CN102791799A - 硅树脂乳液及其在疏水熟石膏中的用途 - Google Patents
硅树脂乳液及其在疏水熟石膏中的用途 Download PDFInfo
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Classifications
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- 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
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
-
- 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
- C04B28/14—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 calcium sulfate cements
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
- C08J2383/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
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- Dispersion Chemistry (AREA)
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Abstract
本发明涉及硅树脂乳液(SE),其可通过以下方法得到,其中,第一步包括将100重量份的通式I的烷基三烷氧基硅烷与0-5重量份的通式II的烷基烷氧基硅烷、400-2500重量份的水和5-50重量份的乳化剂在10-100℃下混合,其中产生醇,在第二步中,将第一步的产物醇馏出,直到总醇含量最大为0.5wt%,其中在权利要求1中描述了通式I的烷基三烷氧基其中由包括通式III、IV、V、VI、和VII的单元的H-硅氧烷和硅树脂乳液(SE)处理石膏,其中在权利要求4中描述了通式III、IV、V、VI、和VII的单元。
Description
本发明涉及硅树脂乳液,以及使石膏疏水的方法,其中用H-硅氧烷和硅树脂乳液处理石膏。
含有两个或多个直接附着在硅上的氢原子的硅氧烷(H-硅氧烷),尤其是多甲基氢硅氧烷,非常适于石膏的疏水化。这是所有试剂当中最有效的,即,通过添加非常少的量得到非常良好的疏水性,通常利用量为0.2-0.6%。由于所述含H产物的量受合成需要的Müller-Rochow法硅烷的限制,因此需要寻找替代方案。
石膏的疏水化在建筑产品化学中是典型的情况。在Linda Jakobsmeier的论文(Munich Technical University,2000)中对石膏疏水化做了深入的描述。多甲基氢硅氧烷和三甲氧基甲基硅烷的效果被详细报道。三甲氧基甲基硅氧烷是不利的,因为其形成甲醇。
DE 10220659 A描述了通过添加淀粉醚而改善H-硅氧烷的憎水效果。
H-硅氧烷的憎水效果同样可以通过添加碱性化合物而改善。这通常引起与其他石膏板成分的不相容。在碱性区域中脱附氢使得增加安全要求成为必要。
多甲基氢硅氧烷的水乳液也用于石膏的疏水化。
EP 1083157 A描述了由有机氢硅氧烷、聚乙烯醇、水和含氨基官能团的化合物组成的乳液,所述含氨基官能团的化合物例如为氨基硅烷或有机胺。
US 2007022913 A描述了由石膏、作为非常昂贵催化剂的粉煤灰、氧化镁和水与无溶剂的甲基氢硅氧烷的乳液的石膏浆体。
DE 19517346 A描述了有机硅化合物的乳液,尤其是含有烷氧基的有机硅化合物的乳液。其指出了烷氧基硅烷的乳液的弱的储存稳定性和减低的疏水效果。例如在DE 19707219和DE 19904496中也探讨了甲氧基硅烷的应用。
例如,US 5776245声明,乳化剂的存在不利于疏水效果。
本发明解决的问题是提供有机氢化聚硅氧烷的替代品用于石膏的疏水化。
本发明提供硅树脂乳液(SE),其通过一种方法得到,在该方法中第一步包括将100重量份的通式I的烷基三烷氧基硅烷
R(R1O)3Si (I),
与0-5重量份的通式II的烷基烷氧基硅烷
R′a(R1’O)bSi (II),
与400-2500重量份的水和
5-50重量份的乳化剂在10-100℃下混合,形成醇R1OH,具有或没有R1′OH,第二步包括将第一步的产物醇R1OH和任选存在的R1′OH蒸馏出,直到总醇含量不超过0.5wt%,其中
R和R′是1-10个碳原子的烷基部分,
R1和R1′是1-6个碳原子的烷基部分,
a是0、1、2或3,和
b是1、2、3或4。
本发明还提供一种用于石膏疏水化的方法,所述方法包括用由通式III、IV、V、VI、和VII的单元构造的H-硅氧烷和上述硅树脂乳液(SE)处理石膏:
R3 3SiO1/2 (III),
R3HSiO2/2 (IV),
R3 2SiO2/2 (V),
R3SiO3/2 (VI),
SiO4/2 (VII),
其中
R3代表1-10个碳原子的烷基部分。
在石膏的疏水化中,硅树脂乳液(SE)不仅替代一些H-硅氧烷,而且相比于单独使用H-硅氧烷,在硅树脂乳液(SE)中明显更少量的硅树脂(S)足以达到相当或高出的石膏疏水化。存在协同效应。
与甲基三甲氧基硅烷的浓乳液或完全水解产物不同,硅树脂乳液(SE)在数月的储存时间后仍保留其石膏疏水能力。令人惊奇的是,储存数月的硅树脂乳液(SE)与H-硅氧烷组合使用,产生显著的石膏疏水化效果。由于含有乳化剂得到的石膏疏水性通过乳化的硅树脂的疏水效应而被强烈地超补偿。
硅树脂乳液(SE)用于使石膏疏水化的应用是不干扰环境的,因为醇的残留量很小。
烷基部分R和R′各自优选具有1-6个碳原子,特别优选乙基和甲基。
烷基部分R1和R1’各自优选具有1-3个碳原子,特别优选乙基和甲基。
本方法优选使用不超过2重量份的通式II的烷基烷氧基硅烷,本方法更优选使用不超过0.5重量份的通式II的烷基烷氧基硅烷,本方法尤其优选不使用通式II的烷基烷氧基硅烷。
用于本方法的水的量优选不少于500重量份,更优选不少于600重量份,和不超过2000重量份,更优选不超过900重量份。
在本方法中使用的乳化剂的量优选不少于10重量份,更优选不少于15重量份,和不超过50重量份,更优选不超过30重量份。
实施本方法的温度优选不低于15℃和不超过95℃,更优选不超过50℃。本方法设定的含水量越高,允许的温度越高。
混合步骤优选进行不少于10分钟,更优选进行不少于30分钟。在至多50℃下,反应时间至少为30分钟且不超过2小时。温度越高,相应方式下的反应时间越短。
在第一步末端形成的乳化的硅树脂(S)的水平优选不低于乳液的2wt%,更优选不低于4wt%和尤其不低于5wt%,和不超过10wt%,优选不超过8wt%。
在第二步中的蒸馏优选实施到总醇含量不超过0.1wt%,更优选不超过0.01wt%,尤其不超过0.001%。
蒸馏用于降低含水量以及去除醇。可以设定乳液期望的浓度,过量的水重新用于乳液生产。
当蒸馏步骤被再分成两个或多个阶段时,对于硅树脂乳液(SE),得到特别良好的储存稳定性。第一阶段优选在不低于93℃的温度下实施,尤其不低于95℃,优选不超过105℃,更优选不超过102℃,和尤其不超过100℃。在此选择压力以确定期望的温度。压力优选为900-1000mbar。
第二阶段优选在不低于20℃下实施,更优选不低于30℃和尤其不低于40℃,并且优选不超过70℃,更优选不超过60℃和尤其不超过50℃。在此选择压力以确定期望的温度。压力优选为1-100mbar。
当还有其他蒸馏阶段时,优选选择第二阶段的优选范围的压力条件。
两个或多个阶段中的蒸馏为硅树脂乳液(SE)提供总计至少一年的储存稳定性。
蒸馏,尤其在第一蒸馏阶段中,能够回收绝大多数醇R1OH和任选存在的R1′OH。
可以使用任何适合生产硅树脂乳液的乳化剂。
适合的阴离子乳化剂特别是:
1.烷基硫酸盐,特别是具有8-18个碳原子的链长的那些,疏水部分中具有8-18个碳原子和1-40个亚乙基氧(EO)和/或亚丙基氧(PO)单元的烷基和烷芳基醚硫酸盐。
2.磺酸盐,特别是具有8-18个碳原子的烷基磺酸盐,具有8-18个碳原子的烷基芳基磺酸盐,氨基乙磺酸盐(taurides),磺基琥珀酸与一元醇或具有4-15个碳原子的烷基酚的酯或单酯;所述醇或烷基酚可以任选地还用具有1-40个EO单元乙氧基化。
3.在烷基、芳基、烷芳基或芳烷基部分中具有8-20个碳原子的羧酸的碱金属盐和铵盐。
4.磷酸偏酯及其碱金属和铵盐,特别是在有机部分中具有8-20个碳原子的烷芳基磷酸盐、在烷基或分别在烷芳基部分中具有8-20个碳原子和1-40个EO单元的烷基醚或烷芳基醚磷酸盐。
适合的非离子乳化剂特别是:
5.聚乙烯醇,优选仍含有5-50%,尤其是8-20%的醋酸乙烯酯单元的聚乙烯醇,优选的聚合度为500-3000。
6.烷基聚乙二醇醚,尤其是具有8-40个EO单元和8-20个碳原子的烷基的那些。
7.烷基芳基聚乙二醇醚,优选具有8-40个EO单元和在烷基和芳基部分中8-20个碳原子的那些。
8.环氧乙烷-环氧丙烷(EO-PO)嵌段共聚物,优选具有8-40个EO和/或PO的那些。
9.具有8-22个碳原子的烷基的烷基胺与环氧乙烷或环氧丙烷的加成产物。
10.6-24个碳原子的脂肪酸。
11.通式为R*-O-Zo的烷基多糖苷(polyglycoside),其中R*是直链或支化的、饱和或不饱和的具有8-24个碳原子的烷基,Zo是具有平均o=1-10的己糖或戊糖单元或其混合物的寡糖苷部分。
12.天然产物及其衍生物,如卵磷脂、羊毛脂、皂甙、纤维素;纤维素烷基醚和羧烷基纤维素,其每个烷基具有至多4个碳原子。
13.含有极性基团的直链有机(聚)硅氧烷,尤其是包含具有至多24个碳原子的烷氧基和/或至多40个EO和/或PO基团的那些直链有机(聚)硅氧烷。
适合的阳离子乳化剂特别为:
14.8-24个碳原子的伯、仲和叔脂肪胺与醋酸、硫酸、盐酸和磷酸的盐。
15.烷基和烷基苯季铵盐,尤其是烷基具有6-24个碳原子的那些,尤其是卤化物、硫酸盐、磷酸盐和醋酸盐。
16.烷基吡啶鎓盐、烷基咪唑鎓盐和烷基噁唑盐,尤其是烷基链具有至多18个碳原子的那些,尤其是卤化物、硫酸盐、磷酸盐和醋酸盐。
适合的两性乳化剂特别为:
17.具有长链取代基的氨基酸,如N-烷基二(氨基乙基)甘氨酸或N-烷基-2-氨基丙酸盐。
18.甜菜碱,如具有C8-C18酰基的N-(3-酰氨基丙基)-N,N-二甲基铵盐和烷基咪唑鎓甜菜碱。
特别优选非离子乳化剂,尤其是聚乙烯醇。
可用于石膏的疏水化的H-硅氧烷优选具有通式VIII
R3 3SiO(R3HSiO)x(R3 2SiO)ySiR3 3 (VIII)
其中R3如上所限定,
x是10-200的整数,和
y是0-100的整数。
x优选不小于20,更优选不小于30和尤其不小于40,优选不超过150,更优选不超过100和尤其不超过70。
y优选不超过50,更优选不超过20和尤其不超过5。在一个特别优选情况下,y是0。
在石膏的类型中,优选熟石膏(CaSO4·0.5H2O),例如以煅烧石膏、灰泥石膏、造型石膏或绝热石膏的形式。其他类型的石膏,如地板石膏、金纳水泥、无水石膏和烟道气脱硫硫酸钙也是非常适合的。石膏可以含有添加剂,以利于锐利(sharped)石膏制品的生产,并改善锐利石膏制品的性能。添加剂包括,例如填料,如二氧化硅和纤维素纤维,增速剂,如硫酸钾和硫酸铝,延迟剂,如蛋白质或酒石酸盐,石膏体增塑剂,如木质素磺酸盐,和纸板的粘合促进剂,如淀粉。
每100重量份的通式III的H-硅氧烷中,优选使用含有不低于5,更优选不低于10和尤其不低于15重量份且不超过60,更优选不超过50和尤其不超过30重量份的乳化的硅树脂(S)作为活性成分的硅树脂乳液(SE)的量处理石膏。上述活性成分含量也提供特别储存稳定的硅树脂乳液(SE)。
每100重量份的石膏,优选使用不少于0.05和更优选不少于0.1重量份且不超过1和更优选不超过0.5重量份的H-硅氧烷处理石膏。
优选使用无溶剂形式的H-硅氧烷处理石膏,但是也可以用溶剂稀释。
H-硅氧烷和硅树脂乳液(SE)优选彼此分开储存。其优选在疏水化之前连续添加到石膏中或立即混合。
石膏疏水化优选作为大量疏水化实施。当为此而将石膏、H-硅氧烷和硅树脂乳液(SE)合并成可成形组合物时,必须添加水。优选每100重量份的石膏添加30-140和尤其是50-100重量份的水。
在一个优选实施方案中,制备的石膏体含有石膏、水、H-硅氧烷和硅树脂乳液(SE)。所述石膏体还可以通过混入空气而膨胀成石膏泡沫。
石膏体可以成形,以制备成形的石膏制品。
在成形后、固化后或甚至干燥后,成形的石膏制品也可以用H-硅氧烷和硅树脂乳液(SE)给予疏水处理。处理可以采用如下形式,例如用硅树脂乳液(SE)和H-硅氧烷浸渍、喷涂或刷涂。
成形的石膏制品的实例为石膏板面板,如墙板面板或石膏-纸张石膏板面板。
所有上述通式中的上述标记各自具有其彼此独立的意义。在所有式中,硅原子是四价的。
在以下实施例中,除非在各自情况下另外说明,所有量和百分数以重量计,所有压力为0.10MPa(abs.),和所有温度为20℃。
制备水性、无溶剂的甲基树脂乳液(SE)
在配有搅拌器和蒸馏头的1.5L反应烧瓶中,初始在搅拌下加入600g水和90g的20%聚乙烯醇溶液。于30min内,计量加入102g甲基三甲氧基硅烷至该液体中,而后在室温下再搅拌两小时。水解结束后的活性成分浓度为6.3wt%。
随后启动2-阶段蒸馏。第一阶段在93℃-99℃下进行,第二阶段在45℃和50mbar下进行。
依据两阶段的馏出物量,得到的活性成分(甲基树脂)和乳化剂(聚乙烯醇)的浓度如下:
200g馏出物→8.5%甲基树脂,3%乳化剂
400g馏出物→12.8%甲基树脂,4.6%乳化剂
500g馏出物→17.2%甲基树脂,6.2%乳化剂
乳液能够稳定储存超过一年,不会改变其石膏疏水性。
甲基树脂乳液(SE)在石膏疏水化中的应用
石膏物质制品的生产如下:
将80重量份的部分无离子水、通式(CH3)3SiO((CH3)HSiO)xSi(CH3)3x48-55的H-硅氧烷和甲基树脂乳液在1000rpm下搅拌混合120s。而后,添加100重量份的造型石膏,继续再搅拌120s。
将得到的石膏体倒入PVC模具中,形成直径8cm、高2cm的样品盘。在20℃下储存1小时后,将凝固的样品脱模。样品首先在40℃下垂直干燥24小时,而后在20℃下储存3天。
而后依据DIN 18180测定吸水量(water imbition)。将样品水平浸渍在23℃的水中,以使2cm的水柱高于样品表面。浸渍在水中两小时后,从水中取出样品,去除附着在表面上的水,称重确定增重。
由于石膏疏水效果基本上非常依赖于石膏的性质,因此也进行了纯粹用H-硅氧烷的测定,作为系列测试的一部分。表中报告的值通常是重复测定的结果。
实施例报告了每100重量份的造型石膏中使用的H-硅氧烷和甲基树脂乳液的量。
实施例1:使用石膏批次A(造型石膏)的测试系列
作为对比,即非依据本发明,测试T1包含添加0.4重量份的H-硅氧烷。
依据本发明,测试T2-T8包含添加0.2重量份的H-硅氧烷和0.2重量份的甲基树脂乳液。
表1报告了甲基树脂乳液中的甲基树脂、乳化剂和总固体的水平,以及T1-T8测试的DIN 18180吸水量。
表1:
*非依据本发明
实施例2:使用石膏批次B(造型石膏)的测试系列
作为对比,即非依据本发明,测试T9包含添加0.4重量份的H-硅氧烷。
依据本发明,测试T10i-T12i包含添加0.2重量份的H-硅氧烷和0.2重量份的甲基树脂乳液。甲基树脂乳液各自含有0.5%的醋酸。
表2报告了甲基树脂乳液中的甲基树脂、乳化剂和总固体的水平,以及T9和T10i-T12i测试的DIN 18180吸水量。
表2:
*非依据本发明
实施例3:使用石膏批次C(造型石膏)的测试系列
作为对比,即非依据本发明,测试T13包含添加0.4重量份的H-硅氧烷。
依据本发明,测试T14-T22包含添加0.2重量份的H-硅氧烷和表3中报告的重量份的甲基树脂乳液。
表3报告了甲基树脂乳液中的甲基树脂、乳化剂和总固体的水平,以及T13-T22测试的DIN 18180吸水量。
表3:
*非依据本发明
所有依据本发明的测试显示与改进的疏水化相匹配的H-硅氧烷的显著节省。
乳液的浓度越高,石膏疏水化需要的用量越少。然而,较高的浓度与粘度的明显升高相关,这样存在较大分子导致石膏疏水功能降低或丧失的风险。那么乳液早已乳脂化,其不利于量取。
Claims (8)
1.通过以下方法得到的硅树脂乳液(SE),所述方法中,第一步包括将100重量份的通式I的烷基三烷氧基硅烷
R(R1O)3Si (I),
与0-5重量份的通式II的烷基烷氧基硅烷
R′a(R1’O)bSi (II),
400-2500重量份的水和
5-50重量份的乳化剂在10-100℃下混合,形成醇R1OH与R1′OH,或没有R1′OH,第二步包括将第一步的产物醇R1OH和任选存在的R1′OH蒸馏出,直到总醇含量不超过0.5wt%,其中
R和R′是1-10个碳原子的烷基部分,
R1和R1′是1-6个碳原子的烷基部分,
a是0、1、2或3,和
b是1、2、3或4。
2.权利要求1的硅树脂乳液(SE),其中烷基部分R、R′、R1和R1是甲基。
3.权利要求1或2的硅树脂乳液(SE),其中在合成中的蒸馏步骤分为两个或多个阶段,第一阶段在不低于93℃的温度下进行。
4.一种使石膏疏水化的方法,所述方法包括用
由以下通式III、IV、V、VI、和VII的单元构造的H-硅氧烷和权利要求1、2或3的硅树脂乳液(SE)处理石膏:
R3 3SiO1/2 (III),
R3HSiO2/2 (IV),
R3 2SiO2/2 (V),
R3SiO3/2 (VI),
SiO4/2 (VII),
其中,
R3代表1-10个碳原子的烷基部分。
5.权利要求4的方法,其中每100重量份的通式III的H-硅氧烷所用硅树脂乳液的量含有5-60重量份的乳化的硅树脂(S)作为活性成分。
6.权利要求4或5的方法,其中每100重量份的石膏使用0.05-0.5重量份的H-硅氧烷。
7.权利要求4、5或6的方法,其中所述石膏的疏水化是大量疏水化。
8.权利要求7的方法,其中制备的石膏体含有石膏、水、H-硅氧烷和硅树脂乳液(SE)。
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DE102009047582A DE102009047582A1 (de) | 2009-12-07 | 2009-12-07 | Siliconharzemulsion und deren Einsatz bei der Hydrophobierung von Gips |
DE102009047582.6 | 2009-12-07 | ||
PCT/EP2010/068310 WO2011069843A1 (de) | 2009-12-07 | 2010-11-26 | Siliconharzemulsion und deren einsatz bei der hydrophobierung von gips |
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EP (1) | EP2510057A1 (zh) |
JP (1) | JP5279957B2 (zh) |
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CN111116917A (zh) * | 2019-12-18 | 2020-05-08 | 宁波辉宏新材料有限公司 | 一种乳液聚合法合成乳液型mdq硅树脂的方法 |
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US20150274970A1 (en) * | 2014-03-26 | 2015-10-01 | Wacker Chemical Corporation | Control of internal viscosity in in situ polymerized organopolysiloxane emulsions |
EP3656804A1 (en) * | 2015-06-29 | 2020-05-27 | KCC Corporation | Waterproof silicone emulsion, waterproof board exhibiting excellent crack resistance |
EP3707107B1 (de) * | 2018-01-19 | 2021-06-16 | Wacker Chemie AG | Alkylsiliconharz als additiv zur hydrophobierung von faserzement |
CN111410860A (zh) * | 2019-01-08 | 2020-07-14 | 疏科纳米疏水科技(嘉兴)有限公司 | 制备超疏水墙体装修用材料的方法 |
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JP2831877B2 (ja) * | 1992-06-23 | 1998-12-02 | 東芝シリコーン株式会社 | エマルジョン組成物 |
US5300327A (en) * | 1993-03-22 | 1994-04-05 | Dow Corning Corporation | Water repellent organosilicon compositions |
DE19517346A1 (de) | 1995-05-11 | 1996-11-14 | Wacker Chemie Gmbh | Emulsionen von Organosiliciumverbindungen für die Hydrophobierung von Baustoffen |
GB9605706D0 (en) | 1996-03-19 | 1996-05-22 | Dow Corning | Method for hydrophobing gypsum |
DE19707219A1 (de) | 1997-02-24 | 1998-08-27 | Wacker Chemie Gmbh | Wäßrige Dispersionen für die Behandlung saugfähiger Materialien zum Schutz gegen Verschmutzung |
DE19904496A1 (de) | 1999-02-04 | 2000-08-10 | Wacker Chemie Gmbh | Wäßrige Cremes von Organosiliciumverbindungen |
US6106607A (en) | 1999-09-10 | 2000-08-22 | Dow Corning Corporation | Composition for hydrophobing gypsum and methods for the preparation and use thereof |
DE10220659A1 (de) | 2002-05-09 | 2003-11-27 | Wacker Chemie Gmbh | Behandlung von Gips mit H-Siloxan und Stärkeether |
US7803226B2 (en) | 2005-07-29 | 2010-09-28 | United States Gypsum Company | Siloxane polymerization in wallboard |
JP2007084668A (ja) * | 2005-09-21 | 2007-04-05 | Sumitomo Seika Chem Co Ltd | 有機ケイ素化合物エマルション |
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CN111116917A (zh) * | 2019-12-18 | 2020-05-08 | 宁波辉宏新材料有限公司 | 一种乳液聚合法合成乳液型mdq硅树脂的方法 |
CN111116917B (zh) * | 2019-12-18 | 2022-02-08 | 宁波辉宏新材料有限公司 | 一种乳液聚合法合成乳液型mdq硅树脂的方法 |
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EP2510057A1 (de) | 2012-10-17 |
WO2011069843A1 (de) | 2011-06-16 |
KR20120074302A (ko) | 2012-07-05 |
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