CN110650934A - 基于硫铝酸钙的无机泡沫 - Google Patents
基于硫铝酸钙的无机泡沫 Download PDFInfo
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- CN110650934A CN110650934A CN201880030017.8A CN201880030017A CN110650934A CN 110650934 A CN110650934 A CN 110650934A CN 201880030017 A CN201880030017 A CN 201880030017A CN 110650934 A CN110650934 A CN 110650934A
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- DAFQZPUISLXFBF-UHFFFAOYSA-N tetraoxathiolane 5,5-dioxide Chemical compound O=S1(=O)OOOO1 DAFQZPUISLXFBF-UHFFFAOYSA-N 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- 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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- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/04—Alkali metal or ammonium silicate cements ; Alkyl silicate cements; Silica sol cements; Soluble silicate cements
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- C04B14/041—Aluminium silicates other than clay
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- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/0048—Fibrous materials
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- C04B22/068—Peroxides, e.g. hydrogen peroxide
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- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
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- C04B22/142—Sulfates
- C04B22/143—Calcium-sulfate
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- C04B28/06—Aluminous cements
- C04B28/065—Calcium aluminosulfate cements, e.g. cements hydrating into ettringite
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Abstract
本发明涉及一种制备基于硫铝酸钙的颗粒稳定化无机泡沫的方法,一种基于硫铝酸钙的颗粒稳定化无机泡沫,一种可以通过硬化并任选干燥该基于硫铝酸钙的颗粒稳定化无机泡沫得到的泡孔材料以及一种制备用于提供基于硫铝酸钙的颗粒稳定化无机泡沫的无机泡沫配制剂的组合物。
Description
本发明涉及一种制备基于硫铝酸钙(calcium sulfoaluminate)的颗粒稳定化无机泡沫的方法,一种基于硫铝酸钙的颗粒稳定化无机泡沫,一种可以通过硬化并任选干燥该基于硫铝酸钙的颗粒稳定化无机泡沫得到的泡孔材料以及一种制备用于提供基于硫铝酸钙的颗粒稳定化无机泡沫的无机泡沫配制剂的组合物。
无机泡沫可以用作绝缘材料,例如用作绝热体、隔音材料或吸音材料以及具有低密度的建筑材料。与基于有机聚合物的泡沫相反,该材料环保、结实且不可燃。后者还可以在消防领域中产生应用。泡沫通常可以通过使用表面活性剂或颗粒稳定化。通过表面活性剂稳定的无机泡沫通常具有开孔泡沫结构。然而,特别令人感兴趣的是闭孔泡沫,因为它们具有改进的隔热性能,同时具有改进的机械稳定性。
已经发现具有闭孔泡沫结构的稳定无机泡沫可以通过将无机颗粒用作泡沫稳定剂而得到。通常要求存在两亲分子以诱发所用颗粒的表面活性。WO 2007/068127 A1公开了通过例如与没食子酸丙酯组合的胶态颗粒稳定湿泡沫。Juillerat等(F.K.Juillerat,U.T.Gonzenbach,P.Elser,A.R.Studart,L.J.Gauckler,J.Am.Ceram.Soc.2011,94,77-83)公开了通过胶态Al2O3颗粒稳定陶瓷泡沫,这些颗粒通过吸附没食子酸丙酯分子而部分疏水化。US 9,540,287 B2公开了没食子酸丙酯分子与胶凝颗粒组合使用以稳定发泡的胶凝淤浆。根据DE 102014103258 A1,石膏无机泡沫可以通过与两亲分子如庚基胺组合的无机颗粒稳定。
特别令人感兴趣的是基于活化硅铝酸盐(土工聚合物)的无机泡沫作为不可燃绝缘材料。已经发现颗粒稳定化闭孔土工聚合物泡沫与表面活性剂稳定化闭孔土工聚合物泡沫相比具有有利性能,尤其就干密度、抗压强度和气流电阻而言。同时,可以提供类似导热性。然而,颗粒稳定化闭孔土工聚合物泡沫对于凝结要求约14的高pH值,这就安全和处理而言引起问题。此外。土工聚合物泡沫的原料成本相当高。
因此,本发明的目的是要提供与土工聚合物泡沫相比具有类似或改进性能的闭孔无机泡沫,但同时确保其制备方法不要求如此高的pH值。此外,本发明的目的是要在更低原料成本下提供该类无机泡沫。本发明的目的尤其是要提供呈现令人满意的导热性并且在低干密度下具有高抗压强度的无机泡沫以及一种制备该类无机泡沫的安全方法。此外,目的是与土工聚合物泡沫相比还要提高无机泡沫的气流电阻。
惊人地发现上述目的可以由下文描述的本发明实现。尤其已经发现通过组合(i)至少一类无机颗粒,(ii)至少一种两亲化合物以及(iii)至少一种包含至少一种硫铝酸钙混合物和任选地,至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂的无机粘合剂混合物,可以得到无机泡沫,而不会中间形成具有高pH值的无机泡沫配制剂。相反,该无机泡沫配制剂的pH值可以保持低于12,这就安全和监管障碍而言以及就添加剂相容性(例如增塑剂)而言对该无机泡沫配制剂而言是有利的。结果得到具有精细且均匀闭孔结构的稳定无机泡沫。此外,本发明的无机泡沫呈现令人满意的导热性并且在低干密度下具有高抗压强度以及非常高的气流电阻。
在一个实施方案中,本发明涉及一种制备无机泡沫的方法,包括下列步骤:
(1)混合下列组分:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
(iv)水;以及任选地
(v)至少一种添加剂;以及
(2)通过化学、物理或机械发泡使所得泡沫配制剂发泡。
CN105645887A公开了一种高效结构阻燃纤维材料,其按重量计由7-13份阻燃增效剂氧化锑、4-8份高岭土、0.7-1.6份防腐剂、10-14份粉煤灰、4-7份麦草浆、10-20份苎麻纤维、3-5份草炭、8-13份仲醇乙氧基化物、0.5-1.2份十六烷基三甲基溴化铵、2-4份抗氧化剂、0.8-1.4份增韧剂、4-7份甲基丙烯酸环氧丙基酯、0.3-0.6份没食子酸丙酯、2-4份氧化钙、0.5-1.4份石蜡、18-26份发泡硫铝酸盐水泥、3-5份锂基固化剂、4-6份复合稳定剂和7-13份碳酸钙制备。与此相反,本发明不使用发泡硫铝酸盐水泥。本发明的整个泡沫配制剂随后通过化学、物理或机械发泡而发泡。
US 2014/0272376 A1公开了一种形成产品的淤浆,该淤浆包含:(a)水;(b)胶凝颗粒;(c)具有由水形成的壁的气泡;以及(d)有效改性至少一些胶凝颗粒的表面的表面改性剂,从而使得改性颗粒充分稳定气泡而在产物中形成气隙。据说胶凝颗粒包含厚浆灰泥、二水合硫酸钙、波特兰水泥、粉煤灰或其组合。与此相反,本发明不使用如US 2014/0272376A1中所定义的胶凝体系。
在另一实施方案中,本发明涉及一种可以通过本发明方法得到的无机泡沫。
在再一实施方案中,本发明涉及一种无机泡沫,其包含:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
(iv)水;以及任选地
(v)至少一种添加剂。
在再一实施方案中,本发明涉及一种可以通过硬化并任选干燥如本文所定义的无机泡沫得到的泡孔材料。
在再一实施方案中,本发明涉及一种制备无机泡沫配制剂的组合物,其包含如下作为组分:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
其中
组分(i)、(ii)和(iii)分开存在;或者
组分(i)和(ii)作为混合物存在且组分(iii)分开存在;或者
组分(i)、(ii)和(iii)作为混合物存在。
本发明由图1、2、3和4进一步说明。为对比目的提供图1,其显示具有开孔结构的表面活性剂稳定化土工聚合物泡沫的图片。为对比目的还提供图2,其显示主要具有闭孔结构的颗粒稳定化土工聚合物泡沫的图片。图3显示本发明颗粒稳定化无机泡沫的图片,其中无机粘合剂混合物仅包含硫铝酸钙混合物且不包含其他无机粘合剂。图4显示本发明颗粒稳定化无机泡沫的图片,其中无机粘合剂混合物包括硫铝酸钙混合物以及偏高岭土和粉煤灰的混合物作为其他无机粘合剂。在所有图中,左下侧的比例尺是2mm。
下列定义就本发明的实施方案而言相关。
就可测量单位而言术语“约”涉及所述可测量单位的正态偏差。该偏差取决于测量设备的精度或者取决于熟练技术人员预期的统计偏差。应理解的是术语“约”是指±15%,优选±10%,更优选±5%的偏差。
若无其他说明,术语“重量%”是指相应组分的质量相对于除水以外的所有组分的质量之和的比例,以%表示。术语体积%是指相应组分的体积相对于所有组分的体积之和的比例,以%表示。
术语“包含”的含义应解释为包括所有具体提到的特征以及任选的、额外的、未说明特征,而术语“由……构成”仅仅包括那些说明的特征。此外,在每种实际情况下本发明配制剂的所说明和未说明的成分的所有百分数之和意欲总是为100%。
就该制备无机泡沫的方法、该无机泡沫、可以通过硬化并任选干燥该无机泡沫得到的泡孔材料以及本发明用于制备无机泡沫配制剂的组合物而言,下列定义相关。
通常区分术语“无机泡沫配制剂”和“无机泡沫”。无机泡沫配制剂可以由适合通过加入水以及任选至少一种添加剂制备如本文所定义的无机泡沫配制剂的组合物得到。然后可以使用该无机泡沫配制剂来通过机械、物理或化学发泡制备无机泡沫。新制备的无机泡沫应区分于已硬化的无机泡沫,即可以通过硬化和任选干燥由新制备的无机泡沫得到的泡孔材料。除非另有所指,本文所用术语“无机泡沫”是指新制备的无机泡沫,而术语“泡孔材料”是指硬化且任选干燥的无机泡沫。
无机泡沫是三相体系,其中一相是气体,一相是液体且一相是固体。因此,应理解的是该无机泡沫包含气体。该气相以细气泡存在,其被由液相和固相得到的孔壁分隔。孔壁在于结点处相交的边缘相交,从而形成骨架。气相在无机泡沫中的含量可以在20-99体积%,优选50-98体积%范围内变化。液相优选为水相,因而无机泡沫通常还包含水。然而水可以在干燥时部分除去。无机泡沫的固相包含无机粘合剂。无机泡沫可以是开孔泡沫或闭孔泡沫。在闭孔泡沫中,气体完全被孔壁围绕。在相同密度下,闭孔泡沫通常比开孔泡沫更结实。因此,由于其改进的机械稳定性优选闭孔泡沫。
泡孔材料可以通过硬化并任选干燥无机泡沫而由无机泡沫得到。
本文所示的水可以涉及纯、去离子H2O或者含有至多0.1重量%杂质和/或盐的水,如普通自来水。
存在于泡沫中的气相可以通过机械、物理或化学发泡引入。气体的非限制性实例包括空气、氮气、稀有气体、二氧化碳、烃类、氢气、氧气及其混合物.
存在于泡沫中的气相可以通过在相应气体存在下机械发泡而引入。机械发泡例如可以通过使用混合机或者通过振荡方法或者通过定子-转子方法进行。
气相还可以通过物理或化学发泡引入泡沫中,其中物理或化学发泡方法适合释放气体。优选使用发泡剂,其蒸发、分解或者与水和/或酸反应,从而释放气体。发泡剂的非限制性实例是过氧化物,如过氧化氢、过氧化二苯甲酰、过氧苯甲酸、过氧乙酸、碱金属过氧化物、高氯酸、过氧单硫酸、过氧化二枯基或氢过氧化异丙苯;异氰酸盐、碳酸盐和碳酸氢盐,如CaCO3、Na2CO3和NaHCO3,它们优选与酸,例如无机酸组合使用;金属粉,如铝粉;叠氮化物,如甲基叠氮化物;酰肼,如对甲苯磺酰肼;肼。
化学发泡可以通过使用催化剂促进。合适的催化剂优选包含Mn2+、Mn4+、Mn7+或Fe3+阳离子。或者可以将过氧化氢酶用作催化剂。合适催化剂的非限制性实例是MnO2和KMnO4。该类催化剂优选与过氧化物发泡剂组合使用。
有关该制备无机泡沫的方法中所用组分、无机泡沫、可以通过硬化并任选干燥该无机泡沫得到的泡孔材料以及制备无机泡沫配制剂的本发明组合物的其他细节在下文提供。
本文所用术语“无机颗粒”优选是指选自如下的无机颗粒:
·氧化物,包括纯和混合金属氧化物(特别是氧化铝、二氧化硅、尖晶石、氧化铈-钆、氧化锆、氧化镁、氧化锡、氧化钛和氧化铈);
·氢氧化物(特别是氢氧化铝、氢氧化钙、氢氧化镁,非常特别的是氢氧化铝);
·碳化物(特别是碳化硅、碳化硼);
·氮化物(特别是氮化硅、氮化硼);
·磷酸盐(特别是磷酸钙,如磷酸三钙、羟基磷灰石);
·碳酸盐(特别是碳酸镍、碳酸钙(碎石灰或沉淀碳酸钙)、碳酸镁);
·硅酸盐(特别是二氧化硅、硅灰、粉煤灰、石英、玻璃粉、炉渣、硅酸钙、莫来石、堇青石、粘土矿物如高岭土或膨润土、硅酸锆、沸石、硅藻土,非常具体为硅灰、粘土矿物、硅酸锆;具体为粘土矿物);
·硫酸盐(特别是硫酸钙)。
应理解的是如上文所例举的无机颗粒(i)与无机粘合剂iiia和/或iiib并不相同。
优选无机颗粒由碳酸盐和/或氧化物得到。优选的氧化物包括选自氧化铝(包括Al-Mg尖晶石)、二氧化硅、二氧化锆和氧化锌,特别是氧化铝、二氧化硅和二氧化锆的纯和混合金属氧化物。优选的碳酸盐是碳酸钙。
本文所用术语“无机颗粒类”应理解为一种多元性无机颗粒。还应理解的是根据本发明可以使用至少一类,即一类或多类无机颗粒,这意味着上面定义的无机颗粒的各种混合物也是可能的。
因此,在本发明的优选实施方案中,该至少一类无机颗粒选自氧化物、氢氧化物、碳化物、氮化物、磷酸盐、碳酸盐、硅酸盐、硫酸盐及其混合物。
在更优选的实施方案中,该至少一类无机颗粒选自二氧化硅颗粒、氧化铝颗粒、氧化锆颗粒和CaCO3颗粒及其混合物。
该至少一类无机颗粒的粒度可以在宽范围内变化。对于粉末(初级颗粒),合适的平均粒度D50在30nm-300μm,优选100nm-250μm,更优选100nm-150μm,甚至更优选100nm-100μm范围内。在另一实施方案中,合适的粒度为100nm-10μm,优选100nm-2μm。发现粒度分布不太重要。可以得到具有窄和宽粒度分布的良好泡沫。
在本发明的优选实施方案中,该至少一类无机颗粒具有的平均粒度D50通过动态光散射测量在30nm-300μm范围内。
术语“粒度(Dx)”是指颗粒分布的直径,其中x%的颗粒具有更小直径。因此,D50粒度是平均粒度。Dx粒度例如可以通过激光衍射或动态光散射(DLS)方法测量。根据本发明优选使用根据ISO 22412:2008的动态光散射(DLS)。动态光散射(DLS),有时称为准弹性光散射(QELS)是测量通常在亚微米范围内的分子和颗粒的尺寸和尺寸分布的众所周知的非侵入式技术。在本发明中,表征已经分散于液体,优选水或乙醇中的颗粒。悬浮液中颗粒或分子的布朗运动引起激光在不同强度下散射。这些强度波动的分析得到布朗运动的速度并且因此使用Stokes-Einstein关系得到粒度。该分布可以是体积分布(Dv)、表面分布(Ds)或数量分布(Dn)。就本申请而言,Dx值是指数量分布,其中x(数量)%的颗粒具有更小的直径。
术语“两亲化合物”在本领域是已知的且涉及具有非极性部分(也称为尾部或基团R)和极性部分(也称为头基)的有机化合物。因此,合适的两亲分子含有通常由共价键与头基偶联的尾部。该类两亲分子通常含有一个尾部和一个头基,但也可以含有不止一个头基。
该尾部可以是脂族(线性或支化的)或环状的(脂环或芳族的)并且可以带有取代基。该类取代基例如是其中n≤8的CnH2n+1、仲-OH、仲-NH2等。优选的尾部是具有2-8个碳原子的任选被取代线性碳链,更优选具有3-8,4-8或5-8个碳原子的线性碳链。在整个说明书中,“仲-OH”和“仲-NH2”应指所得取代的尾基构成仲醇或仲胺。
与尾部偶联的头基优选为离子性基团、可离子化基团和/或极性基团。可能头基和相应盐的实例如下表1所述(其中尾部表示为R)。
表1:
优选的头基选自羧酸基团、没食子酸化物、胺类和磺酸化物。特别优选的头基选自羧酸基团(即-C(O)OH基团)、没食子酸化物和胺基团,其中X优选表示H或甲基。优选的羧酸是庚酸。优选的没食子酸化物是没食子酸丁酯。优选的胺是庚胺。最优选羧酸基团。
优选两亲分子对于小于或等于0.5mol/l的浓度将空气-水界面的表面张力降至小于或等于65mN/m的值。
优选两亲分子具有高于10μmol/l的临界胶束浓度(CMC)和/或它们具有高于1μmol/l的溶解度。
应理解的是根据本发明可以使用至少一种,即一种或多种两亲化合物,这意味着上面所定义的两亲化合物的各种混合物也是可能的。
因此,在本发明的优选实施方案中,该至少一种两亲化合物包括具有至少一个极性头基和至少一个非极性尾基的两亲化合物,
其中该至少一个头基选自磷酸化物、膦酸化物、硫酸化物、磺酸化物、醇类、胺类、酰胺类、吡咯烷类、没食子酸化物和羧酸;
并且其中该至少一个尾基选自具有2-8个碳原子的脂族或芳族或环状基团,其中碳原子任选被一个或多个选自C1-C8烷基、仲-OH和仲-NH2的相同或不同取代基取代。
在本发明的更优选实施方案中,该至少一种两亲化合物包括具有至少一个选自羧酸、没食子酸化物和胺类的头基以及至少一个选自具有2-8个碳原子的脂族基团的尾基的两亲化合物。
应理解的是在将如本文所定义的无机颗粒与如本文所定义的两亲化合物组合时形成疏水化无机颗粒。术语“疏水化无机颗粒”涉及其中颗粒的表面被两亲分子改性,以降低无机颗粒的亲水性能的无机颗粒。就此而言,表面改性是指两亲化合物吸附在颗粒的表面上。
在优选实施方案中,两亲化合物在无机颗粒表面上的量为0.5-160μmol/m2,优选10-140μmol/m2,更优选20-120μmol/m2,尤其是40-100μmol/m2。在另一优选实施方案中,无机颗粒相对于该至少一种无机粘合剂混合物的量以0.1-25重量%,优选0.25-15重量%,更优选0.5-15重量%,尤其是1-15重量%的量提供。
疏水化无机颗粒适合稳定基于本文所定义的无机粘合剂混合物的无机泡沫。在优选实施方案中,在泡沫配制剂中水与无机粘合剂混合物的重量比为0.1-2.0,优选0.2-1.5,更优选0.3-1.2,尤其是0.3-1。
无机粘合剂是在含水环境中(水硬性)或在空气存在下(非水硬性)硬化的无机化合物。例如,波特兰水泥是水硬性无机粘合剂,而石膏是非水硬性粘合剂。潜在水硬性粘合剂涉及仅在暴露于碱性活化剂时变为水硬性的粘合剂。
就本发明而言,使用的无机粘合剂混合物(iii)包含至少一种硫铝酸钙混合物(iiia)以及任选地,至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂(iiib)。
本发明的至少一种无机粘合剂混合物包含至少一种硫铝酸钙混合物(iiia)。术语“硫铝酸钙混合物”涉及一种在与水接触时可以形成硫铝酸钙相,如钙矾石((CaO)3(Al2O3)(CaSO4)3·30-32H2O)的混合物。
该硫铝酸钙混合物例如可以含有:
a)硫铝酸钙(4CaO×3Al2O3×SO3)以及任选斜硅灰石(2CaO×SiO2),和
b)硬石膏(CaSO4)和/或半水硫酸钙(CaSO4×0.5H2O)和/或石膏(CaSO4×2H2O),
a):b)的重量比为90:10-60:40,优选80:20-65:35。
该硫铝酸钙混合物具有大致如下的典型分析氧化物组成:
5-35重量%SO3
30-60重量%CaO
0-30重量%SiO2
5-35重量%Al2O3,
优选
10-30重量%SO3
30-50重量%CaO
0-20重量%SiO2
15-35重量%Al2O3,
更优选
17-27重量%SO3
37-47重量%CaO
5-15重量%SiO2
20-30重量%Al2O3。
本发明的至少一种无机粘合剂混合物可以任选额外包含至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂(iiib)。
术语“潜在水硬性粘合剂”和“凝硬性粘合剂”涉及尤其称为“土工聚合物”的无机粘合剂体系。土工聚合物例如描述于US 4,349,386,WO 85/03699和US 4,472,199中。
土工聚合物是主要基于SiO2和/或Al2O3,如聚铝硅酸盐(poly(sialate))、聚硅氧(poly(siloxo))、聚铝硅酸盐-硅氧(poly(sialate-siloxo))或聚铝硅酸盐-二硅氧(poly(sialate-disiloxo))的在碱性含水环境中硬化的粘合剂。铝硅酸盐(sialate)是硅-氧代-铝的缩写。土工聚合物材料类似于沸石,然而微观结构是无定形而非结晶的。这些粘合剂还可以含有基于Fe2O3、TiO2、CaO、MgO、NaO或K2O的化合物。纯土工聚合物通常具有低钙含量。WO 2011/064005 A1描述了一种包含12-25重量%CaO且允许生产耐受化学侵袭的建筑化学产品的无机粘合剂体系。土工聚合物的其他非限制性实例包括微细二氧化硅、偏高岭土、硅铝酸盐、粉煤灰、活性粘土、火山灰(pozzolan)或其混合物。火山灰是含硅或含硅和含铝化合物。
对本发明而言,“潜在水硬性粘合剂”优选为其中摩尔比(CaO+MgO):SiO2为0.8-2.5,特别是1.0-2.0的粘合剂。笼统地,上述潜在水硬性粘合剂可以选自工业和/或合成炉渣,尤其选自高炉渣、电热磷渣、钢渣及其混合物,而“凝硬性粘合剂”通常可以选自无定形二氧化硅,优选沉淀二氧化硅、气相二氧化硅和微细二氧化硅,玻璃粉,偏高岭土,硅铝酸盐,粉煤灰,优选褐煤粉煤灰和硬煤粉煤灰,天然火山灰如凝灰岩、粗面凝灰岩和火山灰,天然和合成沸石及其混合物。
如本文所用,术语“炉渣”是指冶炼工艺的副产物或合成炉渣。冶炼工艺的主要用途是将矿石、碎屑或含有不同金属的材料混合物转化成可以作为金属层从其刮削所需金属并且不需要的金属氧化物,例如硅酸盐、氧化铝等,作为炉渣保留的形式。
高炉渣(BFS)作为铁矿石在高炉中冶炼过程中的副产物形成。其他材料是粒化高炉渣(GBFS)和粒化高炉渣粉(GGBFS),后者为已经精细粉碎的粒化高炉渣。粒化高炉渣粉在磨矿细度和粒度分布方面变化,这取决于来源和处理方法,并且磨矿细度在这里影响反应性。将布莱恩值用作磨矿细度的参数并且其通常具有200-1000m2kg-1,优选300-500m2kg-1数量级。更细研磨给出更高反应性。然而,对本发明而言,表述“高炉渣”意欲包括来自所有处理、研磨程度并且具有所述质量的材料(即BFS、GBFS和GGBFS)。高炉渣通常包含30-45重量%CaO,约4-17重量%MgO,约30-45重量%SiO2和约5-15重量%Al2O3,通常是约40重量%CaO,约10重量%MgO,约35重量%SiO2和约12重量%Al2O3。
无定形二氧化硅优选为X射线无定形二氧化硅,即粉末衍射方法没有显示结晶度的二氧化硅。本发明无定形二氧化硅中的SiO2含量有利地为至少80重量%,优选至少90重量%。沉淀二氧化硅在工业规模上通过由水玻璃开始的沉淀方法得到。来自某些生产方法的沉淀二氧化硅也称为硅胶。
微细二氧化硅是细粉,主要包含无定形SiO2粉末并且为硅或硅铁合金生产的副产物。这些颗粒具有约100nm的直径和约15-30m2g-1的比表面积。
气相二氧化硅经由氯代硅烷类,例如四氯化硅在氢/氧焰中的反应生产。气相二氧化硅是粒径为5-50nm且比表面积为50-600m2 g-1的无定形SiO2粉末。
偏高岭土在高岭土脱水时生产。在100-200℃下高岭土释放物理结合的水,在500-800℃下发生脱羟基,晶格结构坍塌并形成偏高岭土(Al2Si2O7)。因此,纯偏高岭土包含约54重量%SiO2和约46重量%Al2O3。
硅铝酸盐是包含铝、硅和氧的矿物,其可以通过提到SiO2和Al2O3含量表达。它们是高岭土和其他粘土矿物的主要组分。红柱石、蓝晶石和硅线石是具有组成Al2SiO5的天然硅铝酸盐矿物。
粉煤灰尤其在煤在发电厂中燃烧过程中产生并且包含具有可变组成的细颗粒。粉煤灰的主要成分是氧化硅、氧化铝和氧化钙。C级粉煤灰(褐煤粉煤灰)根据WO 08/012438包含约10重量%CaO,而F级粉煤灰(硬煤粉煤灰)包含小于8重量%,优选小于4重量%,通常约约2重量%CaO。
烧页岩,尤其是焦油页岩在约800℃的温度下通过燃烧天然页岩并随后研磨而得到。
适合土工聚合物的原料的综述例如在Caijun Shi,Pavel V.Krivenko,DellaRoy,Alkali Activated Cements and Concretes,Taylor&Francis,London&New York,2006,第6-63页找到。
在优选实施方案中,该至少一种其他无机粘合剂选自高炉渣、微细二氧化硅、偏高岭土、硅铝酸盐、粉煤灰及其混合物。在特别优选的实施方案中,该至少一种其他无机粘合剂选自偏高岭土、粉煤灰及其混合物。
优选的是本发明组合物、无机泡沫配制剂、无机泡沫和泡孔材料不饱和额外的碱性活化剂。然而,若作为添加剂加入碱性活化剂,则优选碱性活化剂选自式MOH的碱金属氢氧化物和式m SiO2×n M2O的碱金属硅酸盐,其中M为碱金属,优选Li、Na或K或其混合物,并且摩尔比m:n≤4.0,优选≤3.0,进一步优选≤2.0,尤其是≤1.70。
该碱金属硅酸盐优选为水玻璃,特别优选含水水玻璃,尤其是钠水玻璃或钾水玻璃。然而,还可以使用锂水玻璃或铵水玻璃或所述水玻璃的混合物。优选不应超过上述m:n比(也称为“比率”),因为否则的话各组分的反应可能不完全。还可以使用小得多的比率,例如约0.2。具有更高比率的水玻璃应在使用之前通过使用合适的碱金属氢氧化物水溶液调节到本发明范围内的比率。
术语“水玻璃”是指水溶性碱金属硅酸盐。水玻璃可以通过碱金属碳酸盐与石英砂(二氧化硅)的反应得到。然而,它们还可以由反应性二氧化硅与合适的碱金属氢氧化物水溶液的混合物生产。水玻璃的非限制性实例包括Na2SiO3、K2SiO3和Li2SiO3。除了无水形式外,还存在水玻璃的各种水合物。典型的痕量杂质基于元素Al、Ca、Cr、Cu、Fe、Mg和Ti。碱金属与硅酸盐的比例可以变化。该比例如上所述以m SiO2与n M2O的摩尔比定义。比例m:n的典型值是小于4、小于3、小于2或在1.7附近的值。
在有利比率范围内的钾水玻璃主要以水溶液销售,因为它们非常吸湿;在有利比率范围内的钠水玻璃也可以作为固体市售得到。水玻璃水溶液的固体含量通常为20-60重量%,优选40-60重量%。
若使用碱性活化剂,则该碱性活化剂的优选量为1-55重量%,尤其是5-25重量%。
在优选实施方案中,该至少一种无机粘合剂混合物(iii)包含至少一种选自如下的水泥(iiic):根据DIN EN 197-1(11/2011)的CEM I、CEM II、CEM III、CEM IV、CEM V水泥,或铝酸钙水泥,优选CEM I水泥。该至少一种水泥可以存在于组分(iiia)、(iiib)中活着分开加入。
水泥是细碎的无机水硬性粘合剂。不同类型的水泥根据DIN EN 197-1(11/2011)分类为类别CEM I-V。这些不同的水泥在其对各种腐蚀剂的稳定性上相互变化,因此这些水泥具有不同的应用。
也称为波特兰水泥的CEM I水泥含有约70重量%CaO和MgO,约20重量%SiO2,约10重量%Al2O3和Fe2O3。该水泥通过研磨并烘烤石灰石、白垩和粘土而得到。CEM II水泥是具有低(约6-20重量%)或中等(约20-35重量%)量的额外组分的波特兰水泥。该水泥可以进一步含有高炉渣、气相二氧化硅(至多10重量%)、天然火山灰、煅烧的天然火山灰、粉煤灰、烧页岩或其混合物。也称为高炉渣水泥的CEM III水泥由含有36-85重量%炉渣的波特兰水泥构成。也称为凝硬性水泥的CEM IV水泥接近波特兰水泥含有11-65%火山灰、硅灰和粉煤灰的混合物。也称为复合水泥的CEM V水泥接近波特兰水泥含有18-50重量%炉渣或者天然火山灰、煅烧火山灰和粉煤灰的混合物。额外地,不同类型的水泥可以含有5重量%额外的细碎无机矿物化合物。
此外,根据本发明可以使用各种添加剂。在优选实施方案中,该至少一种添加剂选自pH改性剂、填料、促进剂、阻滞剂、流变改性剂、高效减水剂、表面活性剂、纤维、水玻璃、其他疏水化剂、催化剂及其混合物。
流变改性剂调节粘度并且因此调节流动性为,确保稠度、耐用性和应用性能之间的良好平衡。这些改性剂可以基于合成聚合物(例如丙烯酸系聚合物)、纤维素、二氧化硅、淀粉或粘土。
高效减水剂是用作分散剂以避免颗粒偏集,改进悬浮液的流变性并因此改善可加工性的聚合物。高效减水剂通常可以分为四类:木素磺酸盐,密胺磺酸盐,萘磺酸盐和梳状聚合物(例如聚羧酸酯醚、聚芳族醚、阳离子共聚物及其混合物)。
无机泡沫的凝结时间可以通过加入某些称为阻滞剂/促进剂的化合物延长/缩短。阻滞剂可以分为如下组:木素磺酸盐、纤维素衍生物、羟基羧酸、有机磷酸酯、合成阻滞剂和无机化合物。阻滞剂的非限制性实例是羟乙基纤维素、羧甲基羟乙基纤维素、柠檬酸、酒石酸、葡糖酸、葡庚糖酸盐、马来酸酐、2-丙烯酰胺基-2-甲基丙烷磺酸(AMPS)共聚物、硼砂、硼酸和ZnO。促进剂的非限制性实例是CaCl2、KCl、Na2SiO3、NaOH、Ca(OH)2和CaO×Al2O3、硅酸锂、硅酸钾,以及铝盐,如硫酸铝。
在发泡工艺过程中可以加入纤维(或稳定性纤维)以进一步提高泡沫稳定性。该纤维可以由各种材料,如岩石(例如玄武岩),玻璃,碳,有机聚合物(例如聚乙烯、聚丙烯、聚丙烯腈、聚酰胺和聚乙烯醇),纤维素,木素纤维素,金属(例如铁或钢)及其混合物制成。优选有机纤维。纤维的量基于该至少一种无机粘合剂混合物可以为至多3重量%,优选0.1-2重量%,更优选0.1-1.5重量%,尤其是0.2-1重量%。纤维优选具有至多200mm或者至多120mm,优选至多100mm,更优选至多50mm,最优选至多25mm,尤其是至多20mm的长度以及至多100μm的直径。
术语“填料”主要涉及可以加入以增加体积但不损害泡沫性能的材料。所述填料可以选自石英砂或石英粉,碳酸钙,岩粉,低密度填料(例如蛭石、珍珠岩、硅藻土、云母、滑石粉、氧化镁、发泡玻璃、中空球、泡沫砂、粘土、聚合物颗粒),颜料(例如二氧化钛),高密度填料(例如硫酸钡),金属盐(例如锌盐、钙盐等)及其混合物。在这里适合的粒度尤其是至多500μm。特别优选平均粒度为至多300μm,优选至多150μm。
除了本文所定义的两亲化合物外可以使用的表面活性剂包括非离子表面活性剂、阴离子表面活性剂、阳离子表面活性剂、两性离子表面活性剂和蛋白质或合成聚合物。然而,表面活性剂并不是优选的,因为它们倾向于得到开孔泡沫。
非离子表面活性剂包括脂肪醇、鲸蜡醇、硬脂醇和鲸蜡硬脂醇(主要包含鲸蜡醇和硬脂醇)和油醇。其他实例包括聚乙二醇烷基醚(Brij)CH3-(CH2)10-16-(O-C2H4)1-25-OH,如八乙二醇单十二烷基醚或五乙二醇单十二烷基醚;聚丙二醇烷基醚CH3-(CH2)10-16-(O-C3H6)1-25-OH;葡糖苷烷基醚CH3-(CH2)10-16-(O-葡糖苷)1-3-OH,如癸基葡糖苷、月桂基葡糖苷、辛基葡糖苷;聚乙二醇辛基苯基醚C8H17-(C6H4)-(O-C2H4)1-25-OH,如Triton X-100;聚乙二醇烷基苯基醚C9H19-(C6H4)-(O-C2H4)1-25-OH,如壬苯醇醚-9;甘油烷基酯,如月桂酸甘油酯;聚氧乙烯二醇脱水山梨醇烷基酯,如聚山梨酸酯;脱水山梨醇烷基酯,如Span类;椰油酰胺MEA,椰油酰胺DEA;十二烷基二甲基氧化胺;聚乙二醇和聚丙二醇的嵌段共聚物如泊洛沙姆;聚乙氧基化牛脂胺(POEA)。优选的非离子表面活性剂还包括烷基聚葡糖苷。烷基聚葡糖苷通常具有式H-(C6H10O5)m-O-R1,其中(C6H10O5)为葡萄糖单元,R1为C6-C22烷基,优选C8-C16烷基,尤其是C8-C12烷基且m=1-5。
阴离子表面活性剂在其头部含有阴离子官能基团,如硫酸盐、磺酸盐、磷酸盐和羧酸盐。重要的烷基硫酸盐包括月桂基硫酸铵、月桂基硫酸钠(十二烷基硫酸钠,SLS或SDS),以及相关烷基醚硫酸盐月桂醇聚醚硫酸钠(月桂基醚硫酸钠或SLES)和肉豆蔻醇聚醚硫酸钠。其他包括多库酯(磺基琥珀酸二辛酯钠)、全氟辛烷磺酸盐(PFOS)、全氟丁烷磺酸盐、烷基芳基醚磷酸盐、烷基醚磷酸盐。优选的羧酸盐包括烷基羧酸盐,如硬脂酸钠。最特殊的物质包括月桂酰肌氨酸钠和羧酸盐基氟表面活性剂如全氟壬酸盐、全氟辛酸盐(PFOA或PFO)。
阳离子表面活性剂取决于pH包括伯、仲或叔胺:伯和仲胺在pH<10下变得带正电荷。实例是奥替尼啶二盐酸盐。此外,阳离子表面活性剂包括永久带电的季铵盐,如十六烷基三甲基溴化铵(CTAB)、十六烷基氯化吡啶(CPC)、氯苄烷铵(BAC)、苄索氯铵(BZT)、二甲基二-十八烷基氯化铵、二-十八烷基二甲基溴化铵(DODAB)。
两性离子(两性)表面活性剂同时具有与相同分子连接的阳离子和阴离子中心。阳离子部分基于伯、仲或叔胺或季铵阳离子。阴离子部分可以更可变且包括磺酸盐,如在磺基甜菜碱CHAPS(3-[(3-胆碱酰胺丙基)二甲基铵]-1-丙烷磺酸盐)和椰油酰胺丙基羟基磺基甜菜碱中那样。甜菜碱如椰油酰胺丙基甜菜碱具有带铵的羧酸根。最常见的生物两性离子表面活性剂具有带胺或铵的磷酸根阴离子,如磷脂磷脂酰丝氨酸、磷脂酰乙醇胺、磷脂酰胆碱和鞘磷脂类。蛋白质的非限制性实例是牛血清白蛋白、卵白蛋白、乳酪蛋白或β-乳球蛋白。
表面活性剂的比例可以在宽范围内变化。表面活性剂可以以至多2.5重量%,优选至多1.5重量%的量存在。
水玻璃可以如上所解释的那样用作碱性活化剂。术语“水玻璃”也已经如上所定义。
可以用作添加剂的催化剂是可以与发泡剂组合用于发泡的催化剂。合适的催化剂如上文和下文就发泡剂而言所述。
有关本发明所用组分的量的其他细节如下所定义。
如上所解释的那样,本发明组分的量优选如下。具体而言,两亲化合物在无机颗粒表面上的量尤其为0.5-160μmol/m2;和/或无机颗粒相对于该至少一种无机粘合剂混合物的量以0.1-25重量%的量提供;和/或水与干无机粘合剂混合物的重量比为0.1-2.0。
在一个示例性实施方案中,两亲化合物在无机颗粒表面上的量为10-140μmol/m2,优选20-120μmol/m2;和/或无机颗粒相对于该至少一种无机粘合剂混合物的量以0.25-15重量%的量提供;和/或水与无机粘合剂混合物的重量比为0.2-1.5。
如上所解释的那样,应理解的是可以使用至少一类,即一类或多类无机颗粒以及至少一种,即一种或多种两亲化合物。上述量分别涉及用于本发明方法中或者存在于本发明组合物、无机泡沫或泡孔材料中的两亲化合物和无机颗粒的总量。此外,与无机粘合剂混合物相关的上述量涉及用于本发明方法中或者存在于本发明组合物、无机泡沫或泡孔材料中的无机粘合剂的总量。
若该至少一种无机粘合剂混合物包含:
(iiia)至少一种硫铝酸钙混合物,以及
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂,
则组分(iiib)和(iiia)可以以0.1-3.4,优选0.1-2.0,更优选0.3-1.5的相对重量比存在。
添加剂的合适量可以在宽范围内变化且还取决于添加剂类型。通常基于该至少一种无机粘合剂的量以0.0003-30重量%或0.03-25重量%的重量比提供该至少一种添加剂。然而,填料还可以以更高的量使用。该填料尤其可以以与无机粘合剂类似的量存在。优选填料与至少一种无机粘合剂混合物的重量比可以为2:1-1:100,优选1:1-1:10。
有关本发明方法的其他细节在下文提供。
在本发明方法的优选实施方案中,步骤(1)包括下列步骤:
(1a)将该至少一类无机颗粒、该至少一种两亲化合物以及任选地,该至少一种添加剂分散于水中,得到水分散体;以及
(1b)将该水分散体与该至少一种无机粘合剂混合物混合。
应理解的是优选在步骤(1a)中首先使该至少一类无机颗粒、该至少一种两亲化合物以及任选地,该至少一种添加剂相互组合,然后将所得混合物分散于水中。
在优选的实施方案中,在本发明方法的步骤(1)中得到的无机泡沫配制剂具有小于12的pH值,这就安全、处理和与常用添加剂的相容性而言是本发明的重要优点。
在本发明方法的优选实施方案中,步骤(2)包括使所得泡沫配制剂通过化学发泡而发泡。在本发明方法的另一优选实施方案中,步骤(2)包括使所得泡沫配制剂通过物理发泡而发泡。在本发明方法的再一优选实施方案中,步骤(2)包括使所得泡沫配制剂通过机械发泡而发泡。
在优选实施方案中,该制备无机泡沫的方法的步骤(2)包括用发泡剂使所得泡沫配制剂发泡,优选通过将步骤(1)中得到的泡沫配制剂与碳酸盐或碳酸氢盐,如CaCO3、Na2CO3和NaHCO3,铝粉,对甲苯磺酰肼,过氧化氢,过氧化二苄基,高氯酸,过氧单硫酸,过氧化二枯基,氢过氧化异丙苯或其混合物,更优选过氧化氢混合。在更优选的实施方案中,泡沫配制剂在步骤(2)中的发泡用发泡剂进行,优选通过将步骤(1)中得到的泡沫配制剂与铝粉或碳酸盐在酸存在下混合或者与过氧化氢水溶液任选在催化剂存在下混合。
在更优选的实施方案中,制备无机泡沫的方法的步骤(2)包括用发泡剂,优选如上所定义的发泡剂使所得泡沫配制剂发泡,其中发泡剂基于泡沫配制剂的总量以0.1-10重量%的量加入。
可以通过加入合适的催化剂促进发泡过程,尤其是用过氧化物作为发泡剂发泡。因此,在优选实施方案中,该制备无机泡沫的方法的步骤(2)包括在催化剂存在下用化学法发泡剂使所得泡沫配制剂发泡,其中优选该催化剂包含Mn2+、Mn4+、Mn7+或Fe3+阳离子,或者该催化剂为过氧化氢酶。更优选该催化剂选自MnSO4、MnO2、KMnO4及其混合物。该催化剂基于泡沫配制剂的总量可以以0.01-5重量%,优选0.01-2重量%,更优选0.05-1.0重量%,尤其是0.1-0.6重量%的量使用。
在优选实施方案中,化学发泡剂是作为包含10-60重量%,优选20-60重量%,尤其是40-60重量%过氧化氢的过氧化氢水溶液提供的过氧化氢,其中过氧化氢水溶液基于泡沫配制剂的总重量以0.1-6重量%,优选0.5-5.0重量%,尤其是1-4重量%的量加入,使用约50重量%过氧化氢溶液。
在另一优选实施方案中,进行机械发泡,优选通过使用混合机或者通过振荡方法或者通过定子-转子方法。
在发泡步骤(2)之后,得到本发明的无机泡沫。
在优选实施方案中,使新制备的无机泡沫在步骤2)之后在密封容器中硬化。在更优选的实施方案中,使新制备的无机泡沫在步骤2)之后在密封容器中硬化至少12小时。硬化可以在0-100℃,优选20-80℃的温度下进行。
泡孔材料通过硬化以及任选地,干燥上述无机泡沫得到。本发明的泡孔材料可以呈隔热元件、吸声元件或消防元件形式,其中该元件在每种情况下可以是例如片或板。
本发明无机泡沫和泡孔材料具有大部分闭孔的结构和下列有利特征。
干密度通常小于300kg/m3,适当的是小于200kg/m3,优选小于150kg/m3,更优选小于100kg/m3。干密度尤其甚至可以进一步降至小于100kg/m3,优选小于90kg/m3,若该至少一种无机粘合剂混合物不仅仅包含该至少一种硫铝酸钙混合物,而且还包含该至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂的话。有利的是干密度小于表面活性剂稳定化土工聚合物泡沫和基于其的泡孔材料的干密度。
导热性(DIN EN 12667)优选小于50mW/mK,更优选小于45mW/mK,尤其是小于40mW/mK。导热性通常甚至好于表面活性剂稳定化土工聚合物泡沫和基于其的泡孔材料的导热性。
抗压强度(DIN EN 826)优选为至少30kPa。抗压强度通常类似于表面活性剂稳定化土工聚合物泡沫和基于其的泡孔材料的抗压强度。事实上由于更低的干密度,抗压强度与干密度之比改善。
气流电阻(DIN EN 29 053)优选为至少1000kPa s/m2,更优选至少1500kPa s/m2,最优选至少1800kPa s/m2。气流电阻尤其甚至可以进一步提高到至少2000kPa s/m2,若该至少一种无机粘合剂混合物不仅仅包含该至少一种硫铝酸钙混合物,而且还包含该至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂的话。有利的是气流电阻显著高于表面活性剂稳定化土工聚合物泡沫和基于其的泡孔材料的气流电阻,后二者通常具有小于200kPa s/m2或甚至小于50kPa s/m2的气流电阻。
本发明由下列实施例进一步说明。
实施例
对比例1
土工聚合物泡沫由下列组成(重量%)的原料制备:
20.5%偏高岭土(ArgicalTMM 1200S,Imerys)
7.8%铝酸钙水泥(CimentKerneos)
0.2%PAN纤维(6mm,6.7dtex)
19.5%水
27.4%水玻璃(“Kaliwasserglass K58”,BASF)
2.9%NaOH
首先将液体原料与NaOH混合。将固体原料加入液体组分中并搅拌,直到产生均相淤浆。然后用厨房混合机产生泡沫。将如此得到的泡沫倾入模具中。发生凝结反应并且泡沫开始固化。将土工聚合物泡沫在潮湿气氛下储存3天以允许适当凝结。然后将其脱模并在70℃下干燥直到恒定质量。
所得土工聚合物泡沫部件具有300mm×300mm×40mm的尺寸。其干密度为144kg/m3且其导热性为42.1mW/mK。抗压强度为48kPa,抗弯强度为28kPa。该样品的特征在于气流电阻率(DIN EN 29 053)为4.2kPa s/m2。该泡沫如图1所示主要呈开孔。
对比例2
将包含79.8重量%碳酸钙(Socal 31)、15.1重量%没食子酸丁酯和5.1重量%氧化锰(IV)的混合物作为“泡沫形成粉末”预混。
土工聚合物泡沫由下列组成(重量%)的原料制备:
19.2%偏高岭土(ArgicalTMM 1200S,Imerys)
2.3%泡沫形成粉末
0.2%PAN纤维(6mm,6.7dtex)
23.4%水
26.3%水玻璃(“Kaliwasserglass K58”,BASF)
2.8%过氧化氢(50%溶液)
首先将泡沫形成粉末分散于水中。然后将该悬浮液加入水玻璃中。加入偏高岭土和粉煤灰的混合物并将该悬浮液搅拌10分钟。然后混合铝酸钙水泥。搅拌15分钟后通过加入过氧化氢引发该悬浮液的发泡。将如此得到的淤浆倾入模具中,在其中逐渐发生泡沫膨胀,直到过氧化氢分解完全。制备的湿泡沫是稳定的,直到约30分钟之后发生凝结反应并且泡沫开始固化。将该土工聚合物泡沫在潮湿气氛中储存3天以允许适当凝结。然后将其脱模并在70℃下干燥直到恒定质量。
所得土工聚合物泡沫部件具有200mm×200mm×50mm的尺寸。其干密度为127kg/m3且其导热性为39.6mW/mK。该样品的特征在于气流电阻率为233kPa s/m2。该泡沫主要呈闭孔。该泡沫的图片提供在图2中。
工作实施例1
将包含88.5重量%碳酸钙(Precarb 100)、5.8重量%庚酸和5.7重量%氧化锰(IV)的混合物作为“泡沫形成粉末”预混。
硫铝酸钙泡沫由下列组成(重量%)的原料制备:
12.2%二水合硫酸钙
6.5%泡沫形成粉末
0.3%PAN纤维(6mm,6.7dtex)
38.7%水
2.9%过氧化氢(50%溶液)
首先将泡沫形成粉末分散于水中。然后混合硫铝酸钙和二水合硫酸钙的混合物。搅拌15分钟之后通过加入过氧化氢引发该悬浮液的发泡。将如此得到的淤浆倾入模具中,在其中逐渐发生泡沫膨胀,直到过氧化氢分解完全。制备的湿泡沫是稳定的,直到约15分钟之后发生凝结反应并且泡沫开始固化。将该硫铝酸钙泡沫在潮湿气氛中储存过夜以允许适当凝结。然后将其脱模并在70℃下干燥直到恒定质量。
所得硫铝酸钙泡沫部件具有240mm×480mm×100mm的尺寸。其干密度为111kg/m3且其导热性为42.1mW/mK。抗压强度为48kPa。该样品的特征在于气流电阻率1990kPa s/m2。该泡沫如图3所示呈闭孔。
工作实施例2
硫铝酸钙泡沫由下列组成(重量%)的原料制备:
18.7%硫铝酸钙(Italcementi)
5.8%二水合硫酸钙
12.2%偏高岭土(ArgicalTMM 1200S,Imerys)
3.7%泡沫形成粉末
0.2%PAN纤维(6mm,6.7dtex)
43.9%水
3.2%过氧化氢(50%溶液)
首先将泡沫形成粉末分散于水中。然后混合硫铝酸钙、二水合硫酸钙、偏高岭土和粉煤灰的混合物。搅拌15分钟之后通过加入过氧化氢引发该悬浮液的发泡。将如此得到的淤浆倾入模具中,在其中逐渐发生泡沫膨胀,直到过氧化氢分解完全。制备的湿泡沫是稳定的,直到约15分钟之后发生凝结反应并且泡沫开始固化。将该硫铝酸钙泡沫在潮湿气氛中储存3天以允许适当凝结。然后将其脱模并在70℃下干燥直到恒定质量。
所得硫铝酸钙泡沫部件具有240mm×480mm×100mm的尺寸。其干密度为83kg/m3且其导热性为36.4mW/mK。抗压强度为43kPa,抗弯强度为28kPa。该样品的特征是气流电阻率为2220kPa s/m2。该泡沫如图4所示呈现闭孔。
Claims (19)
1.一种制备无机泡沫的方法,包括下列步骤:
(1)混合下列组分:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
(iv)水;以及任选地
(v)至少一种添加剂;以及
(2)通过化学、物理或机械发泡使所得泡沫配制剂发泡。
2.根据权利要求1的方法,其中所述至少一类无机颗粒选自氧化物、氢氧化物、碳化物、氮化物、磷酸盐、碳酸盐、硅酸盐、硫酸盐及其混合物。
3.根据权利要求1或2的方法,其中所述至少一类无机颗粒选自二氧化硅颗粒、氧化铝颗粒、氧化锆颗粒和CaCO3颗粒及其混合物。
4.根据权利要求1-3中任一项的方法,其中所述至少一类无机颗粒具有的平均粒度D50在30nm-300μm范围内。
5.根据权利要求1-4中任一项的方法,其中所述至少一种两亲化合物包括具有至少一个极性头基和至少一个非极性尾基的两亲化合物,其中所述至少一个头基选自磷酸化物、膦酸化物、硫酸化物、磺酸化物、醇类、胺类、酰胺类、吡咯烷类、没食子酸化物和羧酸;
并且其中所述至少一个尾基选自具有2-8个碳原子的脂族或芳族或环状基团,其中碳原子任选被一个或多个选自C1-C8烷基、仲-OH和仲-NH2的相同或不同取代基取代。
6.根据权利要求1-5中任一项的方法,其中所述至少一种两亲化合物包括具有至少一个选自羧酸、没食子酸化物和胺类的头基以及至少一个选自具有2-8个碳原子的脂族基团的尾基的两亲化合物。
7.根据权利要求1-6中任一项的方法,其中所述至少一种硫铝酸钙混合物具有5-35重量%SO3,30-60重量%CaO,0-30重量%SiO2和5-35重量%Al2O3的分析氧化物组成。
8.根据权利要求1-7中任一项的方法,其中所述至少一种硫铝酸钙混合物含有a)硫铝酸钙(4CaO×3Al2O3×SO3)以及任选斜硅灰石(2CaO×SiO2)和b)硬石膏(CaSO4)、半水硫酸钙(CaSO4×0.5H2O)和/或石膏(CaSO4×2H2O),a):b)的重量比为90:10-60:40。
9.根据权利要求1-8中任一项的方法,其中所述至少一种其他无机粘合剂选自高炉渣、微细二氧化硅、偏高岭土、硅铝酸盐、粉煤灰及其混合物。
10.根据权利要求1-9中任一项的方法,其中所述至少一种其他无机粘合剂为偏高岭土和粉煤灰的混合物。
11.根据权利要求1-10中任一项的方法,其中所述至少一种无机粘合剂混合物(iii)包含:
(iiic)至少一种选自如下的水泥:根据DIN EN 197-1(11/2011)的CEM I、CEM II、CEMIII、CEM IV、CEM V水泥,或铝酸钙水泥,优选CEM I水泥。
12.根据权利要求1-11中任一项的方法,其中所述至少一种添加剂选自pH改性剂、填料、促进剂、阻滞剂、流变改性剂、高效减水剂、表面活性剂、纤维、水玻璃、其他疏水化剂、催化剂及其混合物。
13.根据权利要求1-12中任一项的方法,其中两亲化合物在无机颗粒表面上的量为0.5-160μmol/m2;和/或其中所述无机颗粒相对于所述至少一种无机粘合剂混合物的量以0.1-25重量%的量提供;和/或其中水与所述无机粘合剂混合物的重量比为0.1-2.0。
14.根据权利要求1-13中任一项的方法,其中步骤(1)包括下列步骤:
(1a)将所述至少一类无机颗粒、所述至少一种两亲化合物以及任选地,所述至少一种添加剂分散于水中,得到水分散体;以及
(1b)使所述水分散体与所述至少一种无机粘合剂混合物混合。
15.一种可以通过根据权利要求1-14中任一项的方法得到的无机泡沫。
16.一种无机泡沫,包含:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
(iv)水;以及任选地
(v)至少一种添加剂。
17.一种可以通过硬化并任选干燥根据权利要求15或16的无机泡沫得到的泡孔材料。
18.一种制备无机泡沫配制剂的组合物,包含如下作为组分:
(i)至少一类无机颗粒;
(ii)至少一种两亲化合物;
(iii)至少一种无机粘合剂混合物,其包含:
(iiia)至少一种硫铝酸钙混合物,以及任选地,
(iiib)至少一种选自水硬性粘合剂、潜在水硬性粘合剂、凝硬性粘合剂及其混合物的其他无机粘合剂;
其中
组分(i)、(ii)和(iii)分开存在;或者
组分(i)和(ii)作为混合物存在且组分(iii)分开存在;或者
组分(i)、(ii)和(iii)作为混合物存在。
19.根据权利要求15或16的无机泡沫、根据权利要求17的泡孔材料和/或根据权利要求18的组合物作为绝热体、隔音材料或吸音材料,用于消防和/或作为具有低密度的建筑材料的用途。
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CN116535122A (zh) * | 2023-05-12 | 2023-08-04 | 辽宁天宝华瑞建材有限公司 | 一种钢渣的粉磨活化方法和钢渣助磨活化剂 |
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PL3592715T3 (pl) | 2022-02-14 |
US11066337B2 (en) | 2021-07-20 |
PL3907203T3 (pl) | 2022-11-21 |
EP3592715B1 (en) | 2021-07-14 |
EP3592715A1 (en) | 2020-01-15 |
JP7150742B2 (ja) | 2022-10-11 |
RU2019130668A3 (zh) | 2021-07-05 |
ES2887030T3 (es) | 2021-12-21 |
WO2018162381A1 (en) | 2018-09-13 |
EP3907203B1 (en) | 2022-07-20 |
AU2023210634A1 (en) | 2023-08-24 |
SA519410064B1 (ar) | 2023-01-17 |
AU2018232506A1 (en) | 2019-09-26 |
RU2019130668A (ru) | 2021-04-07 |
ES2925454T3 (es) | 2022-10-18 |
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CA3055003A1 (en) | 2018-09-13 |
JP2020512256A (ja) | 2020-04-23 |
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