CN102827320A - Styrene acrylic emulsion for interior wall coating material, and preparation method thereof - Google Patents
Styrene acrylic emulsion for interior wall coating material, and preparation method thereof Download PDFInfo
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Abstract
The invention provides a styrene acrylic emulsion for interior wall coating material, and a preparation method of the styrene acrylic emulsion; the preparation method comprises the following steps of: (1) mixing water, composite emulsifying agent, acrylate monomer and functional monomer, and emulsifying to obtain pre-emulsified liquid A; (2) adding reactive organic silicon into the pre-emulsified liquid A, and emulsifying to obtain pre-emulsified liquid B; (3) adding mixture of water, composite emulsifying agent, methyl alcohol and sodium bicarbonate into the pre-emulsified liquid A obtained in the step (1), and adding initiator for reaction to obtain seed emulsion C; (4) adding the pre-emulsified liquid B into the seed emulsion C obtained in the step (3), and simultaneously adding initiator water solution into the mixed solution; carrying out heat preservation after dripping, and cooling the emulsion; and (5) removing residual monomer, and adjusting the pH to be 7-8 to obtain the styrene acrylic emulsion for the interior wall coating material. The styrene acrylic emulsion can be used for preparing the interior wall coating material, and is less in adding quantity and better in scrub resistance than that of other emulsions, thus reducing the cost of coating and saving resources.
Description
Technical field
The present invention relates to a kind of preparation method of benzene emulsion, relate in particular to the preparation method of a kind of interior wall coating with benzene emulsion.
Background technology
The benzene emulsion cost performance is high, has good resistance to soiling, scrub resistance, strong adhesion, characteristics such as good film-forming property.Aspect interior wall coating, Design of Coatings Formulation person is to scrub resistance, stain resistance, the cohesive strength of coating and farthest to reduce formulation cost be the topmost requirement to benzene emulsion.
Be applied to the benzene emulsion of interior wall coating in the market, when needing addition big, just can make coating have scrub resistance preferably, cost performance is lower, can not satisfy needs of people.
Summary of the invention
The object of the present invention is to provide a kind of interior wall coating with benzene emulsion and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
Interior wall coating of the present invention comprises the steps: with the preparation method of benzene emulsion
(1) deionized water, compound emulsifying agent, acrylate monomer and function monomer are mixed, emulsification 20～40 minutes obtains pre-emulsion A.
The parts by weight of each component are following:
Water 15-20 part, compound emulsifying agent 0.4-1.0 part, mix monomer 45-50 part, function monomer 0.5-2 part;
Said compound emulsifying agent is made up of anionic emulsifier and nonionic emulsifying agent, and the weight ratio of nonionic emulsifying agent and anionic emulsifier is 1: 1～1:1.5;
Said mix monomer is made up of vinylbenzene, propenoate and Acrylic Acid Monomer;
Said propenoate is selected from more than one in TEB 3K, Bing Xisuandingzhi or the Isooctyl acrylate monomer;
Said Acrylic Acid Monomer is methylacrylic acid or vinylformic acid, preferable methyl vinylformic acid;
Each components by weight is a vinylbenzene: propenoate: methylacrylic acid=(20～27): (21～28): 1;
Said function monomer is the acrylamide solution of weight concentration 45～55%;
(2) the response type organosilicon is added among the pre-emulsion A, emulsification 10-20min obtains pre-emulsion B;
The parts by weight of component are following:
Response type organosilicon 0.5-1 part, pre-emulsion A55 ~ 66 part;
Said response type an organosilane monomer is γ-methacryloxypropyl trimethoxy silane or vinyltriethoxysilane;
(3) with the mixture of water, compound emulsifying agent, methyl alcohol and sodium hydrogencarbonate, in the nitrogen atmosphere, 150-200r/min stirs down; Add the described preparatory emulsification latex A of step (1) under the 75-80 ℃ of temperature, stir 5 ~ 10min, add initiator; Reaction 10～20min obtains to make seed emulsion C;
The parts by weight of each component are following:
Water 20-30 part, compound emulsifying agent 0.5-0.7 part, methyl alcohol 1-2 part, sodium hydrogencarbonate 0.05-0.1 part, the emulsification emulsion is 2.9 ~ 3.3 parts in advance, initiator 0.1-0.2 part;
Said compound emulsifying agent is made up of anionic emulsifier and nonionic emulsifying agent, and the weight ratio of nonionic emulsifying agent and anionic emulsifier is 1: 1～1:1.5;
Described initiator is a persulphate;
(4) under 80-85 ℃, adopt the mode that drips to add the seed emulsion C of step (3) pre-emulsion B, in 3～5h, drip and finish, drip the mixing solutions of initiator and water simultaneously, drip finish after, be incubated 1-2h, emulsion is cooled to 60-70 ℃;
The parts by weight of each component are following:
Seed emulsion C24～37 part, pre-emulsion B55～66 part, initiator 0.2-0.5 part, 10 parts in water;
(5) residual monomer aftertreatment
The tertbutyl peroxide aqueous solution of gross weight 40～60% is added the product of step (4), and 60-70 ℃ of insulated and stirred 5～10min adds the metabisulfite solution of gross weight 40～60%, 60-70 ℃ of insulated and stirred 5～10min then;
The butylhydroperoxide aqueous solution that adds surplus again; 60-70 ℃ of insulated and stirred 5～10min, and then the metabisulfite solution of adding surplus, 60-70 ℃ is stirred 10～25min; The emulsion of residual monomer has been removed in acquisition; Be cooled to 10～39 ℃, regulate PH to 7-8, obtain described interior wall coating and use benzene emulsion with alkaline matter;
Said alkaline matter is that weight concentration is that 5～25% sodium hydroxide solution or weight concentration are 5～25% ammoniacal liquor;
The weight concentration of the described tertbutyl peroxide aqueous solution is 5～10%;
The weight concentration of described metabisulfite solution is 2～4%;
The parts by weight of each component are following:
0.5 ~ 1.0 part of the tertbutyl peroxide aqueous solution; 0.5 ~ 1.0 part of Sodium Pyrosulfite;
In step (1)～(5), described nonionic emulsifying agent is TX10 or polyoxyethylene nonylphenol;
Described anionic emulsifier is alkyl phenol ether ammonium sulfate or alkyl phenol polyether sulfonic group succinic acid monoester sodium;
Said persulphate is a Sodium Persulfate, ammonium persulphate or Potassium Persulphate;
One end of said response type an organosilane monomer contains the vinyl unsaturated link(age), and the other end contains the oxygen alkyl structure that hydrolyzable is a silanol.A small amount of vinyl silicane coupling agent that adds, intramolecular ethylene double bond and Acrylic Acid Monomer copolymerization form the block compound.The silane coupling agent hydrolysis goes out silanol in the self-vulcanizing process, take place hydroxyl on self-crosslinking reaction and emulsion resin and the ground between the emulsion resin molecule condensation reaction and with the crosslinking of metals ion, formation network structure, the scrub resistance of raising emulsion.
Acrylic amide can make the water-soluble increase of multipolymer, and crosslinked polymer is solidified, and improves into film toughness, obtains high performance copolymer emulsion.
When the present invention is employed in letex polymerization, introduce response type an organosilane monomer and acrylic amide simultaneously, have two kinds in the time of can making coating film simultaneously and be not both crosslinking method, improve the cross-linking density of filming, strengthen the scrub resistance of filming.
Emulsion of the present invention is mixed with interior wall coating, compares with commercially available emulsion of the same type, add a spot of emulsion, scrub resistance also is superior to other emulsions, helps reducing the formulation for coating material cost, and economizes on resources.Wherein the emulsion addition is 10%, and the coating solid is divided into 50%, and scrub resistance is more than 1000 times, other excellent propertys.
Embodiment
As not specifying, among the embodiment, be weight part.
Embodiment 1
(1) in parts by weight; With 16 parts of deionized waters; 0.3 part in alkyl phenol ether ammonium sulfate, polyoxyethylene nonylphenol mixes for 0.3 part, and adding is 2.4 parts of mixtures of forming of acrylamide solution of 50% by 27 parts of vinylbenzene, 1 part of 21 parts of methylacrylic acid of Bing Xisuandingzhi and weight concentration; Emulsification 30 minutes makes pre-emulsion A.
(2) the response type organosilicon is added among the above-mentioned pre-emulsion A, emulsification 15min makes pre-emulsion B;
0.7 part of response type organosilicon, pre-emulsion A are 63.46 parts.
Said response type an organosilane monomer is γ-methacryloxypropyl trimethoxy silane;
(3) with 25 parts in water, 0.3 part in alkyl phenol ether ammonium sulfate, 0.2 part of polyoxyethylene nonylphenol, 1 part of methyl alcohol; 0.08 part of mixing of sodium hydrogencarbonate, 170r/min stirs down, and logical nitrogen is opened water of condensation; Be warming up to 77 ℃, add 3.34 parts of preparatory emulsification latex A, keep 75 ℃ of temperature, stir 5min; Add 0.15 part of initiator Sodium Persulfate, reaction 15min makes seed emulsion C;
(4) pre-emulsion B is added dropwise to seed emulsion C, in 4h, drips and finish, drip the mixing solutions of initiator Sodium Persulfate and water simultaneously, dropwise at 4.5h, temperature remains on 80 ℃, and after dropping finished, insulation 1.5h was cooled to 60 ℃ with emulsion;
The parts by weight of each component are following:
Seed emulsion C30.07 part, pre-emulsion B63.46 part, 0.4 part of initiator, 10 parts in water;
(5) the tertbutyl peroxide aqueous solution of gross weight 50% is added the product of step (4), 60 ℃ of insulated and stirred 5min add the metabisulfite solution of gross weight 50%, 60 ℃ of insulated and stirred 10min then;
The butylhydroperoxide aqueous solution that adds surplus again; 60 ℃ of insulated and stirred 5min, and then the metabisulfite solution of adding surplus, 60 ℃ are stirred 15min; The emulsion of residual monomer has been removed in acquisition; Be cooled to 30 ℃, the use weight concentration is 15% sodium hydroxide solution adjusting PH to 8, obtains described interior wall coating and uses benzene emulsion;
The weight concentration of the described tertbutyl peroxide aqueous solution is 6%;
The weight concentration of described metabisulfite solution is 3%;
The parts by weight of each component are following:
0.6 part of the tertbutyl peroxide aqueous solution; 0.8 part of metabisulfite solution.
Embodiment 2
(1) in parts by weight; With 16 parts in water; 0.3 part in alkyl phenol ether ammonium sulfate, 0.3 part of mixing of TX10, add stirred by 25 parts of vinylbenzene, 24 parts of Bing Xisuandingzhis, 1 part of methylacrylic acid and 2.4 parts of mixtures of forming of 50% acrylamide solution; Emulsification 30 minutes makes pre-emulsion A.
(2) the response type organosilicon is added among the above-mentioned pre-emulsion A, emulsification 15min makes pre-emulsion B;
0.7 part of response type organosilicon, 67.8 parts of pre-emulsions;
Said response type an organosilane monomer is a vinyltriethoxysilane;
(3) with 25 parts in water, 0.3 part in alkyl phenol ether ammonium sulfate, 0.2 part of TX10,1 part of methyl alcohol; 0.08 part of mixing of sodium hydrogencarbonate, 170r/min stirs down, and logical nitrogen is opened water of condensation; Be warming up to 77 ℃, add 3.39 parts of 5% preparatory emulsification latex A, keep 80 ℃ of temperature, stir 5min; Add 0.15 part of initiator ammonium persulfate, reaction 15min makes seed emulsion C;
(4) pre-emulsion B is added dropwise to seed emulsion C, in 4h, drips and finish, drip the mixing solutions of initiator ammonium persulfate and water simultaneously, dropwise at 4.5h, temperature remains on 85 ℃; After dripping end, insulation 1.5h is cooled to 60 ℃ with emulsion;
The parts by weight of each component are following:
Seed emulsion C30.12 part, pre-emulsion B64.41 part, 0.4 part of initiator, 10 parts in water;
(5) the tertbutyl peroxide aqueous solution of gross weight 50% is added the product of step (4), 70 ℃ of insulated and stirred 5min add the metabisulfite solution of gross weight 50%, 70 ℃ of insulated and stirred 10min then;
The butylhydroperoxide aqueous solution that adds surplus again; 70 ℃ of insulated and stirred 5min, and then the metabisulfite solution of adding surplus, 70 ℃ are stirred 20min; The emulsion of residual monomer has been removed in acquisition; Be cooled to 30 ℃, the use weight concentration is 15% ammoniacal liquor adjusting PH to 7, obtains described interior wall coating and uses benzene emulsion;
The weight concentration of the described tertbutyl peroxide aqueous solution is 4%;
The weight concentration of described metabisulfite solution is 3%;
The parts by weight of each component are following:
0.6 part of the tertbutyl peroxide aqueous solution; 0.8 part of sodium metabisulfite solution.
Embodiment 3
(1) in parts by weight; With 16 parts of deionized waters; 0.4 part of alkyl phenol polyether sulfonic group succinic acid monoester sodium, 0.35 part of mixing of polyoxyethylene nonylphenol, adding by 20 parts of vinylbenzene, 7 parts of TEB 3Ks, 21 parts of Bing Xisuandingzhis, 1 part of methylacrylic acid and weight concentration is 2.0 parts of mixtures of forming of 50% acrylamide solution; Emulsification 30 minutes makes pre-emulsion A.
(2) the response type organosilicon is added among the above-mentioned pre-emulsion A, emulsification 15min makes pre-emulsion B;
0.7 part of response type organosilicon, pre-emulsion A66.75 part;
Said response type an organosilane monomer is a vinyltriethoxysilane;
(3) with 25 parts in water, 0.25 part of alkyl phenol polyether sulfonic group succinic acid monoester sodium, 0.15 part of polyoxyethylene nonylphenol, 1 part of methyl alcohol and 0.08 part of mixing of sodium hydrogencarbonate, 170r/min stirs down, logical nitrogen; Open water of condensation, be warming up to 77 ℃, add 3.39 parts of 5% preparatory emulsification latex A; Keep 78 ℃ of temperature, stir 5min, add 0.15 part of initiator potassium persulfate; Reaction 15min makes seed emulsion C;
(4) pre-emulsion B is added dropwise to seed emulsion C, in 4h, drips and finish, drip the mixing solutions of initiator ammonium persulfate and water simultaneously, dropwise at 4.5h, temperature remains on 85 ℃; After dripping end, insulation 1.5h is cooled to 60 ℃ with emulsion;
The parts by weight of each component are following:
Seed emulsion C29.8 part, pre-emulsion B63.41 part, 0.4 part of initiator, 10 parts in water;
(5) the tertbutyl peroxide aqueous solution of gross weight 60% is added the product of step (4), 65 ℃ of insulated and stirred 5min add the metabisulfite solution of gross weight 60%, 65 ℃ of insulated and stirred 10min then;
The butylhydroperoxide aqueous solution that adds surplus again; 65 ℃ of insulated and stirred 5min, and then the metabisulfite solution of adding surplus, 65 ℃ are stirred 20min; The emulsion of residual monomer has been removed in acquisition; Be cooled to 30 ℃, the use weight concentration is 15% ammoniacal liquor adjusting PH to 7, obtains described interior wall coating and uses benzene emulsion;
The weight concentration of the described tertbutyl peroxide aqueous solution is 4%;
The weight concentration of described metabisulfite solution is 3%;
The parts by weight of each component are following:
0.6 part of the tertbutyl peroxide aqueous solution; 0.8 part of sodium metabisulfite solution.
Embodiment 4
Adopt following formulated interior wall coating, the product of embodiment 1～3 is made an experiment, the result is following.
The interior wall coating prescription sees the following form one.
In the table one, the consumption of each component is a mass fraction.
Table one interior wall coating prescription
Detect by the product of standard " GB/T 9756-2009 synthetic resin emulsion interior wall coating " to embodiment 1～3, the result sees table two.
The product coating detected result of table two embodiment 1～3
Claims (9)
1. interior wall coating is characterized in that with the preparation method of benzene emulsion, comprises the steps:
(1) deionized water, compound emulsifying agent, acrylate monomer and function monomer are mixed, emulsification obtains pre-emulsion A;
(2) the response type organosilicon is added among the pre-emulsion A, emulsification obtains pre-emulsion B;
(3) with the mixture of water, compound emulsifying agent, methyl alcohol and sodium hydrogencarbonate, add the described preparatory emulsification latex A of step (1), stir, add initiator, reaction obtains to make seed emulsion C;
(4) mode that pre-emulsion B employing is dripped adds the seed emulsion C of step (3), drips the mixing solutions of initiator and water simultaneously, and after dropping finished, emulsion was lowered the temperature in insulation;
(5) remove residual monomer, regulate PH to 7-8, obtain described interior wall coating and use benzene emulsion with alkaline matter.
2. method according to claim 1 is characterized in that, in the step (1), the parts by weight of each component are following:
Water 15-20 part, compound emulsifying agent 0.4-1.0 part, mix monomer 45-50 part, function monomer 0.5-2 part;
Said compound emulsifying agent is made up of anionic emulsifier and nonionic emulsifying agent, and the weight ratio of nonionic emulsifying agent and anionic emulsifier is 1: 1～1:1.5;
Said mix monomer is made up of vinylbenzene, propenoate and Acrylic Acid Monomer;
Said propenoate is selected from more than one in TEB 3K, Bing Xisuandingzhi or the Isooctyl acrylate monomer;
Said Acrylic Acid Monomer is methylacrylic acid or vinylformic acid;
Each components by weight is:
Vinylbenzene: propenoate: methylacrylic acid=(20～27): (21～28): 1;
Said function monomer is the acrylamide solution of weight concentration 45～55%.
3. method according to claim 1 is characterized in that, in the step (2), the parts by weight of component are following:
Response type organosilicon 0.5-1 part, pre-emulsion A55 ~ 66 part;
Said response type an organosilane monomer is γ-methacryloxypropyl trimethoxy silane or vinyltriethoxysilane.
4. method according to claim 1 is characterized in that, in the step (3); In nitrogen atmosphere, 150-200r/min stirs down, adds the described preparatory emulsification latex A of step (1) under the 75-80 ℃ of temperature; Stir 5 ~ 10min; Add initiator, reaction 10～20min obtains to make seed emulsion C.
5. method according to claim 4 is characterized in that, in the step (3), the parts by weight of each component are following:
Water 20-30 part, compound emulsifying agent 0.5-0.7 part, methyl alcohol 1-2 part, sodium hydrogencarbonate 0.05-0.1 part, the emulsification emulsion is 2.9 ~ 3.3 parts in advance, initiator 0.1-0.2 part;
Said compound emulsifying agent is made up of anionic emulsifier and nonionic emulsifying agent, and the weight ratio of nonionic emulsifying agent and anionic emulsifier is 1: 1～1:1.5;
Described initiator is a persulphate.
6. method according to claim 1 is characterized in that, in the step (4); Under 80-85 ℃, adopt the mode that drips to add the seed emulsion C of step (3) pre-emulsion B, in 3～5h, drip and finish; Drip the mixing solutions of initiator and water simultaneously; After dripping end, insulation 1-2h is cooled to 60-70 ℃ with emulsion.
7. method according to claim 6 is characterized in that, in the step (4), the parts by weight of each component are following: seed emulsion C24～37 part, pre-emulsion B55～66 part, initiator 0.2-0.5 part, 10 parts in water.
8. according to each described method of claim 1～7, it is characterized in that in step (1)～(5), described nonionic emulsifying agent is TX10 or polyoxyethylene nonylphenol;
Described anionic emulsifier is alkyl phenol ether ammonium sulfate or alkyl phenol polyether sulfonic group succinic acid monoester sodium;
Said persulphate is Sodium Persulfate, ammonium persulphate or Potassium Persulphate.
9. use benzene emulsion according to the interior wall coating of each said method preparation of claim 1～8.
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Application publication date: 20121219 |