CN101346323A - 以蓖麻油为基础的新型多羟基化合物乳状液 - Google Patents
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- 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
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- C—CHEMISTRY; METALLURGY
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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
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Abstract
本发明涉及由蓖麻油和单环氧化物制备的新型多元醇化合物乳状液，由该多元醇化合物乳状液与二苯基甲烷－4，4’－二异氰酸酯(MDI)和水泥制备的聚合物水泥。
Description
本发明涉及了由蓖麻油和单环氧化物(Monoepoxid)制备的新型多羟基化合物乳状液以及由该多羟基化合物乳状液与二苯基甲烷-4，4’-二异氰酸酯(MDI)和水泥制备的聚合物水泥。
由蓖麻油乳状液、MDI和水泥制备聚合物水泥是已知的，并描述在GB 2353993中。然而，这里使用的蓖麻油乳状液是相对非常粘的，因此不能最佳地加工。
JP 2001-302304和JP 2004067463描述了由蓖麻油与蓖麻油酸和单环氧化物的反应产物制得的多羟基化合物乳状液。这些乳状液的粘度低于纯的蓖麻油乳状液的粘度，但是制备蓖麻油酸-单环氧化物加合物需要附加的反应步骤。
此外，该蓖麻油酸-单环氧化物加合物还包含OH基团，这些OH基团能形成氢桥键，因而提高了粘度。
因此，理想的是蓖麻油和这样的反应性稀释剂制成的乳状液，其中该反应性稀释剂不含OH基团，但在形成聚合物水泥的碱性反应条件下形成游离的OH基团，然后该OH基团与MDI交联而反应掉。
令人惊讶地，人们发现具有期望性能的低粘度乳状液可以从蓖麻油和单环氧化物制备得到，它可以与MDI和水泥反应产生聚合物水泥。在聚合物水泥形成的反应条件下，单环氧化物开环转变成相应的二醇和因而提供需要的OH基团。
因此，本发明的主题是乳状液，其包括
25至45重量份的水，优选25至35重量份，
45至69.5重量份的蓖麻油，优选55至63重量份，
5至30重量份的单环氧化物，优选至7-15重量份，和
0.5至5重量份的助剂和添加剂。
在本发明的上下文中，蓖麻油包括甘油与蓖麻油酸形成的酯，其中甘油的平均至少两个OH基团被蓖麻油酸酯化。其既可以是工业级别的又可以是药品级别的。
在本发明的上下文中，单环氧化物是每个分子有一个环氧基的全部化合物。优选符合通式(I)至(IV)的单环氧化物
其中
R是C4至C18烷基或者三乙氧基甲硅烷基丙基(或三甲氧基甲硅烷基丙基)，和
R’是氢原子，C1至C4烷基或者乙烯基。
优选使用式I或者II的单环氧化物，特别优选使用式I的单环氧化物，其中R表示C8至C16烷基。
助剂和添加剂可以例如是非离子型乳化剂、消泡剂和增稠剂，它们在根据本发明的乳状液中的一个优选实施方案中作为助剂和添加剂而存在。
可使用的非离子型乳化剂是乙氧基化的脂肪醇或烷基酚、聚环氧乙烷的脂肪酸酯、脱水山梨糖醇或乙氧基化脱水山梨糖醇的脂肪酸酯、聚环氧乙烷与其它聚环氧化物(优选聚氧化丙烯)的嵌段共聚醚，乙氧基化脂肪胺或脂肪酰胺或糖苷或糖酯。也可以使用非离子型乳化剂的混合物，总混合物的亲水亲油平衡(HLB)值为8～19，优选10～14。
纯聚环氧乙烷的HLB值是20，纯聚烯烃的HLB值是0，HLB值与聚环氧乙烷含量成正比例。这可以通过式HLB＝20·(Mh/M)表示，其中Mh是亲水的部分的摩尔质量，M是全部分子的摩尔质量(Griffin方法)。
可使用的消泡剂是例如硅酮，含醚基的硅酮，疏水化的二氧化硅，HLB值为3～10的非离子型乳化剂或者矿物油。
优选使用基于脱水山梨糖醇酯或者矿物油的非离子型乳化剂。
可使用的增稠剂是纤维素衍生物，例如羟乙基-、甲基-、羟基丙基-或者羧甲基醚。此外可以使用以聚氨酯或聚脲为基础的增稠剂，无机溶胶，例如氢氧化铝、聚乙烯醇、聚乙烯基吡咯烷酮，(甲基)丙烯酸或(甲基)丙烯酰胺的聚合物(共聚物)。酸官能聚合物优选以它们的碱金属盐或者铵盐的形式使用。
优选的增稠剂是上述类型的纤维素衍生物，特别优选羟乙基纤维素。
根据本发明的乳状液可另外包含多羟基化合物，例如甘油、低聚甘油、三羟甲基乙烷、三羟乙基丙烷、糖醇类、糖类、糖的衍生物或烷氧基化的胺类，例如三乙醇胺或者丙氧基化乙二胺。胺类可用羧酸或者羟基羧酸中和，例如柠檬酸或者酒石酸。
根据本发明的乳状液的粘度在23℃时一般为50～5000mPas，优选90～300mPas。
作为助剂或添加剂，该乳状液包含优选1～3重量份的脱水山梨糖醇单月桂酸酯作为乳化剂和消泡剂，由此实现聚合物水泥的额外改善的耐水性，这通过由静止水引起的“漂白(bleaching)”测定(视觉比较)。
在助剂和添加剂中，纤维素的羟烷基衍生物特别适合用作增稠剂。
通常，包含异氰酸酯反应性基团(例如OH或者NH基团)的助剂和添加剂是优选的。
在特别优选的实施方案中，包含至少1重量份的脱水山梨糖醇酯，至少0.5重量份的乙氧基化脂肪醇和至少0.1重量份的羟乙基纤维素作为助剂和添加剂。
根据本发明的乳状液的制备通过采用搅拌器或者射流分散器剪切来混合组分，优选脂溶性的组分先溶于蓖麻油中和水溶性的组分先溶于水中。将水相计量添加到油相还是反过来，是不重要的。
本发明的另一主题是聚合物水泥，其包含
10～25重量份的根据本发明的乳状液，
10～40重量份的MDI，和
35～80重量份的水泥。
原则上，已知的苯胺与甲醛缩合物的光气化作用产物能被用作MDI(二苯基甲烷-4，4’-二异氰酸酯)。这些光气化产物既可以是每个分子有两个芳族六元环的单体MDI异构体，也可以是每个分子包含三个或更多的芳族六元环的较高分子量的MDI类型。而且也可以使用基于上述的MDI类型和具有异氰脲酸酯-、脲基甲酸酯-、氨基甲酸酯-、碳二亚胺-、脲酮亚胺-(Urethonimin-)和/或脲二酮基团的较高分子量的后续产物。
优选使用的MDI是包含30重量％～85重量％的每个分子有两个芳族六元环的MDI异构体和15重量％-70重量％的每个分子包含三个或更多的芳族六元环的较高分子量的MDI类型的那些。
在本发明的上下文中，水泥是来自于无机的、非金属的、细碎物质的水硬性胶凝材料(hydraulische Bindmittel)，其与水混合而独立地硬化，并在空气或水中保持固态，例如波特兰水泥、铝酸钙水泥、硫酸钙水泥、水合氧化钙、氧氯镁水泥和其与氢氧化钙、氢氧化镁、颜料或者砂的混合物。上述的水泥详细描写在GB 1192864中。水泥的其它描述参见DIN 1164 PR EN 197/1中。优选水泥例如是波特兰水泥、含铁硅酸盐水泥、高炉水泥、火山灰水泥、高炉火山灰水泥、油页岩水泥或者高铝水泥，它们含至少23重量％的CaO，更优选含至少50重量％的CaO。根据本发明使用的水泥混合物优选包含1重量％～10重量％氢氧化钙(熟石灰)。
根据本发明的聚合物水泥的制备通过借助剪切混合组分实施，优选预先置入乳状液，然后再添加MDI和水泥。在混入MDI后，该混合物由于从水包油型乳状液到油包水型乳状液的乳状液变型而经历了粘度最大值。该混合物一般在8～45分钟适用期(Topfzeit)后可硬化产生填充水泥的未发泡的(unfoamed)聚氨酯。根据本发明的聚合物水泥在0℃～40℃温度和任何的空气湿度下硬化，特别适宜作为地板涂料。然而，可以涂覆任意期望的混凝土构件，以向其提供耐酸性。该施加可以通过涂抹或浇注实施。在硬化期间，可以通过翻转钉齿滚镇压器(Stachelwalze)使异氰酸酯-水反应产生的二氧化碳的放出更方便。
实施例：
在该实施例中使用蓖麻油1 DIN 55939。
粘度的测定根据DIN EN ISO 3219/A3在剪切梯度240 1/s和23℃条件下实施。
Polypox R24：C14-C16烷基缩水甘油醚，UPPC AG的商品，Mietingen-Baltringen，DE
Ruetapox EPD HD：1，6-己二醇二环氧甘油醚，Bakelite AG的商品，Duisburg，DE
Wallinat SML：脱水山梨糖醇单月桂酸值，Wall Chemie GmbH的商品，Kempen，DE
Vanquish 100正丁基-1，2-苯并异噻唑啉-3-酮，Avecia Biocides的商品，Frankfurt am Main，DE
Byk 501：经除泡沫的聚合物溶液、不含硅，BYK Chemie GmbH的商品，Wesel，DE
250LR型羟乙基纤维素：羟乙基纤维素，5％浓度水溶液在25℃时布氏粘度为100～180mPas，Hercules International Ltd.，的商品，GMRijswijk，NL
Tergitol 15S40：聚合度为40的聚乙二醇的C15-单烷基醚，DOW化学公司的商品，Midland，Michigan，美国
作为水泥混合物(1kg)使用：
735g的砂，粒度范围：0.3毫米～0.8毫米
9g的无机颜料(Fe2O3)
222g的波特兰水泥，白色
31g的氢氧化钙
3g的白油(矿物油)
加工时间根据采用钉齿滚镇压器处理所施加的涂层来测定。当通过目测钉齿滚镇压器产生的凹坑不再融合时，即为该加工时间的终点。
实施例1(根据本发明)
由60kg的蓖麻油、10kg的Polypox R24、1.85kg的Wallinat SML、0.1kg的Vanquish 100和1.2kg的Byk 501组成的混合物先剪切引入，再泵入由32kg的去离子水、1kg的250LR型纤维素羟乙基醚(Natrosol)和0.65kg的Tergitol 15S40组成的混合物。得到在室温下30天，在50℃ 30天和在3℃ 30天之后保持稳定的乳状液。在23℃时其粘度是140mPas。
116g的上述混合物首先与157.9g的Desmodur XP 2551混合，然后与726g的水泥混合物采用剪切混合。加工时间是18分钟。
实施例2(非根据本发明)
方法过程如实施例1描述，但是Polypox R24被相同的量的RuetapoxEPD HD替代。可得到在室温下30天后保持稳定的乳状液，在50℃ 30天后从5.5cm的填充高度分离出0.1cm高的水相，在4℃ 30天后保持稳定。其在23℃粘度为210mPas。
116g的上述混合物首先与157.9g的Desmodur XP 2551混合，然后与726g的水泥混合物采用剪切混合。加工时间是8分钟，这对于可靠的加工来说太短了。
实施例3(非根据本发明)
方法过程如实施例1描述，但是Polypox R24被相同量的正丁苄基邻苯二甲酸酯替代。可以得到室温下30天后，50℃时30天后和3℃时30天后保持稳定的乳状液。23℃时其粘度为190mPa.s。
实施例4(非根据本发明)
方法过程如实施例1描述，但是Polypox R24被相同量的另外的蓖麻油替代。可以得到室温下30天后，50℃ 30天后和3℃ 30天后保持稳定的乳状液。23℃时其粘度为270mPa.s。
Claims (8)
1.乳状液，其包含
25～45重量份的水，
45～69.5重量份的蓖麻油，
5～30重量份的单环氧化物，和
0.5～5重量份的助剂和添加剂。
2.根据权利要求1的乳状液，其特征在于含有通式(I)的化合物作为单环氧化物
其中R是C8～C16烷基。
3.根据权利要求1或者2的乳状液，其特征在于含有以脱水山梨糖醇酯、矿物油和/或羟乙基纤维素为基础的非离子型乳化剂作为助剂和添加剂。
4.根据权利要求1～3任一项的乳状液，其特征在于其在23℃时的粘度为90～300mPas。
5.聚合物水泥，其包含
10～25重量份的根据权利要求1～4任一项的乳状液，
10～40重量份的MDI(二苯基甲烷-4，4’-二异氰酸酯)，和
35～80重量份的水泥。
6.根据权利要求5的聚合物水泥，其特征在于，其含有作为MDI的具有30重量％～85重量％的每个分子有两个芳族六元环的MDI异构体和15重量％-70重量％的每个分子包含三个或更多的芳族六元环的较高分子量的MDI类型的混合物。
7.根据权利要求5或6的聚合物水泥，其特征在于，所用的水泥包含至少23重量％的CaO和1重量％～10重量％的氢氧化钙。
8.成型体和/或构件，可由根据权利要求5～7任一项的聚合物水泥获得。
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| DE102005062269A DE102005062269A1 (de) | 2005-12-24 | 2005-12-24 | Neue rizinusölbasierende Polyolemulsionen |
| DE102005062269.0 | 2005-12-24 | ||
| PCT/EP2006/011999 WO2007073866A1 (de) | 2005-12-24 | 2006-12-13 | Neue rizinusölbasierende polyolemulsionen |
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| EP (1) | EP1968911B1 (zh) |
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| DE (2) | DE102005062269A1 (zh) |
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| HK (1) | HK1128457A1 (zh) |
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| US7673687B2 (en) * | 2007-12-05 | 2010-03-09 | Halliburton Energy Services, Inc. | Cement compositions comprising crystalline organic materials and methods of using same |
| US8187376B2 (en) | 2010-05-25 | 2012-05-29 | W. R. Grace & Co.-Conn. | Defoamers for hydratable cementitious compositions |
| EP2796483A1 (en) * | 2013-04-26 | 2014-10-29 | Sika Technology AG | Three component composition for the manufacture of polyurethane cementitious flooring |
| JP6452953B2 (ja) * | 2014-05-09 | 2019-01-16 | 伊藤製油株式会社 | ポリオール含有組成物及び塗床形成用セメント組成物 |
| EP2944622A1 (en) * | 2014-05-16 | 2015-11-18 | Sika Technology AG | Three component composition for the manufacture of polyurethane cementitious hybrid flooring or coating with improved surface gloss |
| CN112724347B (zh) * | 2020-12-28 | 2022-07-19 | 上海汇得科技股份有限公司 | 一种生物基水性聚氨酯树脂及其制备方法和应用 |
| WO2023142101A1 (en) * | 2022-01-30 | 2023-08-03 | Sika Technology Ag | Three component composition for the manufacture of polyurethane cementitious hybrid flooring or coating with improved workability |
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| US2175096A (en) * | 1935-11-07 | 1939-10-03 | Ig Farbenindustrie Ag | Floor and wall covering material |
| GB509929A (en) * | 1937-12-21 | 1939-07-21 | Arthur Carpmael | Improvements in or relating to the manufacture of glass cements or putties |
| US3351574A (en) * | 1965-02-24 | 1967-11-07 | Celanese Coatings Co | Castor oil polyglycidyl ether |
| GB1131543A (en) * | 1966-04-15 | 1968-10-23 | Ciba Ltd | Epoxide resin compositions |
| BE793375A (fr) * | 1972-01-03 | 1973-06-27 | Ici Ltd | Nouvelles compositions cimentaires |
| DE2755940C2 (de) * | 1977-12-15 | 1986-01-02 | Basf Ag, 6700 Ludwigshafen | Mittel zur Regulierung des Pflanzenwachstums |
| GB2353993B (en) | 1999-09-09 | 2002-03-06 | Sterling Technology Ltd | Cement and castor oil mixtures for binding aggregates |
| JP4363742B2 (ja) * | 2000-04-17 | 2009-11-11 | 株式会社Ａｄｅｋａ | ポリオール樹脂組成物及びこれを用いたポリマーセメント硬化性組成物 |
| AU2003226136A1 (en) * | 2002-06-12 | 2003-12-31 | Dow Global Technologies Inc. | Cementitious composition |
| JP3897657B2 (ja) | 2002-08-08 | 2007-03-28 | 戸田建設株式会社 | 抗菌性ポリマーセメント硬化物の施工方法 |
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| US20090258970A1 (en) | 2009-10-15 |
| US20070149721A1 (en) | 2007-06-28 |
| ATE431320T1 (de) | 2009-05-15 |
| US8110621B2 (en) | 2012-02-07 |
| EP1968911A1 (de) | 2008-09-17 |
| ES2325223T3 (es) | 2009-08-28 |
| PL1968911T3 (pl) | 2009-10-30 |
| DE502006003749D1 (de) | 2009-06-25 |
| HK1128457A1 (en) | 2009-10-30 |
| WO2007073866A1 (de) | 2007-07-05 |
| RU2008130172A (ru) | 2010-01-27 |
| CN101346323B (zh) | 2012-09-05 |
| DE102005062269A1 (de) | 2007-06-28 |
| EP1968911B1 (de) | 2009-05-13 |
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