid ester emulsion, comprising the following steps:
A) pre-emulsification I: under normal temperature and pressure, 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response types are non-
Ionic emulsifying agent and 20-30 parts of water mix in emulsion tank, then stirring sequentially adds 5-15 parts of butyl acrylates, and 15-23 parts
Styrene, 5-15 parts of Isooctyl acrylate monomers, 0.1-0.5 parts of self-cross linking monomers, 0.1-2 parts of carboxylic monomers, 0.1-1 parts of acryloyls
Amine, 0.01-0.1 parts of silane coupling agents, stirring obtain pre-emulsion I；
B) polymerize I: in a kettle be added 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response types it is non-from
Sub- emulsifier and 4.5-15 parts of water are warming up to 80-87 DEG C, after 0.01-0.1 parts of persulfate reactions are added, start that over cure is added dropwise
Acid salt solution and step a) gained pre-emulsion I, keep the temperature after completion of dropwise addition；
C) pre-emulsification II: under normal temperature and pressure, by remaining response type anion emulsifier, response type nonionic emulsifier and
3-8 parts of water mix in emulsion tank, and then stirring sequentially adds remaining butyl acrylate, styrene, Isooctyl acrylate monomer,
Self-cross linking monomer, carboxylic monomer, acrylamide, silane coupling agent, stirring obtain pre-emulsion II；
D) it polymerize II: after polymerization I heat preservation, starts that pre-emulsion II obtained by persulfate solution and step c) is added dropwise,
It is kept the temperature after completion of dropwise addition；
E) tailing material after post-processing: after polymerization II heat preservation, it is cooled to 50-70 DEG C, is post-processed, is then successively added
Enter ammonium hydroxide, adipic acid dihydrazide, polyethyleneimine, after insulated and stirred, filtering and discharging.
Further, in step b), persulfate solution is made by 0.1-0.3 parts of persulfate and 2-5 part water；It is added dropwise
80-87 DEG C of temperature, time for adding 2-4h；Soaking time 1h；
Further, in step d), persulfate solution is made by 0.01-0.05 parts of persulfate and 0.5-2 part water；
80-87 DEG C of dropping temperature, time for adding 20-60min, soaking time 1h.
Further, in step e), post-processing specifically: when temperature is 50-70 DEG C, it is molten that tert-butyl hydroperoxide is added dropwise
Liquid and solution of sodium bisulfite, time for adding 40min after being added dropwise to complete, keep the temperature 20min；
Wherein, tert-butyl hydroperoxide solution is made by 0.01-0.1 parts of tert-butyl hydroperoxide and 0.5-1.5 parts of water；It is sub-
Sodium bisulfate is made by 0.01-0.1 parts of sodium hydrogensulfites and 0.5-1.5 parts of water.
Further, in step e), ammonium hydroxide is dripped, adipic acid dihydrazide, after polyethyleneimine, also dropwise addition defoaming agent
0.005-0.015 parts, 0.1-0.2 parts of fungicide；The time of insulated and stirred is 0.5-1h.
The present invention also proposes a kind of dope for inner wall of architecture, includes lotion in raw material, and the lotion is above-mentioned acrylate cream
Liquid.
Lotion proposed by the invention and preparation method thereof has the advantage that
A kind of dope for inner wall of architecture acrylic acid ester emulsion proposed by the present invention, with butyl acrylate, Isooctyl acrylate monomer
Deng based on, the components synergistic effect such as addition carboxylic monomer, silane coupling agent, polyethyleneimine, adipic acid dihydrazide, so that lotion
There can be lower MFFT without adding coalescing agent, and have excellent scrub resistance and freeze thawing steady with its coating obtained
Qualitative, VOC content is low, and the feature of environmental protection is good.
Carboxylic monomer is added in lotion, carboxylic monomer can provide steric hindrance after neutralizing for latex particle, effectively protect
Its freeze-thaw stability is demonstrate,proved；Simultaneously as the collective effect of carboxylic monomer and polyethyleneimine, can greatly improve the friendship of film
The interaction for joining each component in density and coating, so that scrub resistance be made to be obviously improved；The polarity and silane of carboxylic monomer
The bridge joint of coupling agent acts on, and the cohesive force between lotion and powder can be improved.In addition, self-cross linking monomer and adipic acid dihydrazide it
Between collective effect, improve the scrub resistance of lotion；Self-cross linking monomer can also be solved since the glass transition temperature (Tg) of lotion is lower
Caused by paint film intensity deficiency problem, further improve scrub resistance；Reactive emulsifier is improving lotion freeze-thaw stability
While property, it ensure that the hydrophobicity of paint film, reduce emulsifier negative effect caused by scrub resistance.
Technique, packet is added dropwise using segmentation in the preparation method of dope for inner wall of architecture acrylic acid ester emulsion proposed by the present invention
It includes first segment pre-emulsification I, polymerization I and second segment pre-emulsification II, polymerize II, it is particular kind of due to being added in every segment process
Monomer, and the additive amount of monomer is also different, intermediate products Tg obtained by two-stage process is different and relatively low, gained intermediate products
Lower second segment process of Tg can wrap up the resulting intermediate products of the first slightly higher segment process of Tg, to further decrease most
The MFFT of gained lotion eventually.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
The embodiment of the present invention proposes a kind of dope for inner wall of architecture acrylic acid ester emulsion, by including following parts by weight raw material
It is prepared: 6-20 parts of butyl acrylate, 15.5-26 parts of styrene, 6-20 parts of Isooctyl acrylate monomer, self-cross linking monomer 0.11-
0.55 part, 0.15-1.3 parts of acrylamide, 0.2-3 parts of carboxylic monomer, 0.015-0.12 parts of silane coupling agent, response type anion
0.21-0.81 parts of emulsifier, 0.21-0.81 parts of response type nonionic emulsifier, 0.1-2 parts of polyethyleneimine, two acyl of hexanedioic acid
0.1-0.2 parts of hydrazine, 0.12-0.45 parts of persulfate, 0.2-2 parts of ammonium hydroxide, 30-60 parts of water.
For dope for inner wall of architecture, scrub resistance, freeze-thaw stability etc. are its important performance indicators, and influence this
A little most important factors of index are selected lotions.Conventional method is often added in lotion to improve the freeze-thaw stability of coating
The higher nonionic surfactant of ethoxy radix, but its scrub resistance can be reduced.The MFFT of coating lotion is also to consider cream
Fluidity can important indicator, lower minimum film formation temperature (MFFT) lotion in order to obtain, using improving coalescing agent additive amount, but
It often will increase cost and improve the VOC content of coating, the feature of environmental protection is low.
A kind of dope for inner wall of architecture acrylic acid ester emulsion that the embodiment of the present invention proposes, with butyl acrylate, acrylic acid
Based on different monooctyl ester etc., addition self-cross linking monomer, carboxylic monomer, silane coupling agent and response type anion emulsifier, response type
The components collective effect such as nonionic emulsifier, polyethyleneimine, adipic acid dihydrazide, so that without adding coalescing agent in lotion
There can be lower MFFT, and there is excellent scrub resistance and freeze-thaw stability with its coating obtained, VOC content is low,
The feature of environmental protection is good.
In the present invention, selected specific components type and its corresponding additive amount, collective effect between each component, so that most
The Tg of the lotion of institute is lower eventually, realizes without adding coalescing agent, that is, may make it is final made from lotion MFFT it is lower.Also,
The effect between effect and self-cross linking monomer and adipic acid dihydrazide between carboxylic monomer and polyethyleneimine, for improving
The scrub resistance of lotion has important influence；Carboxylic monomer can provide steric hindrance after neutralizing for latex particle, effectively
It ensure that its freeze-thaw stability.In an embodiment of the present invention, the self-cross linking monomer is Diacetone Acrylamide (DAAM), second
It is one or more kinds of in ethyl acetoacetic acid amino ethyl methacrylate (AAEM).The addition of self-cross linking monomer, solves due to lotion
Glass transition temperature (Tg) it is lower caused by paint film intensity deficiency problem, be conducive to improve lotion scrub resistance.And selfing receipts or other documents in duplicate
Collective effect between body and adipic acid dihydrazide improves scrub resistance.
In an embodiment of the present invention, the silane coupling agent is vinyltrimethoxysilane, γ-methacryloxypropyl
It is one or more kinds of in base propyl trimethoxy silicane.After silane coupling agent hydrolysis the silanol groups that are formed can in coating
Powder (such as titanium dioxide, coarse whiting) interaction form covalent bond, improve the intensity of coating, while silanol groups can also be with painting
Substrate to be coated in material, such as wall form covalent bond, improve adhesive force, further increase scrub resistance.
In an embodiment of the present invention, the carboxylic monomer be acrylic acid, methacrylic acid, it is one or two kinds of in itaconic acid
More than.The addition of carboxylic monomer, provides steric hindrance after neutralization for latex particle, is effectively guaranteed its freeze-thaw stability.
In an embodiment of the present invention, the polyethyleneimine is Lupasol G20, Lupasol G35, Lupasol
It is one or more kinds of in G100.Wherein Lupasol G20, Lupasol G35, Lupasol G100 are that BASF AG is raw
It produces.The collective effect of carboxylic monomer and polyethyleneimine can greatly improve each component in the crosslink density and coating of film
Interaction force, so that scrub resistance be made to be obviously improved.
In an embodiment of the present invention, the response type anion emulsifier is one or two kinds of in SR-10 and SR-20
More than.The SR-10 and SR-20 is the production of Japanese Ai Dike (ADEKA) company.
In an embodiment of the present invention, the response type nonionic emulsifier is one or two kinds of in ER-10 and ER-20
More than.ER-10 and ER-20 is Japanese ADEKA company production.Select response type anion emulsifier and response type nonionic Emulsion
Agent ensure that the hydrophobicity of paint film, reduce emulsifier and cause to scrub resistance while improving lotion freeze-thaw stability
Negative effect.
In an embodiment of the present invention, the persulfate is a kind of in ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate
Or it is two or more.
It may be noted that raw material selected in the embodiment of the present invention, is not such as specifically described it, i.e., comes to raw material
Source does not have special limitation, using commercial goods well known in the art.
The embodiment of the present invention proposes a kind of preparation method of above-mentioned dope for inner wall of architecture acrylic acid ester emulsion, including following
Step:
A) pre-emulsification I: under normal temperature and pressure, 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response types are non-
Ionic emulsifying agent and 20-30 parts of water mix in emulsion tank, then stirring sequentially adds 5-15 parts of butyl acrylates, and 15-23 parts
Styrene, 5-15 parts of Isooctyl acrylate monomers, 0.1-0.5 parts of self-cross linking monomers, 0.1-2 parts of carboxylic monomers, 0.1-1 parts of acryloyls
Amine, 0.01-0.1 parts of silane coupling agents, stirring obtain pre-emulsion I；
B) polymerize I: in a kettle be added 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response types it is non-from
Sub- emulsifier and 4.5-15 parts of water are warming up to 80-87 DEG C, after 0.01-0.1 parts of persulfate reactions are added, start that over cure is added dropwise
Acid salt solution and step a) gained pre-emulsion I, keep the temperature after completion of dropwise addition；
C) pre-emulsification II: under normal temperature and pressure, by remaining response type anion emulsifier, response type nonionic emulsifier and
3-8 parts of water mix in emulsion tank, and then stirring sequentially adds remaining butyl acrylate, styrene, Isooctyl acrylate monomer,
Self-cross linking monomer, carboxylic monomer, acrylamide, silane coupling agent, stirring obtain pre-emulsion II；
D) it polymerize II: after polymerization I heat preservation, starts that pre-emulsion II obtained by persulfate solution and step c) is added dropwise,
It is kept the temperature after completion of dropwise addition；
E) tailing material after post-processing: after polymerization II heat preservation, it is cooled to 50-70 DEG C, is post-processed, is then successively added
Enter ammonium hydroxide, adipic acid dihydrazide, polyethyleneimine, after insulated and stirred, filtering and discharging.
The preparation method of dope for inner wall of architecture acrylic acid ester emulsion proposed by the present invention is divided to two sections of progress, first stage
Including pre-emulsification I and polymerization I, specially first by the butyl acrylate of specific quantity, styrene, Isooctyl acrylate monomer and self-crosslinking
Pre-emulsion I is obtained after the pre-emulsifications such as monomer carries out polymerization I again；Second stage includes pre-emulsification II and polymerization II, will specially be remained
Pre-emulsion II is obtained after the pre-emulsifications such as remaining butyl acrylate, styrene, Isooctyl acrylate monomer and self-cross linking monomer, is then existed
After carrying out polymerization II reaction on the basis of polymerization I to it, post-processing tailing material discharging obtains final lotion.
The present invention uses two sections of dropwise addition techniques compared with the existing technology, and particular kind of list is added in every segment process
The additive amount of body, monomer is also different, cause the glass transition temperature (Tg) of gained intermediate products after the completion of every segment process different and
Lower, first segment Tg is about between -10~10 DEG C, and second segment Tg is about between -40~-10 DEG C, and gained intermediate products Tg is more
The second low segment process can wrap up the resulting intermediate products of the first slightly higher segment process of Tg, to further decrease final institute
Obtain the MFFT of lotion.
Also, in pre-emulsification I, part propylene acid butyl ester is successively added dropwise, the stabilization of pre-emulsion can be improved in styrene etc.
Property；In pre-emulsification II, remaining butyl acrylate, styrene etc. is successively added dropwise, final gained emulsion intercalation method can be improved.
Further, in step b), 80-87 DEG C of dropping temperature, time for adding 2-4h；Soaking time 1h；In step d), drop
80-87 DEG C of heating degree, time for adding 20-60min, soaking time 1h.
Further, in the step e), post-processing includes: that tert-butyl hydroperoxide is added dropwise when temperature is 50-70 DEG C
Solution and solution of sodium bisulfite, time for adding 40min after being added dropwise to complete, keep the temperature 20min；
Wherein tert-butyl hydroperoxide solution is made by 0.01-0.1 parts of tert-butyl hydroperoxide and 0.5-1.5 parts of water；It is sub-
Sodium bisulfate is made by 0.01-0.1 parts of sodium hydrogensulfites and 0.5-1.5 parts of water.
Further, in the step e), ammonium hydroxide is dripped, after polyethyleneimine, defoaming is also added dropwise in adipic acid dihydrazide
0.005-0.015 parts of agent, 0.1-0.2 parts of fungicide；The time of insulated and stirred is 0.5-1h.
Further, in the step e), the parts by weight point of the ammonium hydroxide of addition, adipic acid dihydrazide, polyethyleneimine
Wei not be 0.2-2 parts of ammonium hydroxide, 0.1-0.2 parts of adipic acid dihydrazide, 0.1-2 parts of polyethyleneimine.
Further, the step a) and c) in mixing plant be high speed agitator, step b) and d) in reaction kettle
For the four-hole boiling flask for being equipped with reflux condensing tube, agitating paddle, thermometer.
The present invention also proposes a kind of dope for inner wall of architecture, includes lotion in raw material, and the lotion is any of the above-described acrylic acid
Ester lotion.
Technical solution of the present invention is described in detail combined with specific embodiments below.
Embodiment 1
A kind of dope for inner wall of architecture acrylic acid ester emulsion, by including prepared by following parts by weight raw material:
The preparation method of above-mentioned dope for inner wall of architecture acrylic acid ester emulsion, comprising the following steps:
A) pre-emulsification I: under normal temperature and pressure, by 0.3 part of response type anion emulsifier, 0.17 part of response type non-ionic emulsifier
Agent and 23.4 parts of water mix in emulsion tank, are sufficiently stirred and are uniformly dissolved, and then sequentially add 10 parts of butyl acrylates, and 21.4 parts
Styrene, 9.5 parts of Isooctyl acrylate monomers, 0.22 part of self-cross linking monomer, 1.25 parts of carboxylic monomers, 0.59 part of acrylamide, 0.04
Part silane coupling agent, is sufficiently stirred and is uniformly dissolved, that is, pre-emulsion I is made；
B) it polymerize I: 0.34 part of response type anion emulsifier, 0.3 part of response type nonionic emulsifier is added in reaction kettle
With 9.8 parts of water, be warming up to 85 DEG C, be added 0.07 part of persulfate, start after 5min pre-emulsion I obtained by a dropping step a) and by
The persulfate solution that 0.2 part of persulfate and 4 parts of water are made into, 85 DEG C of dropping temperature, time for adding 2.5h, after completion of dropwise addition
Keep the temperature 1h, 85 DEG C of holding temperature；
C) pre-emulsification II: under normal temperature and pressure, by remaining response type anion emulsifier, response type nonionic emulsifier and
5.4 parts of water mix in emulsion tank, are sufficiently stirred and are uniformly dissolved, and then sequentially add remaining butyl acrylate, styrene, and third
The different monooctyl ester of olefin(e) acid, self-cross linking monomer, carboxylic monomer, acrylamide, silane coupling agent are sufficiently stirred and are uniformly dissolved, that is, are made pre-
Emulsion II；
D) it polymerize II: after polymerization I heat preservation, pre-emulsion II obtained by beginning a dropping step c) and the over cure by 0.03 part
The persulfate solution that hydrochlorate and 0.8 part of water are made into, 85 DEG C of dropping temperature, time for adding 30min keeps the temperature 1h after completion of dropwise addition,
85 DEG C of holding temperature；
E) post-process: after polymerization II heat preservation, being cooled to 70 DEG C, start to be added dropwise by 0.06 part of tert-butyl hydroperoxide and
The tert-butyl hydroperoxide solution that 0.8 part of water is made into and the sodium hydrogensulfite being made by 0.05 part of sodium hydrogensulfite and 0.8 part of water
Solution, time for adding 40min drip off heat preservation 20min；
Tailing material: being cooled to 50 DEG C, sequentially adds ammonium hydroxide, adipic acid dihydrazide, polyethyleneimine, and 0.01 part of defoaming agent,
0.15 part of fungicide；
Discharging: maintaining the temperature at 50 DEG C, stirs filtering and discharging after 0.5h.
Embodiment 2
A kind of dope for inner wall of architecture acrylic acid ester emulsion, by including prepared by following parts by weight raw material:
The preparation method of above-mentioned dope for inner wall of architecture acrylic acid ester emulsion, with embodiment 1.
Embodiment 3
A kind of dope for inner wall of architecture acrylic acid ester emulsion, by including prepared by following parts by weight raw material:
The preparation method of above-mentioned dope for inner wall of architecture acrylic acid ester emulsion, with embodiment 1.
Embodiment 4
A kind of dope for inner wall of architecture acrylic acid ester emulsion, by including prepared by following parts by weight raw material:
| Raw material | Parts by weight |
| Butyl acrylate | 13 |
| Styrene | 22 |
| Isooctyl acrylate monomer | 12 |
| Acrylamide | 0.6 |
| Self-cross linking monomer: acetoacetoxyethyl methacrylate | 0.35 |
| Carboxylic monomer: itaconic acid, acrylic acid | 2 |
| Silane coupling agent: vinyltrimethoxysilane | 0.07 |
| Response type anion emulsifier: SR-20 | 0.66 |
| Response type nonionic emulsifier: ER-10 | 0.6 |
| Persulfate: sodium peroxydisulfate | 0.3 |
| Polyethyleneimine: Lupasol G100, Lupasol G35 | 2 |
| Adipic acid dihydrazide | 0.2 |
| Ammonium hydroxide | 1 |
| Water | 45 |
The preparation method of above-mentioned dope for inner wall of architecture acrylic acid ester emulsion, with embodiment 1.
Comparative example 1
The present embodiment is to prepare acrylic acid ester emulsion using traditional preparation method.
Raw material and its corresponding parts by weight are the same as embodiment 1.
The preparation method of the dope for inner wall of architecture acrylic acid ester emulsion, comprising the following steps:
A) pre-emulsification: under normal temperature and pressure, by 0.325 part of response type anion emulsifier, 0.2 part of nonionic part emulsifier and
28.8 parts of water mix in emulsion tank, are sufficiently stirred and are uniformly dissolved, and then sequentially add 12.4 parts of butyl acrylates, 22.8 parts of benzene
Ethylene, 11.9 parts of Isooctyl acrylate monomers, 1.84 parts of carboxylic monomers, 0.71 part of acrylamide, 0.05 part of vinyl trimethoxy silicon
Alkane is sufficiently stirred and is uniformly dissolved, that is, pre-emulsion is made；
B) it polymerize: 0.32 part of anion emulsifier, 0.3 part of nonionic emulsifier and 9.8 parts of water, heating is added in reaction kettle
To 85 DEG C, 0.07 part of persulfate is added, pre-emulsion obtained by beginning a dropping step a) and the persulfuric acid by 0.23 part after 5min
The persulfate solution that salt and 4.8 parts of water are made into, keeps the temperature 1h, heat preservation temperature by 85 DEG C of dropping temperature, time for adding 4h after completion of dropwise addition
85 DEG C of degree；
C) after post-processing then tailing material discharges, with embodiment 1.
The basic index of 1 gained lotion of above-described embodiment 1-4 and comparative example is shown in Table 1.
The basic index of 1 gained lotion of 1 embodiment 1-4 of table and comparative example
It can be obtained by table 1, the MFFT of lotion obtained is down to 0.1 DEG C through the invention, and uses cream made from conventional method
Liquid MFFT is 10.3 DEG C, hence it is evident that higher than the MFFT of lotion of the present invention.
Lotion made from embodiment 1-4, comparative example 1-3 is used for dope for inner wall of architecture, wherein in coating composition, removes lotion
In addition, it is selected from conventional coating preparation component, is specifically shown in Table 2.
The formula of 2 coating of table
| Material name | Dosage | Remarks |
| Water | 41.17 | |
| SN-5040 | 0.45 | Dispersing agent |
| LCN-407 | 0.2 | Wetting agent |
| NXZ | 0.3 | Defoaming agent |
| R706 | 7.5 | Titanium dioxide |
| DB80 | 10 | Calcined kaolin |
| CC800 | 22.5 | Coarse whiting |
| Talcum powder | 5 | Talcum powder |
| 250HBR | 0.63 | Cellulose |
| Ammonium hydroxide | 0.1 | PH adjusting agent |
| Texanol | 1 | Coalescing agent |
| EG | 1 | Antifreezing agent |
| TT935 | 0.05 | Alkali swollen thickener |
| GT50 | 0.1 | Fungicide |
| Lotion | 10 | Embodiment 1 is made |
| Total amount | 100 |
Detection method is carried out according to following standard:
Scrub resistance: it is executed by GB/T 9266-2009；Freeze-thaw stability: it is executed by the A method in GB/T 9268-2008；
VOC content: it is executed by GB 18582-2008.Test result is shown in Table 3.
The performance detection of coating obtained by 3 embodiment 1-4 of table and 1 lotion of comparative example
There is excellent scrub resistance and freeze-thaw stability using coating made from lotion of the invention.Simultaneously as newborn
Liquid has lower MFFT, and coating VOC content obtained is lower.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of dope for inner wall of architecture acrylic acid ester emulsion, by including that following parts by weight raw material is prepared:
6-20 parts of butyl acrylate, 15.5-26 parts of styrene, 6-20 parts of Isooctyl acrylate monomer, self-cross linking monomer 0.11-0.55
Part, 0.15-1.3 parts of acrylamide, 0.2-3 parts of carboxylic monomer, 0.015-0.12 parts of silane coupling agent, response type is anionic emulsifying
0.21-0.81 parts of agent, 0.21-0.81 parts of response type nonionic emulsifier, 0.1-2 parts of polyethyleneimine, adipic acid dihydrazide
0.1-0.2 parts, 0.12-0.45 parts of persulfate, 0.2-2 parts of ammonium hydroxide, 30-60 parts of water.
2. acrylic acid ester emulsion according to claim 1, which is characterized in that the self-cross linking monomer is diacetone acrylamide acyl
It is one or more kinds of in amine, acetoacetoxyethyl methacrylate.
3. acrylic acid ester emulsion according to claim 1, which is characterized in that the silane coupling agent is vinyl trimethoxy
It is one or more kinds of in base silane, γ-methacryloxypropyl trimethoxy silane.
4. acrylic acid ester emulsion according to claim 1, which is characterized in that the carboxylic monomer is acrylic acid, methyl-prop
It is one or more kinds of in olefin(e) acid, itaconic acid；The polyethyleneimine is Lupasol G20, Lupasol G35, Lupasol
It is one or more kinds of in G100.
5. acrylic acid ester emulsion according to claim 1, which is characterized in that the response type anion emulsifier is
At least one of SR-10 and SR-20；The response type nonionic emulsifier be ER-10 and ER-20 in one or two with
On.
6. acrylic acid ester emulsion according to claim 1, which is characterized in that the persulfate is ammonium persulfate, mistake
It is one or more kinds of in potassium sulfate and sodium peroxydisulfate.
7. the preparation method of acrylic acid ester emulsion described in any one of claims 1-6, which comprises the following steps:
A) pre-emulsification I: under normal temperature and pressure, by 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response type nonionics
Emulsifier and 20-30 parts of water mix in emulsion tank, then stirring sequentially adds 5-15 parts of butyl acrylates, 15-23 parts of benzene second
Alkene, 5-15 parts of Isooctyl acrylate monomers, 0.1-0.5 parts of self-cross linking monomers, 0.1-2 parts of carboxylic monomers, 0.1-1 parts of acrylamides,
0.01-0.1 parts of silane coupling agents, stirring, obtain pre-emulsion I；
B) it polymerize I: 0.1-0.4 parts of response type anion emulsifiers, 0.1-0.4 parts of response type nonionic Emulsions is added in a kettle
Agent and 4.5-15 parts of water are warming up to 80-87 DEG C, after 0.01-0.1 parts of persulfate reactions are added, start that persulfate is added dropwise
Solution and step a) gained pre-emulsion I, keep the temperature after completion of dropwise addition；
C) pre-emulsification II: under normal temperature and pressure, by remaining response type anion emulsifier, response type nonionic emulsifier and 3-8
Part water mixes in emulsion tank, stirs, and then sequentially adds remaining butyl acrylate, styrene, Isooctyl acrylate monomer, selfing
Receipts or other documents in duplicate body, carboxylic monomer, acrylamide, silane coupling agent, stirring obtain pre-emulsion II；
D) it polymerize II: after polymerization I heat preservation, starts that pre-emulsion II obtained by persulfate solution and step c) is added dropwise, be added dropwise
After keep the temperature；
E) tailing material after post-processing: after polymerization II heat preservation, it is cooled to 50-70 DEG C, is post-processed, ammonia is then sequentially added
Water, adipic acid dihydrazide, polyethyleneimine, after insulated and stirred, filtering and discharging.
8. the preparation method of acrylic acid ester emulsion according to claim 7, which is characterized in that
In step b), persulfate solution is made by 0.1-0.3 parts of persulfate and 2-5 part water；80-87 DEG C of dropping temperature,
Time for adding 2-4h；Soaking time 1h；
In step d), persulfate solution is made by 0.01-0.05 parts of persulfate and 0.5-2 part water；Dropping temperature 80-87
DEG C, time for adding 20-60min, soaking time 1h.
9. the preparation method of acrylic acid ester emulsion according to claim 7, which is characterized in that
In step e), post-processing specifically: when temperature is 50-70 DEG C, tert-butyl hydroperoxide solution and bisulfite is added dropwise
Sodium solution, time for adding 40min after being added dropwise to complete, keep the temperature 20min；
Wherein, tert-butyl hydroperoxide solution is made by 0.01-0.1 parts of tert-butyl hydroperoxide and 0.5-1.5 parts of water；Sulfurous acid
Hydrogen sodium solution is made by 0.01-0.1 parts of sodium hydrogensulfites and 0.5-1.5 parts of water；
In step e), ammonium hydroxide is dripped, adipic acid dihydrazide after polyethyleneimine, is also added dropwise defoaming agent 0.005-0.015 parts,
0.1-0.2 parts of fungicide；The time of insulated and stirred is 0.5-1h.
It include lotion in raw material 10. a kind of dope for inner wall of architecture, which is characterized in that the lotion is any one of claim 1-6
The acrylic acid ester emulsion.
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| CN112250784B (en) * | 2020-09-23 | 2022-04-05 | 泰州东方特种化工有限公司 | Emulsion for latex mattress and preparation method thereof |
| CN112358562A (en) * | 2020-10-29 | 2021-02-12 | 江苏日出化工有限公司 | High-viscosity transparent waterproof emulsion and preparation method thereof |
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| CN115109199A (en) * | 2022-05-31 | 2022-09-27 | 镇江永义新材料技术有限责任公司 | Organosilicon modified styrene acrylate self-emulsifying emulsion, preparation method and antifouling high-color-fastness water-based paint prepared from emulsion |
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