CN108219061A - A kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap - Google Patents

A kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap Download PDF

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Publication number
CN108219061A
CN108219061A CN201810114501.0A CN201810114501A CN108219061A CN 108219061 A CN108219061 A CN 108219061A CN 201810114501 A CN201810114501 A CN 201810114501A CN 108219061 A CN108219061 A CN 108219061A
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monomer
solution
initiator
eau
iii
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单秀军
朱立伟
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Suzhou Mahayana Environmental Protection New Material Co Ltd
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Suzhou Mahayana Environmental Protection New Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D133/00Coating 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
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/08Homopolymers or copolymers of acrylic acid esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1808C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate

Abstract

The preparation method of pure acrylic latex is synthesized with no soap the present invention relates to a kind of aqueous EAU; the main preparation for including protection sol solution, the preparation of initiator solution I, initiator solution II, initiator solution III; the preparation of monomer I, monomer II, monomer III and rear additive solution; after fetching protection the slow heating of sol solution again; initiator solution I, monomer I are poured into uniform stirring reaction; monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system, is kept the temperature after being added dropwise;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, finally system, which cools down, again adjusts pH, agitation and filtration;The aqueous EAU acrylic emulsions being prepared in the present invention are in reticular structure and adhered to the high-environmental required by aqueous EAU technologies, high-weatherability feature, and with good mechanicalness and ductility.

Description

A kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap
Technical field
The present invention relates to more particularly to a kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap.
Background technology
Aqueous EAU technologies full name is Eco-friendly Acrylics Unity, is a kind of ecology close friend environment-friendly water-based third Olefin(e) acid crosslinking technological is the full water-based system to be researched and developed to eco-friendly as eternal theory;This requires produce, transport Defeated, storage, construction and using it is safe and environment-friendly in overall process have no irritating odor, unharmful substance discharge, extremely low VOC etc.. The sports place such as football pitch and runway is required at present is completed using aqueous EAU technologies, i.e., by with various nontoxic nothings Harmful functional additive and meet the elastic granule of environmental requirement and powder combines with basic adhesive and is integrally formed to complete. In aqueous EAU technologies, basic adhesive plays critically important effect;It, which will not only meet, newly mixes under state to performance It is required that while to meet after hardening sports field movenent performance and durability requirement.
If application publication number is a kind of nucleocapsid selfing bipropenyl disclosed in the Chinese patent of " CN106977654A " Yogurt liquid and preparation method thereof, the raw material of center part mainly include Ah's acrylic compounds hard monomer, self-cross linking monomer I, inclined chlorine Ethylene, organic inhibitor, emulsifier I and initiator, shell parts mainly include acrylic compounds soft monomer, self-cross linking monomer II, breast Agent II, phosphoric acid ester monomer, Organic fluoride activated monomer and initiator II;Largely using emulsifier, breast in this preparation method Agent and initiator generate a large amount of bubble or foam, cause to make simultaneously in use, emulsion reaction can occur for extra emulsifier There is defect during standby obtained acrylic acid solution use, such as occur cratering in later stage film or occur in film formation surface Aperture or flake.
Invention content
The preparation method of pure acrylic latex is synthesized with no soap the object of the present invention is to provide a kind of aqueous EAU.
The present invention above-mentioned technical purpose technical scheme is that:A kind of aqueous EAU is closed with no soap Into the preparation method of pure acrylic latex, include the following steps:
Step 1:8% Protection glue is taken, protection sol solution is hybridly prepared into ionized water;
Step 2:Heat partition agent and deionized water are hybridly prepared into initiator solution I, initiator solution II, initiator solution Ⅲ;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;
Step 4:Rear additive is taken to be hybridly prepared into rear additive solution with deionized water;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in reaction kettle again, time for adding 1-2h is dripped 1-2h is kept the temperature after finishing;
Step 6:Reaction kettle is cooled to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in reaction kettle, is protected after being added dropwise Reaction kettle is cooled to 35-45 DEG C of addition pH adjusting agent later, system pH is adjusted to 7-8, stirring is equal later by warm 0.5h-2h Filtering obtains emulsifier-free emulsion polymerization core-shell acrylic lotion after even.
Preferably, I concentration=2 times initiator solution of initiator solution, II concentration=2 times initiator solution, III concentration.
Preferably, the pH adjusting agent is mixed using one or both of ammonium hydroxide or 2-amino-2-methyl-1-propanol Match.
Preferably, additive is using hydrogen peroxide after described, sodium hydrogensulfite, one kind in isopropyl benzene hydroperoxide or A variety of mixtures.
Preferably, the thermal decomposition initiating is using one or more in sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate Mixture.
Preferably, the hard monomer is acrylic acid, acrylamide, methyl methacrylate, one kind in acrylonitrile or A variety of mixtures.
Preferably, the soft monomer is butyl acrylate, butyl methacrylate, one kind in Isooctyl acrylate monomer or A variety of mixtures.
Preferably, the cross-linking monomer is itaconic acid, and Diacetone Acrylamide, hydroxyethyl methacrylate, vinyl In trimethoxy silane, phenyl benzyl dimethyl amine butanone, one or more mixtures in glycidyl methacrylate.
In conclusion the invention has the advantages that:
(1) the aqueous EAU acrylic emulsions being prepared in the present invention, synthesis step mainly includes being nucleated and the step greatly of growth two Suddenly, the initiator solution being prepared, monomer is dropped evenly after being nucleated in sol solution is protected, then by its remaining initiator Solution, monomer and rear additive solution are slowly added dropwise in system, the secondary monomer being added in system adjacent nucleome it Between grow and be connected, make the acrylic emulsion being prepared in reticular structure and adhered to the height required by aqueous EAU technologies The feature of environmental protection, high-weatherability feature, and with good mechanicalness and ductility;
(2) prior art is in the preparation process of acrylic emulsion, and usually addition emulsifier causes monomer, water, initiation thereto Agent etc. uniformly disperses in system and forms small monomer droplet, so as to complete the preparation of acrylic emulsion;But in this programme The middle use that emulsifier is replaced using protection sol solution, monomer, initiator etc. is added dropwise into protection sol solution, and in Protection glue A series of reaction is carried out in solution;It is whole in emulsion process due to there is no the participation of emulsifier in entire reaction process Big bubble will not be generated in a system will not generate fine and close several minute bubbles, so as to influence the membrane body product after coating film forming Matter;
(3) secondly, in the preparation process of this aqueous EAU pure acrylic latexes, the glass transition temperature of nucleome and housing is- Between 40-60 DEG C, thus when heat up so far temperature range when, contribute to the good growth of nucleocapsid;
(4) monomer mainly includes hard monomer, soft monomer and cross-linking monomer, is mixed into after three kinds of monolithic designs are combined into preparation system In;Since monomer therein is divided into soft monomer and hard monomer, the nucleome that is formed and it is connected between adjacent nucleome Serobila is also therefore hard-soft, and when this acrylic emulsion is coated in runway surface or other material surfaces, these long-chains are equal Even expansion, hard monomer therein can improve structural strength and load-bearing, bearing capacity, and soft monomer can then improve the soft of whole system Toughness, it is final so that the acrylic emulsion being prepared has better mechanical performance;
(5) later stage, original center housing was by autoemulsification by cross-linking monomer under the action of initiator and rear additive Emulsion particle surface or inside are adsorbed onto, initiated polymerization makes nucleocapsid become the nucleocapsid with interpenetrating networks later, So that the mechanical property for the acrylic emulsion being prepared is obviously improved;This programme makes in preparation process is produced Material is substantially nontoxic, and overlength chain substance and aromatic substance do not have substantially, therefore the influence to environment is smaller.
Specific embodiment
This specific embodiment is only explanation of the invention, is not limitation of the present invention, people in the art Member can as needed make the present embodiment the modification of no creative contribution after this specification is read, but as long as at this It is all protected in the right of invention by Patent Law.
Embodiment 1:
Step 1:6 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 9.5 parts of Isooctyl acrylate monomers, 1.48 parts of methyl methacrylates, 0.12 part of acryloyl Amine is configured to monomer I;By 85.3 parts of Isooctyl acrylate monomers, 13.3 parts of methyl methacrylates, 1.08 parts of acrylamide configuration Into monomer II, by 17.2 parts of methyl methacrylates, 4.79 parts of Isooctyl acrylate monomer, 1.07 parts of acrylic acid, 0.18 part Vinyltrimethoxysilane, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 2:
Step 1:6 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 9.5 parts of Isooctyl acrylate monomers, 1.48 parts of methyl methacrylates, 0.12 part of acryloyl Amine is configured to monomer I;By 85.3 parts of butyl acrylates, 13.3 parts of methyl methacrylates, 1.08 parts of acrylamide is configured to Monomer II, by 17.2 parts of methyl methacrylates, 4.79 parts of Isooctyl acrylate monomer, 1.07 parts of acrylic acid, 0.18 part of second Alkenyl trimethoxy silane, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 3:
Step 1:8 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 9.5 parts of Isooctyl acrylate monomers, 1.48 parts of methyl methacrylates, 0.12 part of acryloyl Amine is configured to monomer I;By 85.3 parts of Isooctyl acrylate monomers, 13.3 parts of methyl methacrylates, 1.08 parts of acrylamide configuration Into monomer II, by 17.2 parts of methyl methacrylates, 4.79 parts of Isooctyl acrylate monomer, 1.07 parts of acrylic acid, 0.18 part Vinyltrimethoxysilane, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 4:
Step 1:10 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 9.5 parts of Isooctyl acrylate monomers, 1.48 parts of methyl methacrylates, 0.12 part of acryloyl Amine is configured to monomer I;By 85.3 parts of Isooctyl acrylate monomers, 13.3 parts of methyl methacrylates, 1.08 parts of acrylamide configuration Into monomer II, by 17.2 parts of methyl methacrylates, 4.79 parts of Isooctyl acrylate monomer, 1.07 parts of acrylic acid, 0.18 part Vinyltrimethoxysilane, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 5:
Step 1:10 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III, the concentration of the initiator solution I after preparation are other two twice, II He of initiator solution The concentration of initiator solution III is identical;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;9.5 parts of butyl acrylates, 1.48 parts of acrylamides, 0.12 part of acrylonitrile are configured to list by the present embodiment Body I;By 85.3 parts of butyl acrylates, 13.3 parts of methyl methacrylates, 1.08 parts of methyl methacrylate is configured to monomer II, by 17.2 parts of acrylic acid, 4.79 parts of butyl methacrylate, 1.07 parts of acrylic acid, 0.18 part of methacrylic acid contracting Water glyceride, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture uses hydrogen phosphite in the present embodiment Rear additive solution is prepared in sodium;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, pH adjusting agent uses ammonium hydroxide, is filtered after stirring evenly later and obtains emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 6:
Step 1:8 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment matches 12 parts of Isooctyl acrylate monomers, 1.5 parts of methyl methacrylates, 0.2 part of acrylamide It is set to monomer I;By 86 parts of Isooctyl acrylate monomers, 14 parts of methyl methacrylates, 1.1 parts of acrylamide is configured to monomer II, By 18 parts of methyl methacrylates, 5.0 parts of Isooctyl acrylate monomer, 1.1 parts of acrylic acid, 0.2 part of vinyl trimethoxy Silane, 1.5 parts of phenyl benzyl dimethyl amine butanone, 1 part of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 7:
Step 1:8 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 8.5 parts of Isooctyl acrylate monomers, 1.6 parts of methyl methacrylates, 0.15 part of acrylamide It is configured to monomer I;By 87.2 parts of Isooctyl acrylate monomers, 12.6 parts of methyl methacrylates, 0.98 part of acrylamide is configured to Monomer II, by 16.3 parts of methyl methacrylates, 4.5 parts of Isooctyl acrylate monomer, 1.15 parts of acrylic acid, 0.25 part of ethylene Base trimethoxy silane, 1.72 parts of phenyl benzyl dimethyl amine butanone, 1.2 parts of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Embodiment 8:
Step 1:6 parts of Protection glues are taken, protection sol solution is hybridly prepared into ionized water;
Step 2:By heat partition agent according to 4:2:2 ratio is hybridly prepared into initiator solution I, initiator with deionized water respectively Solution II, initiator solution III;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;The present embodiment is by 9.8 parts of Isooctyl acrylate monomers, 1.32 parts of methyl methacrylates, 0.17 part of acryloyl Amine is configured to monomer I;By 86.1 parts of Isooctyl acrylate monomers, 12.7 parts of methyl methacrylates, 1.1 parts of acrylamide is configured to Monomer II, by 16.5 parts of methyl methacrylates, 4.55 parts of Isooctyl acrylate monomer, 1.07 parts of acrylic acid, 0.25 part of second Alkenyl trimethoxy silane, 1.35 parts of phenyl benzyl dimethyl amine butanone, 1.5 parts of itaconic acid are configured to monomer III;
Step 4:Rear additive is taken to be hybridly prepared into a concentration of 5% rear additive solution with deionized water, rear additive uses One or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in system again, time for adding 1-2h is added dropwise After keep the temperature 1-2h;
Step 6:Whole system temperature is reduced to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in system, is added dropwise After keep the temperature 0.5h-2h, later by whole system be cooled to 35-45 DEG C addition pH adjusting agent, pH adjusting agent use ammonium hydroxide or 2- ammonia Base -2- methyl-1s-propyl alcohol, using ammonium hydroxide and 2-amino-2-methyl-1-propanol 1 in the present embodiment:1 mixing, system pH is adjusted To 7-8, filtered after stirring evenly later and obtain emulsifier-free emulsion polymerization core-shell acrylic lotion.
Comparative example is conventional propylene acid solution.
The property of acrylic emulsion being prepared in embodiment 1- embodiments 8 and comparative example is measured, and is recorded in down In Tables 1 and 2.
Table 1:
Table 2:
Conclusion can be obtained according to upper table:The acrylic emulsion being prepared in this programme, which compares common acrylic acid solution, to be had preferably Adhesive force, corrosion resistance, water resistance and mechanical stretching performance, and after dried coating film, surface has no aperture, flake and falls into Cave.

Claims (8)

1. a kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap, which is characterized in that includes the following steps:
Step 1:8% Protection glue is taken, protection sol solution is hybridly prepared into ionized water;
Step 2:Heat partition agent and deionized water are hybridly prepared into initiator solution I, initiator solution II, initiator solution Ⅲ;
Step 3:Hard monomer, soft monomer, cross-linking monomer mixed preparing is taken to form the different monomer I of concentration, monomer II, monomer III 3 Part monomer mixture;
Step 4:Rear additive is taken to be hybridly prepared into rear additive solution with deionized water;
Step 5:It fetches protection sol solution and 75-85 DEG C is to slowly warm up in reaction kettle, initiator solution I, monomer I are poured into uniformly It is stirred to react 0.5-1.0h;Monomer II, II continuously and smoothly of initiator are added dropwise and be mixed into system again, time for adding 1-2h, drop 1-2h is kept the temperature after adding;Initiator III, monomer III is taken at the uniform velocity to be added dropwise in reaction kettle again, time for adding 1-2h is dripped 1-2h is kept the temperature after finishing;
Step 6:Reaction kettle is cooled to 50-60 DEG C, rear additive solution is at the uniform velocity added dropwise in reaction kettle, is protected after being added dropwise Reaction kettle is cooled to 35-45 DEG C of addition pH adjusting agent later, system pH is adjusted to 7-8, stirring is equal later by warm 0.5h-2h Filtering obtains emulsifier-free emulsion polymerization core-shell acrylic lotion after even.
2. a kind of aqueous EAU according to claim 1 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:I concentration=2 times initiator solution of initiator solution, II concentration=2 times initiator solution, III concentration.
3. a kind of aqueous EAU according to claim 1 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:The pH adjusting agent uses one or both of ammonium hydroxide or 2-amino-2-methyl-1-propanol mixture.
4. a kind of aqueous EAU according to claim 3 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:Additive is using one or more of hydrogen peroxide, sodium hydrogensulfite, isopropyl benzene hydroperoxide mixture after described.
5. a kind of aqueous EAU according to claim 4 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:The thermal decomposition initiating is using one or more of sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate mixture.
6. a kind of aqueous EAU according to claim 5 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:The hard monomer is acrylic acid, acrylamide, methyl methacrylate, one or more mixtures in acrylonitrile.
7. a kind of aqueous EAU according to claim 6 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:The soft monomer is butyl acrylate, butyl methacrylate, one or more mixtures in Isooctyl acrylate monomer.
8. a kind of aqueous EAU according to claim 7 synthesizes the preparation method of pure acrylic latex with no soap, feature exists In:The cross-linking monomer is itaconic acid, Diacetone Acrylamide, hydroxyethyl methacrylate, in vinyltrimethoxysilane, Phenyl benzyl dimethyl amine butanone, one or more mixtures in glycidyl methacrylate.
CN201810114501.0A 2018-02-05 2018-02-05 A kind of aqueous EAU synthesizes the preparation method of pure acrylic latex with no soap Pending CN108219061A (en)

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Application publication date: 20180629