CN105764929B - 用于生产具有阳离子官能性的水可再分散聚合物粉末组合物的方法 - Google Patents
用于生产具有阳离子官能性的水可再分散聚合物粉末组合物的方法 Download PDFInfo
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- CN105764929B CN105764929B CN201480062692.0A CN201480062692A CN105764929B CN 105764929 B CN105764929 B CN 105764929B CN 201480062692 A CN201480062692 A CN 201480062692A CN 105764929 B CN105764929 B CN 105764929B
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- protecting colloid
- cation
- vinyl
- polymer powder
- cationic
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- 229920000642 polymer Polymers 0.000 title claims abstract description 51
- 239000000843 powder Substances 0.000 title claims abstract description 51
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 239000000084 colloidal system Substances 0.000 claims abstract description 61
- -1 halide ion Chemical class 0.000 claims abstract description 49
- 239000006185 dispersion Substances 0.000 claims abstract description 42
- 239000000178 monomer Substances 0.000 claims abstract description 38
- 150000001768 cations Chemical class 0.000 claims abstract description 35
- 229920001577 copolymer Polymers 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 24
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 13
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 11
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- 238000000034 method Methods 0.000 claims description 31
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 18
- 125000004432 carbon atom Chemical group C* 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- 229920001567 vinyl ester resin Polymers 0.000 claims description 13
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
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- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 5
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- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- OYINQIKIQCNQOX-UHFFFAOYSA-M 2-hydroxybutyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCC(O)C[N+](C)(C)C OYINQIKIQCNQOX-UHFFFAOYSA-M 0.000 claims description 3
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- IOMDIVZAGXCCAC-UHFFFAOYSA-M diethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](CC)(CC)CC=C IOMDIVZAGXCCAC-UHFFFAOYSA-M 0.000 claims 1
- UXYBXUYUKHUNOM-UHFFFAOYSA-M ethyl(trimethyl)azanium;chloride Chemical compound [Cl-].CC[N+](C)(C)C UXYBXUYUKHUNOM-UHFFFAOYSA-M 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
- 238000005349 anion exchange Methods 0.000 abstract description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 23
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 239000003999 initiator Substances 0.000 description 6
- 238000001728 nano-filtration Methods 0.000 description 6
- 239000012875 nonionic emulsifier Substances 0.000 description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 4
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- 230000009477 glass transition Effects 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
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- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000005639 Lauric acid Substances 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- NEYTXADIGVEHQD-UHFFFAOYSA-N 2-hydroxy-2-(prop-2-enoylamino)acetic acid Chemical group OC(=O)C(O)NC(=O)C=C NEYTXADIGVEHQD-UHFFFAOYSA-N 0.000 description 2
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 2
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- AGGIJOLULBJGTQ-UHFFFAOYSA-N sulfoacetic acid Chemical compound OC(=O)CS(O)(=O)=O AGGIJOLULBJGTQ-UHFFFAOYSA-N 0.000 description 1
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- NIAGBSSWEZDNMT-UHFFFAOYSA-M tetraoxidosulfate(.1-) Chemical compound [O]S([O-])(=O)=O NIAGBSSWEZDNMT-UHFFFAOYSA-M 0.000 description 1
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- UZNHKBFIBYXPDV-UHFFFAOYSA-N trimethyl-[3-(2-methylprop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)NCCC[N+](C)(C)C UZNHKBFIBYXPDV-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2623—Polyvinylalcohols; Polyvinylacetates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
- C04B24/383—Cellulose or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0042—Powdery mixtures
-
- 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
- C08F218/00—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 acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/26—Removing halogen atoms or halogen-containing groups from the molecule
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0045—Polymers chosen for their physico-chemical characteristics
- C04B2103/0054—Water dispersible polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0045—Polymers chosen for their physico-chemical characteristics
- C04B2103/0063—Polymers chosen for their physico-chemical characteristics obtained by an unusual polymerisation process, e.g. by changing the molar ratio of the different monomers during the polymerisation process
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00482—Coating or impregnation materials
- C04B2111/00508—Cement paints
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00663—Uses not provided for elsewhere in C04B2111/00 as filling material for cavities or the like
- C04B2111/00672—Pointing or jointing materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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Abstract
本发明提供了用于生产具有阳离子官能性的水可再分散聚合物粉末组合物的方法,其中在保护胶体和/或乳化剂存在下在水性介质中自由基聚合一种或多种烯键式不饱和单体,并且在作为干燥助剂的阳离子保护胶体的添加之后干燥产生的水性聚合物分散体,其特征在于,使用具有季铵卤化物基团的一种或多种阳离子单体的均聚物或共聚物作为阳离子保护胶体,其中基于聚合物粉末组合物的总重量,季铵卤化物基团中的按重量计50%至按重量计100%的卤素离子被非卤素阴离子交换,并且卤素离子的分数按重量计小于1%。
Description
技术领域
本发明涉及用于生产具有阳离子官能性(阳离子官能团,阳离子官能度,cationicfunctionality)的水可再分散聚合物粉末组合物的方法,涉及通过该方法可获得的具有阳离子官能性的水可再分散聚合物粉末组合物,并且涉及其用途。
背景技术
水可再分散聚合物粉末(分散体粉末)通常是在干燥助剂(通常为保护胶体)存在下通过相应的水性聚合物分散体的干燥获得的聚合物粉末。保护胶体部分的一个作用是防止聚合物颗粒在干燥操作过程中经历不可逆的结合,这是由于聚合物颗粒被保护胶体的水溶性颗粒包裹。当聚合物粉末分散在水中时,再溶解的这种保护胶体基质的第二作用是在水性再分散体中,聚合物颗粒再次以原始分散体的颗粒尺寸存在。
这种类型的分散体粉末尤其在化学建筑产品诸如干砂浆配方(dry mortarformulation)中使用,例如其通过水的添加准备使用。分散体粉末的添加改善了砂浆的加工性能并且导致了凝结砂浆中的较高的机械强度。
从现有技术中已经得知,在这些之中具有阳离子官能性的保护胶体可以用于制备水可再分散聚合物粉末。WO 00/05275 A1公开了一种方法,其中阳离子单体在水性介质中聚合,并且在这种情况下在原位形成的聚合物的存在下,聚合进一步的单体。然后,在聚乙烯醇存在下将因此获得的聚合物分散体喷雾干燥(spray-dried)。WO 00/05283 A1中描述了与这个类似的方法,在这种情况下方法被以这种方式控制以形成具有异构形态的共聚物颗粒。
EP 0770640 A2描述了通过水性聚合物分散体的干燥用于生产分散体粉末的方法。关键点在于水中的分散体中聚合物颗粒具有表面正电荷或表面负电荷并且使用干燥助剂(drying assistant)进行干燥,其中干燥助剂的电荷与水性聚合物分散体中聚合物颗粒的电荷相反。
WO 98/13411 A1描述了通过具有阴离子基团的乳液聚合物的喷雾干燥的聚合物粉末的生产,使用天然来源的两性聚合物(多糖,优选酪蛋白、明胶和蛋白质)或合成类型的两性聚合物(在侧链上具有叔或季铵基团的不饱和羧酸和丙烯酸酯的共聚物)。
WO 2007/093551 A1描述了在作为干燥助剂的阳离子保护胶体存在下通过干燥聚合物分散体获得的水可再分散聚合物粉末。使用的阳离子保护胶体是具有季铵基团和卤化物抗衡离子(平衡离子,counterion),更具体的为氯离子的单体的聚合物。与使用聚乙烯醇作为干燥助剂干燥的分散体粉末相比,这些粉末在砂浆化合物的生产中通过更好的加工性能进行区分。然而,因此获得的砂浆化合物的机械强度仍需要加强。
发明内容
因此,目的在于开发在用其改性的建筑材料中的具有改善的机械性能的阳离子聚合物粉末组合物,对于阳离子聚合物粉末组合物,可以在没有限制的情况下使用水溶性阳离子保护胶体。
本发明提供了用于生产具有阳离子官能性的水可再分散聚合物粉末组合物的方法,所述方法通过在水性介质中在保护胶体和/或乳化剂存在下自由基聚合一种或多种烯键式不饱和单体,并且在作为干燥助剂的阳离子保护胶体的添加之后干燥产生的水性聚合物分散体,其特征在于使用的所述阳离子保护胶体包括具有季铵卤化物基团的一种或多种阳离子单体的均聚物或共聚物,基于聚合物粉末组合物的总重量,通过非卤素阴离子取代季铵卤化物基团中的50wt%至100wt%的卤素离子,并且卤素离子的分数小于1wt%。
在这个方法中使用的阳离子保护胶体,其中通过非卤素阴离子取代季铵基团中基于具有季铵卤化物基团的一种或多种阳离子单体的均聚物或共聚物的50wt%至100wt%的卤素离子,并且基于聚合物粉末组合物的总重量在其用作干燥助剂时卤素离子的部分小于1wt%,阳离子保护胶体在下文中也称为低卤素阳离子保护胶体。
阳离子保护胶体适用于生产在例如E.W.Flick,Water-Soluble Resins-anIndustrial Guide,Noyes Publications,Park Ridge,N.J.,1991中描述的低卤素阳离子保护胶体。给予优选的是包括以下的组中的一种或多种阳离子单体的均聚物或共聚物:二烯丙基二甲基氯化铵(DADMAC)、二烯丙基二乙基氯化铵(DADEAC)、(3-甲基丙烯酰氧基)丙基三甲基氯化铵(MPTAC)、(2-甲基丙烯酰氧基)乙基三甲基氯化铵(METAC)、(3-甲基丙烯酰胺基)丙基三甲基氯化铵(MAPTAC)。
通常,基于阳离子保护胶体的总重量,阳离子保护胶体包括10至100wt%,优选50至100wt%,更优选60至100wt%,非常优选90至100wt%,最优选约100wt%的具有季铵基团的单体单元。适合的非离子、可共聚单体是在羧酸基团中具有1至15个C原子的乙烯基酯,诸如乙酸乙烯酯、丙酸乙烯酯、十二酸乙烯酯,丙烯酰胺,(甲基)丙烯酸羟基乙酯,(甲基)丙烯酸羟基丙酯,甲基丙烯酸和丙烯酸与具有4至13个C原子的醇的酯,具有C2至C4亚烷基单元且分子量为350至2000g/mol的聚亚烷基二醇(甲基)丙烯酸酯,并且也包括N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、丙烯酰氧基丙基三烷氧基-和甲基丙烯酰氧基丙基三烷氧基-硅烷诸如甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三烷氧基硅烷诸如乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷、以及乙烯基甲基二烷氧基硅烷诸如乙烯基甲基二甲氧基硅烷和/或所述非离子共聚单体的混合物。
可以通过本领域技术人员已知的聚合方法制备具有季铵基团的阳离子保护胶体,例如通过在水溶液中、在溶剂混合物中或在盐存在下的自由基聚合,包括例如沉淀聚合例如悬浮、或例如通过反相乳液聚合。在这些情况下,引发剂可以是水溶性的或油溶性的并且可以来自于过硫酸盐、过氧化物、偶氮类化合物以及氧化/还原引发剂对的组。尤其利用随后的反相乳液聚合或油包水聚合(water-in-oil polymerization)的方法,超高分子量阳离子聚合物实现为具有>5000000g/mol的分子量。
最优选的制备为在水溶性引发剂诸如偶氮类引发剂或氧化还原引发剂存在下,可选地在链转移剂诸如巯基丙酸或2-巯基乙醇存在下,通过具有低固体含量(优选≤40wt%)的水中的溶液聚合。
适合制备低卤素阳离子保护胶体的阳离子保护胶体也是可商购的。例如,以Catiofast BP(BASF)或C-592(Kemira,Water Solutions B.V)提供的聚二烯丙基二甲基氯化铵(聚-DADMAC)。
为了制备低卤素、阳离子保护胶体,可以通过本领域技术人员已知的方法来发生阳离子保护胶体中的卤素离子的减少。例如,通过DE 102005050201 B3已知的离子交换方法,诸如使用阴离子交换树脂的阴离子交换,或膜过滤方法,更特别地为纳米过滤。在纳米过滤方法的实例中,通过纳米过滤膜循环水性阳离子保护胶体溶液,并且以相同速率用含非卤素无机盐溶液提供含聚合物的保留物,在该速率下含卤素渗透物通过纳米过滤膜沉淀。例如,在这种情况下通常是氯的卤素离子由非卤素离子诸如硫酸根、硝酸根、乙酸根、硫代硫酸根或亚硫酸根取代。卤素离子优选由硫酸根或硫代硫酸根离子取代。通常,在每种情况下基于阳离子保护胶体中的卤素离子的总重量,50至100wt%的卤素离子,优选80至100wt%的卤素离子,更优选80至95wt%的卤素离子被取代。用于纳米过滤的阳离子聚合物溶液的粘度通常在从50至400mPas的范围内,优选在从70至150mPas的范围内(根据ISO2555,20rpm,23℃,具有推荐用于相应的粘度范围的转子的布氏粘度)。通过使用完全脱矿物质水的稀释,阳离子聚合物溶液的粘度可以调整为优选的粘度范围。
适合制备成膜类聚合物的水性聚合物分散体的单体是具有1至15个C原子的非支化或支化的烷基羧酸的乙烯基酯、具有1至15个C原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳烃、烯烃、二烯烃或乙烯基卤化物。
优选的乙烯基酯是乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、乙烯基-2-乙基己酸酯、月桂酸乙烯酯、乙酸1-甲基乙烯酯、三甲基乙酸乙烯酯和具有9至13个C原子的α-支化单羧酸的乙烯基酯,例如或(商品名Momentive)。特别优选的是乙酸乙烯酯。
优选的甲基丙烯酸酯或丙烯酸酯是丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯、丙烯酸降冰片酯。特别优选地为丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸正丁酯和丙烯酸2-乙基己酯。
烯烃和二烯烃的实例为乙烯、丙烯和1,3-丁二烯。适合的乙烯基芳烃是苯乙烯和乙烯基甲苯。优选的乙烯基卤化物是氯乙烯。
可选地,基于单体的总重量,还可以共聚0.05至50wt%,优选1至10wt%的辅助单体。辅助单体的实例是烯键式不饱和单羧酸和二羧酸,优选丙烯酸、甲基丙烯酸、富马酸和马来酸;烯键式不饱和甲酰胺和甲腈,优选丙烯酰胺和丙烯腈;富马酸和马来酸的单酯和二酯,诸如二乙基和二异丙基酯,以及马来酸酐,烯键式不饱和磺酸和/或其盐,优选乙烯基磺酸、2-丙烯酰胺基-2-甲基丙磺酸。其他实例是预交联的共聚单体诸如聚烯键式不饱和共聚单体,实例为己二酸二乙烯酯、马来酸二烯丙酯、甲基丙烯酸烯丙酯或氰尿酸三烯丙酯,或后交联共聚单体,实例为丙烯酰胺基乙醇酸(AGA)、甲基丙烯酰胺基乙醇酸甲酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺(NMMA)、N-羟甲基烯丙基氨基甲酸酯、烷基酯诸如N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、和N-羟甲基烯丙基氨基甲酸酯的异丁氧基醚或酯。环氧-官能的共聚单体也是适合的,诸如甲基丙烯酸缩水甘油酯和丙烯酸缩水甘油酯。其他实例是硅-官能的共聚单体,诸如丙烯酰氧基丙基三(烷氧基)-和甲基丙烯酰氧基丙基三(烷氧基)-硅烷诸如甲基丙烯酰氧基丙基三甲氧基硅烷,乙烯基三烷氧基硅烷和乙烯基甲基二烷氧基硅烷诸如乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷或乙烯基甲基二甲氧基硅烷,可以存在的烷氧基例如甲氧基、和乙氧基丙二醇醚基团。也可以提及具有羟基基团或CO基团的单体,实例为甲基丙烯酸和丙烯酸羟基烷基酯诸如丙烯酸羟基乙酯、丙烯酸羟基丙酯或丙烯酸羟基丁酯或甲基丙烯酸酯,以及化合物诸如双丙酮丙烯酰胺和丙烯酸乙酰乙酰氧基乙基酯或甲基丙烯酸酯。其他适合的共聚单体为例如乙烯基烷基醚,诸如乙烯基甲基醚、乙烯基乙基醚、乙烯基异丁基醚、乙烯基十八基醚。
适合作为基底聚合物的均聚物和共聚物的实例是乙酸乙烯酯均聚物、乙酸乙烯酯与乙烯的共聚物、乙酸乙烯酯与乙烯和一种或多种其他乙烯基酯的共聚物、乙酸乙烯酯与乙烯和丙烯酸酯的共聚物、乙酸乙烯酯与乙烯和氯乙烯的共聚物、苯乙烯-丙烯酸酯共聚物、苯乙烯-1,3-丁二烯共聚物。
给予优选的是乙酸乙烯酯均聚物;乙酸乙烯酯与1至40wt%的乙烯的共聚物;乙酸乙烯酯与1至40wt%的乙烯和1至50wt%的来自羧酸基团中具有1至15个C原子的乙烯基酯诸如丙酸乙烯酯、十二酸乙烯酯,具有9至13个C原子的α-支化羧酸的乙烯基酯诸如 的组中的一种或多种其他共聚单体的共聚物;乙酸乙烯酯与1至50wt%的来自羧酸基团中具有1至15个C原子的乙烯基酯诸如丙酸乙烯酯、十二酸乙烯酯,具有9至13个C原子的α-支化羧酸的乙烯基酯诸如的组中的一种或多种其他共聚单体的共聚物;乙酸乙烯酯、1至40wt%的乙烯、和优选1至60wt%的具有1至15个C原子的未支化或支化的醇的丙烯酸酯,更具体地,丙烯酸正丁酯或丙烯酸2-乙基己酯的共聚物;30至75wt%的乙酸乙烯酯、1至30wt%的月桂酸乙烯酯或具有9至13个C原子的α支化羧酸的乙烯基酯,以及1至30wt%的具有1至15个C原子的未支化或支化的醇的丙烯酸酯,更具体地,丙烯酸正丁酯或丙烯酸2-乙基己酯的共聚物,其可以可选地包括1至40wt%的乙烯;乙酸乙烯酯、1至40wt%的乙烯、和1至60wt%的氯乙烯的共聚物;一种或多种羧酸基团中具有1至12个C原子的乙烯基酯诸如乙酸乙烯酯,丙酸乙烯酯,月桂酸乙烯酯,具有5至13个C原子的α支化羧酸的乙烯基酯诸如VeoVa9R、VeoVa10R、VeoVa11R,1至40wt%的乙烯,和1至60wt%的氯乙烯的共聚物;其中在每种情况中陈述的辅助单体也可以以陈述的量聚合,并且其中在每种情况中以wt%表示的量加和为100wt%。
还给予优选的是(甲基)丙烯酸酯聚合物,诸如丙烯酸正丁酯或丙烯酸2-乙基己酯的共聚物或甲基丙烯酸甲酯与丙烯酸正丁酯和/或丙烯酸2-乙基己酯和可选的乙烯的共聚物;来自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸正丁酯、丙烯酸2-乙基己酯的组的一种或多种单体的苯乙烯-(甲基)丙烯酸酯共聚物;来自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸正丁酯、丙烯酸2-乙基己酯以及可选的乙烯的组的一种或多种单体的乙酸乙烯酯-(甲基)丙烯酸酯共聚物;苯乙烯和1,3-丁二烯的共聚物;其中在每种情况中陈述的辅助单体也可以以陈述的量聚合,并且其中在每种情况中以wt%表示的数加和为100wt%。
选择单体或选择共聚单体的重量分数,使得通常产生的玻璃化转变温度Tg是从–50℃至+50℃,优选–30℃至+10℃。可以通过差示扫描量热法(DSC)的已知的方式测量聚合物的玻璃化转变温度Tg。也可以预先使用Fox方程近似地计算Tg。根据Fox T.G.,Bull.Am.Physics Soc.1,3,page 123(1956),以下是正确的:1/Tg=x1/Tg1+x2/Tg2+...+xn/Tgn,其中xn表示单体n的质量分数(wt%/100),并且Tgn是以开尔文表示的单体n的均聚物的玻璃化转变温度。均聚物的Tg值在第二版聚合物手册(Polymer Handbook 2ndedition),J.Wiley&Sons,New York(1975)中列出。
优选通过乳液聚合方法制备均聚物和共聚物,聚合温度通常但不必须<100℃。
不依赖于聚合方法,可以在反应混合物的全部或某些成分包括在初始进料中的情况下,或反应混合物的成分或各个成分部分包括在初始进料中且部分随后量入的情况下,或通过量入方法而不存在初始进料在使用或不使用种子胶乳(seed latice)的情况下进行聚合。共聚单体可以全部包括在用于制备分散体的初始进料中(分批方法),或部分单体包括在初始进料中且剩余物计量入(半分批方法)。
使用习惯用于乳液聚合的水溶性引发剂或氧化还原引发剂组合引发聚合。水溶性引发剂的实例是过氧化焦硫酸(peroxodisulfuric acid)的钠、钾和铵盐、过氧化氢、叔丁基氢过氧化物、过氧化二磷酸钾、氢过氧化枯烯、单氢过氧化异丙基苯。在每种情况下基于单体的总重量,通常以0.001至0.02wt%,优选0.001至0.01wt%的量使用陈述的引发剂。使用的氧化还原引发剂是陈述的引发剂与还原剂的组合。合适的还原剂是碱金属的亚硫酸盐和重亚硫酸盐并且例如亚硫酸铵、亚硫酸钠,次硫酸的衍生物诸如锌或碱金属甲醛-次硫酸盐例如甲醛次硫酸氢钠(sodium hydroxymethanesulfinate),抗坏血酸以及2-羟基-2-亚磺酸基乙酸和2-羟基-2-磺酸基乙酸的盐与亚硫酸钠的混合物。在每种情况下基于单体的总重量,还原剂的量通常为0.001至0.03wt%,优选0.001至0.015wt%。
为了调整分子量,可以在聚合过程中加入链转移剂。如果使用这种试剂,基于待聚合的单体,它们通常采用0.01至5.0wt%之间的量,并且单独加入或以与反应组分的预混合物加入。这种试剂的实例是正十二烷基硫醇、叔十二烷基硫醇、巯基丙酸、巯基丙酸甲酯、异丙醇以及乙醛。
优选在非离子保护胶体存在下进行聚合。适合的非离子保护胶体是聚乙烯醇、聚乙烯醇缩醛、聚乙烯吡咯烷酮、水溶形式的多糖诸如淀粉(淀粉酶和支链淀粉)、纤维素和它们的甲基、羟乙基和/或羟丙基衍生物,以及聚(甲基)丙烯酰胺。
给予优选的是部分水解或完全水解的聚乙烯醇,其具有80至100mol%的水解度,更特别地,部分水解的聚乙烯醇具有80至95mol%的水解度,以及在4%浓度(强度,strength)的水溶液中的1至30mPas的郝普勒粘度(在20℃下的郝普勒方法,DIN53015)。还给予优选的是部分水解、疏水性的改性聚乙烯醇,其具有80至95mol%的水解度以及在4%浓度的水溶液中的1至30mPas的郝普勒粘度。它们的实例是部分水解的乙酸乙烯酯与疏水单体的共聚物,诸如乙酸异丙烯酯、新戊酸乙烯酯、乙基己酸乙烯酯、饱和的乙烯基酯、具有5或9至13个C原子的α-支化的单羧酸、二烷基马来酸酯和二烷基富马酸酯诸如马来酸二异丙基酯和富马酸二异丙基酯、氯乙烯、乙烯基烷基醚诸如乙烯基丁基醚,以及烯烃诸如乙烯和癸烯。基于部分水解的聚乙烯醇的总重量,疏水单元的分数优选0.1至10wt%。也可以使用所述聚乙烯醇的混合物。
最优选的是具有85至94mol%的水解度以及在4%浓度的水溶液中的3至15mPas的郝普勒粘度(在20℃下的郝普勒方法,DIN 53015)的部分水解的聚乙烯醇。陈述的保护胶体通过本领域技术人员已知的方法可获得,并且基于在聚合中单体的总重量通常以总计1至20wt%的量加入。
还可以可选地使用一种或多种非离子保护胶体与一种或多种低卤化物、阳离子保护胶体的混合物,在这种情况下,可以使用被认为是干燥助剂的低卤化物阳离子保护胶体。
还可以在非离子乳化剂存在下,或在结合有非离子乳化剂的陈述的非离子保护胶体存在下,或在结合有非离子乳化剂且结合有低卤化物阳离子保护胶体的陈述的非离子保护胶体存在下进行聚合。
适合的非离子乳化剂是表面活性剂,诸如具有8至40个氧化烯单元的烷基聚二醇醚或烷基芳基聚二醇醚。给予优选的是烷氧基化的C8至C16烷醇,其用C2至C4氧化烯,更特别地用氧化乙烯和氧化丙烯或它们的混合物烷氧基化。基于在聚合中单体的总重量,通常以0.05至10wt%的量添加非离子乳化剂。
优选在聚合过程中仅使用非离子保护胶体和/或非离子乳化剂。
在聚合结束后,可以使用已知的技术通过后聚合(通常通过使用氧化还原催化剂引发的后聚合)去除剩余的单体。也可以通过蒸馏,优选在减压的情况下,并且可选地使用通过或越过聚合批次的空气或蒸汽或惰性输送气诸如氮气去除挥发性的剩余单体。可获得的水性分散体因此具有30至75wt%,优选50至60wt%的固体含量。
为了生产具有阳离子官能性的水可再分散聚合物粉末,在作为干燥助剂的低卤化物、阳离子保护胶体的加入之后干燥水性聚合物分散体。在本文中,低卤化物阳离子保护胶体也与非离子保护胶体组合使用。适合于这个目的的非离子保护胶体是那些在上文中已经详细描述的在聚合中适合的非离子保护胶体。在这种类型的组合中,使用的非离子保护胶体优选包括具有80至95mol%水解度以及在4%浓度的水溶液中1至30mPas的郝普勒粘度(在20℃下的郝普勒方法,DIN 53015)的部分水解的聚乙烯醇,更优选具有85至94mol%水解度以及在4%浓度的水溶液中3至15mPas的郝普勒粘度(在20℃下的郝普勒方法,DIN53015)的部分水解的聚乙烯醇。在这种组合中,低卤化物阳离子保护胶体和非离子保护胶体之间的重量比可以为从90:10至10:90,优选从70:30至30:70。
通常而言,每种情况下基于分散体的聚合物成分,干燥助剂以总计0.1至20wt%,优选1至7wt%的量使用。
例如通过流化床干燥、冷冻干燥或喷雾干燥完成干燥。优选分散体是喷雾干燥的。这种喷雾干燥通常在喷雾干燥单元中进行,其中可以使用旋转盘或通过单流体、二流体或多流体喷嘴进行雾化。取决于干燥的单元和期望等级,出口温度通常选择在从45℃至120℃,优选60℃至90℃的范围内。
已经证明通常在干燥过程存在基于基底聚合物的高达2wt%的止泡剂是有利的。为了通过改善阻塞(blocking)稳定性增加保存期限,尤其在粉末具有低玻璃化转变温度的情况下,基于聚合物成分的总重量,产生的粉末可以提供有优选高达30wt%的防阻塞剂(抗凝剂)。防阻塞剂的实例是Ca和/或Mg的碳酸盐、滑石、石膏、二氧化硅、高岭土、偏高岭土和粒径优选在从10nm至100μm范围内的硅酸盐。
可以以这样一种方式通过固体含量调整用于雾化和用于干燥的混合物的粘性,所述方式给出了数字<1000mPas(在20旋转和23℃下的布氏粘度),优选<500mPas,尤其优选<250mPas。用于雾化的混合物的固体含量应该>30wt%,优选>40wt%。
为了改善性能属性,可以在干燥之前或期间或之后进行进一步的添加。包括在分散体粉末组合物的优选实施方式中进一步的成分是例如颜料、填料、发泡稳定剂、疏水剂和增塑剂。
根据本发明获得的具有阳离子官能性的水可再分散聚合物粉末组合物可以用于这些组合物的典型的应用领域。也可以使用具有阳离子官能性的分散体粉末与传统分散体粉末的共混物。
应用的实例是在化学建筑产品中的那些,可选地与液压设置粘合剂诸如水泥(波特兰水泥、高氧化铝水泥、火山土水泥、高炉水泥、氧化镁水泥和磷酸盐水泥)、石膏和水玻璃组合,用于建筑粘合剂尤其是瓷砖粘合剂(例如高弹性粘合剂)和用于外部绝缘和精加工系统(finishing system)的粘合剂,以及抹灰(render)、填充化合物、地板填充化合物、流平化合物(leveling compound)、水泥浆(grout)、接合砂浆和油漆的生产。应用优选的领域为水泥浆和瓷砖粘合剂,特别地包括用于木质衬底的瓷砖粘合剂。通过在粘合剂和涂料行业中的用途带来其他可能的应用,后者例如用于纸和纺织品。
令人惊讶地发现,这些具有阳离子官能性的水可再分散聚合物粉末组合物的用途导致在机械性能中显著的改善,例如以水泥浆作为实施例的示出。
具体实施方式
实施例:
下文中的那些描述了用于生产本发明的聚合物粉末的起始分散体和保护胶体。
低卤化物阳离子保护胶体(PC1)的制备:
使用的起始材料是来自Kemira,Water Solutions B.V的C-592,39wt%浓度的聚二烯丙基二甲基氯化铵的水溶液,其具有22wt%的氯化物含量。使用完全去矿物质水将39wt%浓度的水溶液稀释至10wt%。为了减少氯离子,使用纳米过滤膜(Semicon,Nitto Denko NTR-7450HG F4T)进行膜过滤。在10%浓度的硫代硫酸钠溶液存在下,水溶液通过前述纳米过滤膜(保留物)循环,并且去除的渗透物的量以完全去矿物质水的形式回到循环中。继续膜过滤直到通过使用硫代硫酸根离子取代氯离子将聚二烯丙基二甲基氯化铵中的氯化物含量减少至4.4wt%。通过这个方式氯离子的分数减少了80wt%。然后,进行离子交换过程,仅通过渗透物的去除,保留物的浓度增加至20wt%,但是完全去矿物质的水并未返回至循环。
分散体A:
使用基于单体总重量的6wt%的具有88mol%水解度以及在4%浓度的水溶液中的4mPas的郝普勒粘度的聚乙烯醇制备基于乙酸乙烯酯-乙烯共聚物的水性聚会物分散体,其中聚合物分散体固体含量为53%且Tg为-6℃。
分散体B:
使用基于单体总重量的5wt%的具有88mol%水解度以及在4%浓度的水溶液中的4mPas的郝普勒粘度的聚乙烯醇制备基于乙酸乙烯酯-乙烯-VeoVa10共聚物的水性聚合物分散体,其中聚合物分散体固体含量为50%且Tg为-15℃。
分散体C:
使用基于单体总重量的5.5wt%的具有88mol%水解度以及在4%浓度的水溶液中的4mPas的郝普勒粘度的聚乙烯醇与基于单体总重量的0.5wt%(干分数)的保护胶体PC1制备基于乙酸乙烯酯-乙烯共聚物的水性聚合物分散体,其中聚合物分散体固体含量为53%且Tg为-5℃。
保护胶体-PC1:
具有4.4wt%的氯离子分数以及在4%浓度的水溶液中7mPas的郝普勒粘度的20%浓度的聚二烯丙基二甲基氯化胺的水溶液。
保护胶体-PC2:
具有88mol%的水解度以及在4%浓度的水溶液中4mPas的郝普勒粘度的水性聚乙烯醇溶液。
保护胶体-PC3:
具有88mol%的水解度以及在4%浓度的水溶液中13mPas的郝普勒粘度的水性聚乙烯醇溶液。
保护胶体-PC4:
具有22wt%的氯离子分数以及在4%浓度的水溶液中12.2mPas的郝普勒粘度的39%浓度的聚二烯丙基二甲基氯化胺的水溶液(来自Kemira的C-592,水溶液B.V)。
实施例1至6:
根据表1中表明的量(干重),将初始分散体A至C分别与保护胶体PC1至PC3混合,且加入基于分散体的固体分数的0.3wt%的消泡剂(来自瓦克化学的Silfoam S860),并且搅拌产生的混合物30分钟并过滤。在实施例1至6的任何一个中均未形成凝结物。将混合物与添加的基于分散体的固体分数的15wt%的防阻塞剂(碳酸钙,Omyacarb 5GU)一起喷射干燥。
比较例7:
根据表1中表明的量(干重)将初始分散体A与保护胶体PC4混合,且加入基于分散体的固体分数的0.3wt%的消泡剂(Silfoam S860),并且搅拌产生的混合物30分钟并过滤。将混合物与添加的基于分散体的固体分数的15wt%的防阻塞剂(碳酸钙,Omyacarb 5GU)一起喷射干燥。
表1:粉末组合物
测试:
对获得的粉末分别进行它们的粉末性能和加工为水泥浆的研究。
阻塞分数(blocking score)的测定:
为了测定抗阻塞性(blocking resistance),将分散体粉末引入至具有螺旋闭合(screw closure)的铁管内,并且然后负载金属模具。粉末在负载下储存在50℃的干燥柜中16小时。在冷却到室温之后取出,从管中移出粉末并且通过粉碎粉末定性地测定阻塞稳定性。阻塞稳定性的分级如下:
1=非常好的阻塞稳定性,没有粉碎
2=良好的阻塞稳定性
3=满意的阻塞稳定性
4=不稳定阻塞,在粉碎后粉末不再自由流动。
沉降性能(管沉降)的测定:
再分散体的沉降性能作为粉末的再分散性的测量。使用水中各自的50wt%的分散体粉末通过暴露于强剪切力下产生再分散体。然后在每种情况下使用稀释的再分散体(0.5wt%的固体含量)测定沉降性能。将100ml的每种这些再分散体引入至刻度管中并且测量固体的沉降高度。在1小时后和在24小时之后,以mm沉降记录数字。在1小时之后大于1mm的数字和在24小时之后大于3的数字表示不充分的聚合物粉末的再分散体。
分散体粉末的阻塞分数和管沉降的测试结果在表2中总结。
表2:粉末性能
对于胶凝水泥浆的生产,采用以下配方:
在下列储存条件(DIN CEN 1897)之后,在每种情况下测试组件中的拉伸粘结强度(tensile bond strength)(TBS):
28天的23℃和50%空气湿度的标准-条件储存(28天SC)=干,
7天的标准-条件储存和21天的23℃的湿储存(7天SC+21天水)=湿
根据EN 1348进行测试。为了这个目的,在每种情况下,使用喷标(stencil)(50mm直径,10mm厚度)将砂浆应用于混凝土板,并且如前文指示的储存测试样本。然后,为了进行拉伸粘附测试,使用环氧粘合剂、金属拉伸锚粘附至测试下的砂浆层。使用来自Herion的具有250N/s的负载增速的拉伸装置。由5次测量的平均值以N/mm2表示测量值。
在28天的23℃和50%空气湿度的标准-条件储存(28天SC)=干,7天的标准-条件储存和21天的23℃的湿储存(7天SC+21天H2O)=湿之后,在每种情况下,根据DIN ISO 527使用50mm/min的拉伸速率,使用标准试样3(1B)进行来自拉伸测试的拉伸强度(TS)和拉伸伸长率(TE)的测定。
在表3中再现了组件中的拉伸粘附强度、拉伸强度和拉伸伸长率的结果。
表3:水泥浆中的性能特性
给出的实施例的结果示出了通过使用低卤化物、阳离子保护胶体,获得了聚合物粉末,其对阻塞是稳定的且容易再分散在水中(表2)。此外,令人惊讶地发现本发明的聚合物粉末组合物产生了改善的机械性能:在表3中实施例1与比较例7的比较。
特别地在湿储存后,改善的机械性能是明显的。使用低卤化物阳离子保护胶体与聚乙烯醇的组合作为干燥助剂获得了进一步的改善:实施例1与实施例2的比较。
Claims (11)
1.一种用于生产具有阳离子官能性的水可再分散聚合物粉末组合物的方法,所述方法通过在保护胶体和/或乳化剂存在下在水性介质中自由基聚合一种或多种烯键式不饱和单体并且在添加阳离子保护胶体作为干燥助剂之后干燥产生的水性聚合物分散体来进行,其特征在于,使用的所述阳离子保护胶体包括具有季铵卤化物基团的一种或多种阳离子单体的均聚物或共聚物,其中,所述季铵卤化物基团中的50wt%至小于100wt%的卤素离子被非卤素阴离子取代,并且其中,基于所述聚合物粉末组合物的总重量,所述卤素离子的分数小于1wt%。
2.根据权利要求1所述的方法,其特征在于,使用的所述阳离子保护胶体包括来自包含以下的组的一种或多种阳离子单体的均聚物或共聚物:二烯丙基二甲基氯化铵、二烯丙基二乙基氯化铵、(3-甲基丙烯酰氧基)丙基三甲基氯化铵、(2-甲基丙烯酰氧基)乙基三甲基氯化铵、(3-甲基丙烯酰胺基)丙基三甲基氯化铵。
3.根据权利要求1所述的方法,其特征在于,基于所述阳离子保护胶体的总重量,所述阳离子保护胶体包括至少10wt%的具有季铵卤化物基团的单体单元。
4.根据权利要求1至3中任一项所述的方法,其特征在于,在每种情况下,基于所述阳离子保护胶体中的所述卤素离子的总重量,所述卤素离子的80至小于100wt%被非卤素阴离子取代。
5.根据权利要求1至3中任一项所述的方法,其特征在于,在每种情况下,基于所述分散体的聚合物成分,以0.1至20wt%的量使用所述干燥助剂。
6.根据权利要求1至3中任一项所述的方法,其特征在于,将所述阳离子保护胶体用作唯一的干燥助剂。
7.根据权利要求1至3中任一项所述的方法,其特征在于,使用阳离子保护胶体和非离子保护胶体的组合,所述组合具有90:10至10:90的阳离子保护胶体与非离子保护胶体的重量比。
8.根据权利要求1至3中任一项所述的方法,其特征在于,使用来自包括以下的组的一种或多种烯键式不饱和单体来制备所述水性聚合物分散体:具有1至15个C原子的非支化或支化的烷基羧酸的乙烯基酯、具有1至15个C原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳烃、烯烃、二烯烃以及乙烯基卤化物。
9.一种具有阳离子官能性的水可再分散聚合物粉末组合物,通过根据权利要求1至8中任一项所述的方法来生产。
10.根据权利要求9所述的具有阳离子官能性的水可再分散聚合物粉末组合物在用于生产建筑粘合剂、抹灰、填充化合物、流平化合物、水泥浆、接合砂浆和油漆的化学建筑产品中的用途。
11.根据权利要求10所述的用途,其中填充化合物是地板填充化合物。
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