CN103897095B - Preparation method of acrylic ester latex containing acetic acid - Google Patents
Preparation method of acrylic ester latex containing acetic acid Download PDFInfo
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- CN103897095B CN103897095B CN201210579575.4A CN201210579575A CN103897095B CN 103897095 B CN103897095 B CN 103897095B CN 201210579575 A CN201210579575 A CN 201210579575A CN 103897095 B CN103897095 B CN 103897095B
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- latex
- acetic acid
- agglomeration
- styrene
- deionized water
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- 229920000126 latex Polymers 0.000 title claims abstract description 114
- 239000004816 latex Substances 0.000 title claims abstract description 110
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 66
- -1 acrylic ester Chemical class 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 34
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 17
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 17
- 235000019394 potassium persulphate Nutrition 0.000 claims description 15
- 239000004159 Potassium persulphate Substances 0.000 claims description 11
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 46
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 abstract description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 15
- 239000007787 solid Substances 0.000 abstract description 14
- 229920003048 styrene butadiene rubber Polymers 0.000 abstract description 14
- 239000002174 Styrene-butadiene Substances 0.000 abstract description 13
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 abstract description 13
- 239000011115 styrene butadiene Substances 0.000 abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Polymers OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 abstract 1
- 230000001804 emulsifying effect Effects 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 description 47
- 230000002776 aggregation Effects 0.000 description 47
- 229920000642 polymer Polymers 0.000 description 12
- 239000000178 monomer Substances 0.000 description 10
- 150000002148 esters Chemical class 0.000 description 7
- MPSXZBZUSOMAQW-UHFFFAOYSA-N acetic acid;prop-1-ene Chemical group CC=C.CC(O)=O MPSXZBZUSOMAQW-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000013112 stability test Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 description 1
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 description 1
- YAJYJWXEWKRTPO-UHFFFAOYSA-N 2,3,3,4,4,5-hexamethylhexane-2-thiol Chemical compound CC(C)C(C)(C)C(C)(C)C(C)(C)S YAJYJWXEWKRTPO-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N 2-butenoic acid Chemical compound CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 235000010985 glycerol esters of wood rosin Nutrition 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a preparation method of acrylic ester latex containing acetic acid; stirring and pre-emulsifying sodium dodecyl sulfate, alkylphenol polyoxyethylene (10) ether and deionized water, and adding sodium chloride; after nitrogen replacement, adding a part of a mixture of butyl acrylate and styrene, then adding a potassium persulfate deionized water solution, and reacting for 30-60 minutes at 70-75 ℃; adding acetic acid into the residual butyl acrylate and styrene mixture for further mixing, dropwise adding for 1-2 hours, heating to 75-85 ℃, continuing to react for 2-4 hours, cooling, and filtering to obtain acrylic ester latex containing acetic acid; the latex prepared by the method has the particle size of 65-90nm and the solid content of 30-50%, and the latex can increase the styrene-butadiene latex with the particle size of about 130nm to 240-380nm and increase the butadiene latex with the particle size of about 280nm to 580-650 nm.
Description
Technical field:
The present invention relates to a kind of preparation method of agglomerating latex, particularly relate to a kind of agglomeration technique and small particle size rubber latex is prepared into Large stone rubber latex and the preparation method containing the acrylate latex of acetic acid.
Background technology
ABS resin is a kind of very important engineering plastics, and application is very extensive, first needs the rubber latex synthesizing Large stone, and adopts agglomeration technique synthesis large grain size latex can shorten polymerization time, enhance productivity in its production process.
Polymer agglomeration technique first synthesizes polymer agglomerant, then added by polymer agglomerant in the polymer latex (treating agglomerating latex) needing to increase particle diameter, make the method that the latter's particle diameter increases.Compared with existing chemical agglomeration (as mineral acid agglomeration, inorganic salt agglomeration etc.), material agglomeration (freezing agglomeration, Pressure agglomeration etc.), the difficulty increasing particle diameter is transferred on a kind of suitable polymer agglomerant of synthesis by polymer agglomeration technique, and can realize larger particle diameter increase effect.In the present invention, agglomeration method is simple, agglomerating latex polymerizing condition is gentle, ag-glomeration time is short, use the latex of this method agglomeration, change change of size in time little, by the particle diameter of latex after adjustment agglomerating latex consumption control agglomeration, centralized particle diameter, after agglomeration, latex stability is fabulous, thus there is very large development potentiality and practical value, in ABS resin, ACR resin (series modified dose of esters of acrylic acid), MBS resin (methyl methacrylate, divinyl, styrene copolymer) etc. production in, and be with a wide range of applications in the production of rubber toughened resin.
JP60112841 discloses by (methyl) vinylformic acid, methylene-succinic acid (or butenoic acid), C1-12 alkyl acrylate and vinyl monomer, the multi-component copolymer latex adopting two sections of letex polymerizations to prepare is polymer agglomerant, and agglomeration increases butadiene-propylene acid butyl ester-styrene copolymerized latex.Treat agglomerating latex particle diameter 70nm, agglomeration is particle diameter 290nm after 30 minutes, and agglomeration is particle diameter 310nm after 5 days.
US2002198309 discloses with the method for butadiene-propylene acetoacetic ester-Sipacril 2739OF latex for polymer agglomerant increase diolefine latex particle size.
The synthetic method of CN1260352 Large stone acrylic latex is: add the emulsifying agent accounting for reaction monomers total amount 0.01-9.09wt% to polymeric kettle; The monomer accounting for reaction monomers total amount 30-60wt% is added to polymeric kettle; The initiator accounting for reaction monomers total amount 0.2-0.8wt% is added to polymeric kettle; Water is added to polymeric kettle; Reinforced complete, the emulsifying agent accounting for reaction monomers total amount 0.2-0.8wt% and remaining 40-70wt% monomer is added again after temperature reaction 15-20 minute, this partial emulsifier and monomer can once or gradation add, reinforced complete, isothermal reaction 3-5 hour, gained latex particle size 200-600nm, is aggregated in same reactor and completes, and the reaction times is short, cost is low.
CN87104770 is by treating that the latex of agglomeration mixes with a kind of agglomerating latex the nodulizing carrying out the polymer latex being selected from elastomerics and thermoplastic resin mutually.Agglomerating latex consists of: (A) a kind of polymkeric substance being selected from elastomerics and thermoplastic resin; (H) nonionic surface active agent be made up of block polymer, is selected from the segment of the polymkeric substance of ethene, diene, acrylate or methacrylic ester containing at least one polyoxyethylene segment and at least one in polymkeric substance.By during synthesis (A) polymkeric substance, make a kind of tensio-active agent with (B) and produce above-mentioned agglomerating latex.Polyoxyethylene one polystyrene one polyoxyethylene triblock polymer is mentioned among tensio-active agent (H).
CN1730505 puts into same container butyl acrylate, vinylformic acid, de-salted water, Sodium dodecylbenzene sulfonate etc. and stirs and heating, add Potassium Persulphate and tert-dodecyl mercaptan again, temperature of reaction controls at 30-98 DEG C, and the reaction times is 2-8 hour, prepares agglomerant.This agglomerant is used for, in the agglomeration of PB latex, in polymeric kettle, add PB latex, stirs, heat, then agglomerant, Sodium dodecylbenzene sulfonate, de-salted water are mixed, join in polymeric kettle after stirring; In polymeric kettle, add NaOH solution again, adjusted to ph is 9-13, and after obtaining agglomeration, PB latex particle size is 300-700nm.In the present invention, owing to adding comonomer, to make in agglomerant thermal discharge reduce, reaction conditions is gentleer, and reaction yield almost 100%, does not have environmental pollution.
Summary of the invention
The object of this invention is to provide the simple emulsion polymerization of a kind of technique, prepare a kind of high molecular weight acrylic ester gum breast containing acetic acid, the particle diameter increasing styrene butadiene rubber latex, butadiene latex can be effective to.
Technical scheme of the present invention is as follows:
By sodium lauryl sulphate, alkylphenol-polyethenoxy (10) ether and deionized water and stirring pre-emulsification, add sodium-chlor; After nitrogen replacement, add part propylene acid butyl ester, styrene mixture, then add Potassium Persulphate deionized water solution, at 70-75 DEG C, react 30-60 minute; Remaining butyl acrylate, styrene mixture are added acetic acid and mix further, and time for adding is at 1-2 hour; Be warming up to 75-85 DEG C, continue reaction 2-4 hour, cooling, filtration, obtain the acrylate latex containing acetic acid.
Above monomer forms by following masses 100%:
Butyl acrylate (BA) 25-50%, vinylbenzene (ST) 25-55%, acetic acid 5-25%, sodium-chlor (NaCL) 0.1-0.5%, sodium lauryl sulphate (SDS) 1-3%, alkylphenol-polyethenoxy (10) ether 2-6%, Potassium Persulphate (KPS) 0.1-0.5%; Add above-mentioned monomer mass 150-245% deionized water.
After nitrogen replacement, butyl acrylate and styrene mixture add-on account for 40% of amount of the mixture.
Beneficial effect of the present invention:
Adopt the present invention to prepare latex particle size between 65-90nm, solid content is at 30-50%.This reaction conversion ratio is high, do not need to carry out aftertreatment, this latex effectively can increase the particle diameter of styrene-butadiene latex, butadiene latex, particle diameter can be increased to 240-380nm at the styrene-butadiene latex of about 130nm, particle diameter is increased to 580-650nm at the butadiene latex of about 280nm.
Polymerization technique of the present invention is simple, particular requirement is not had to equipment, agglomeration process gentleness is controlled, ag-glomeration time is short, do not need extraneous stabilizing agents, after agglomeration, the size of latex is only relevant with the amount of agglomerating latex, very little with shelf-time change, there is extraordinary stability, place the not too large change substantially such as latex particle size, mechanical stability after a week.
Under normal temperature and pressure, the acrylate latex (agglomerating latex) containing acetic acid is joined by a certain percentage under whipped state and treats (to provide for oneself) in agglomerating latex, reaction 1-30 minute.
Agglomerating latex with treat that agglomerating latex component (butt mass ratio) is:
Treat agglomerating latex 100 parts
Agglomerating latex 1 ~ 20 part
Treat agglomeration small-particle styrene-butadiene latex solid content: 25 ~ 35%, particle diameter: 120 ~ 140nm;
Macroparticle styrene-butadiene latex particle diameter after agglomeration is 240 ~ 380nm;
Treat agglomeration macroparticle butadiene latex solid content: 45 ~ 65%, particle diameter: 280 ~ 320nm;
Macroparticle butadiene latex particle diameter after agglomeration is 580 ~ 650nm
After agglomeration, latex timing detects the changing conditions that mechanical stability determines latex stability.Mechanical stability detects: adopt the steady instrument of central physics and chemistry Co., Ltd. UP-2 machine to measure the mechanical stability of latex.Granularity Detection: adopt U.S. Brooker Hai Wen company 90Plus particle diameter tester to measure.The mensuration of solid content: get about 1.5 grams polymer latexs putting into air dry oven and dry after weighing in weighing disk, wherein dry-matter accounts for the solid content that the percentage composition of wet emulsion is exactly this latex.
Embodiment
Embodiment 1:
Synthesis is containing acetate propylene acid esters latex (agglomerant) desired raw material composition
Butyl acrylate (BA) 45 grams, vinylbenzene (ST) 45 grams, acetic acid 5 grams, Potassium Persulphate (KPS) 0.4 gram, sodium lauryl sulphate (SDS) 1.5 grams, 3 grams, alkylphenol-polyethenoxy (10) ether, 0.1 gram, sodium-chlor, deionized water 160 grams.
Polymerisation process is as follows:
(1) carrying out pre-emulsification with adding sodium lauryl sulphate (SDS), alkylphenol-polyethenoxy (10) ether and 110 grams of deionized waters in the reaction flask of whipping appts, sodium-chlor is added;
(2) butyl acrylate and vinylbenzene are mixed, getting mixed solution 36 grams joins in reaction flask, and with nitrogen replacement, Potassium Persulphate (water yield is in total deionized water) in 50 gramion water is joined in reaction flask after dissolving, reacts 40 minutes at 70 DEG C;
(3) remaining butyl acrylate and styrene mixture are added acetic acid to mix further, be added drop-wise in reaction flask, time for adding is 60 minutes; Continue reaction at 70 DEG C to be warming up to 78 DEG C after 30 minutes and to react 60 minutes again, obtain containing acetate propylene acid esters latex (agglomerating latex), latex solid content 38.3%, particle diameter 75.8nm.
(4) with the agglomerating latex of above gained to solid content be 34.3%, the styrene-butadiene latex of particle diameter 125nm (treating agglomerating latex) carries out agglomeration, to treat that agglomerating latex 100 grams slowly drips the agglomerating latex of 6.7 grams under stirring at normal temperature condition, stir 20 minutes, obtain the styrene-butadiene latex after agglomeration.Latex particle size after agglomeration, mechanical stability test result are as follows:
| Particle diameter (nm) | Mechanical stability | |
| After agglomeration 1 hour | 313 | 0.032 |
| 8 hours | 316 | 0.041 |
| 3 days | 321 | 0.049 |
| One week | 323 | 0.058 |
| Two weeks | 328 | 0.061 |
Embodiment 2:
Synthesis is containing acetate propylene acid esters latex (agglomerant) desired raw material composition
Butyl acrylate (BA) 35 grams and vinylbenzene (ST) 45 grams, acetic acid 16 grams, Potassium Persulphate (KPS) 0.5 gram, sodium lauryl sulphate (SDS) 1 gram, 2.4 grams, alkylphenol-polyethenoxy (10) ether, 0.1 gram, sodium-chlor, deionized water 170 grams.
Polymerisation process is as follows:
(1) carrying out pre-emulsification with adding sodium lauryl sulphate (SDS), alkylphenol-polyethenoxy (10) ether and 120 grams of deionized waters in the reaction flask of whipping appts, sodium-chlor is added;
(2) butyl acrylate and vinylbenzene are mixed, getting mixed solution 24 grams joins in reaction flask, and with nitrogen replacement, Potassium Persulphate is joined in reaction flask after (water yield is in total deionized water) dissolving in 50 grams of deionized waters, reacts 50 minutes at 70 DEG C;
(3) remaining butyl acrylate and styrene mixture are added acetic acid to mix further, be added drop-wise in reaction flask gradually, time for adding is 60 minutes; Continue reaction at 70 DEG C to be warming up to 75 DEG C after 30 minutes and to react 60 minutes again, obtain containing acetate propylene acid esters latex (agglomerating latex) latex solid content 35.9%, particle diameter 83.6nm.
(4) with the agglomerating latex of above gained to solid content be 32.6%, the styrene-butadiene latex of particle diameter 129nm (treating agglomerating latex) carries out agglomeration, to treat that agglomerating latex 100 grams slowly drips the agglomerating latex of 5.5 grams under stirring at normal temperature condition, stir 20 minutes, obtain the styrene-butadiene latex after agglomeration.Latex particle size after agglomeration, mechanical stability test result are as follows:
| Particle diameter (nm) | Mechanical stability | |
| After agglomeration 1 hour | 342 | 0.042 |
| 8 hours | 349 | 0.049 |
| 3 days | 356 | 0.056 |
| One week | 359 | 0.059 |
| Two weeks | 362 | 0.064 |
(5) with the agglomerating latex of above gained to solid content be 45.8%, the butadiene latex of particle diameter 284nm (treating agglomerating latex) carries out agglomeration and will treat that agglomerating latex 100 grams slowly drips the agglomerating latex of 7.6 grams under stirring at normal temperature condition, stir 20 minutes, obtain the styrene-butadiene latex after agglomeration.Latex particle size after agglomeration, mechanical stability test result are as follows:
| Particle diameter (nm) | Mechanical stability | |
| After agglomeration 1 hour | 589 | 0.049 |
| 8 hours | 596 | 0.053 |
| 3 days | 599 | 0.058 |
| One week | 602 | 0.061 |
| Two weeks | 605 | 0.065 |
Embodiment 3:
Synthesis is containing acetate propylene acid esters latex (agglomerant) desired raw material composition
Butyl acrylate (BA) 40 grams and vinylbenzene (ST) 40 grams, acetic acid 14 grams, Potassium Persulphate (KPS) 0.4 gram, sodium lauryl sulphate (SDS) 2 grams, 3.5 grams, alkylphenol-polyethenoxy (10) ether, 0.1 gram, sodium-chlor, deionized water 185 grams.
Polymerisation process is as follows:
(1) carrying out pre-emulsification with adding sodium lauryl sulphate (SDS), alkylphenol-polyethenoxy (10) ether and 135 grams of deionized waters in the reaction flask of whipping appts, sodium-chlor is added;
(2) butyl acrylate and vinylbenzene are mixed, getting mixed solution 30 grams joins in reaction flask, after nitrogen replacement, by Potassium Persulphate, in 50 grams of deionized waters, (water yield is in total deionized water) joins in reaction flask after dissolving, and reacts 50 minutes at 70 DEG C;
(3) remaining butyl acrylate and styrene mixture are added acetic acid to mix further, be added drop-wise in reaction flask gradually, time for adding is 60 minutes; Continue reaction at 70 DEG C to be warming up to 85 DEG C after 30 minutes and to react 60 minutes again, obtain containing acetate propylene acid esters latex (agglomerating latex), latex solid content 35.1%, particle diameter 74nm.
(4) with the agglomerating latex of above gained to solid content be 33.6%, the styrene-butadiene latex of particle diameter 138nm (treating agglomerating latex) carries out agglomeration, to treat that agglomerating latex 100 grams slowly drips the agglomerating latex of 14.3 grams under stirring at normal temperature condition, stir 20 minutes, obtain the styrene-butadiene latex after agglomeration.Latex particle size after agglomeration, mechanical stability test result are as follows:
| Particle diameter (nm) | Mechanical stability | |
| After agglomeration 1 hour | 369 | 0.032 |
| 8 hours | 375 | 0.041 |
| 3 days | 376 | 0.049 |
| One week | 381 | 0.058 |
| Two weeks | 384 | 0.063 |
(5) with the agglomerating latex of above gained to solid content be 46.5%, the butadiene latex of particle diameter 298nm (treating agglomerating latex) carries out agglomeration and will treat that agglomerating latex 100 grams slowly drips the agglomerating latex of 19.9 grams under stirring at normal temperature condition, stir 20 minutes, obtain the styrene-butadiene latex after agglomeration.Latex particle size after agglomeration, mechanical stability test result are as follows:
| Particle diameter (nm) | Mechanical stability | |
| After agglomeration 1 hour | 626 | 0.058 |
| 8 hours | 635 | 0.063 |
| 3 days | 642 | 0.068 |
| One week | 648 | 0.072 |
| Two weeks | 653 | 0.075 |
Claims (2)
1., containing a preparation method for the acrylate latex of acetic acid, it is characterized in that: by sodium lauryl sulphate, alkylphenol polyoxyethylene and deionized water and stirring pre-emulsification, add sodium-chlor; After nitrogen replacement, add part propylene acid butyl ester and styrene mixture, then add Potassium Persulphate deionized water solution, at 70-75 DEG C, react 30-60 minute; Remaining butyl acrylate, styrene mixture are added acetic acid and mix further, and time for adding, at 1-2 hour, is warming up to 75-85 DEG C, continues reaction 2-4 hour, cooling, filtration, the obtained acrylate latex containing acetic acid;
Above material forms by following masses 100%:
Butyl acrylate 25-50%, vinylbenzene 25-55%, acetic acid 5-25%, sodium-chlor 0.1-0.5%, sodium lauryl sulphate 1-3%, alkylphenol polyoxyethylene 2-6%, Potassium Persulphate 0.1-0.5%, deionized water is the 150-245% of above-mentioned substance quality.
2. the preparation method of a kind of acrylate latex containing acetic acid according to claim 1, is characterized in that: after nitrogen replacement, adds 40% of butyl acrylate and the rear total amount of vinylbenzene mixing.
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