CN1048696C - 干凝胶，其制备方法和用途 - Google Patents

干凝胶，其制备方法和用途 Download PDF

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CN1048696C
CN1048696C CN95108111A CN95108111A CN1048696C CN 1048696 C CN1048696 C CN 1048696C CN 95108111 A CN95108111 A CN 95108111A CN 95108111 A CN95108111 A CN 95108111A CN 1048696 C CN1048696 C CN 1048696C
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gel
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R-M·简森
A·兹莫曼
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Aventis Research and Technologies GmbH and Co KG
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/152—Preparation of hydrogels
    • C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
    • C01B33/1543—Preparation of hydrogels by acidic treatment of aqueous silicate solutions using ion exchangers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/152—Preparation of hydrogels
    • C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract

本发明涉及改性SiO2凝胶(干凝胶)，其制备和作为绝热材料的用途。这样制备该干凝胶：酸化水玻璃水溶液，加入碱使由此产生的硅酸缩聚为SiO2凝胶，用与水形成冷却时分为两相的共沸物的有机溶剂萃取蒸馏，从形成的凝胶中除去水，该凝胶与甲硅烷基化试剂反应，在低于除水所用有机溶剂的临界压力和/或临界温度的压力和温度下干燥此凝胶。

Description

干凝胶，其制备方法和用途
本发明涉及改性SiO2凝胶(以下称为“干凝胶”)的制备方法，按此方法制得的干凝胶本身和其用途。
经干燥适当的凝胶制备广义上的气凝胶，即“用空气作为分散介质的凝胶”。在此意义上的“气凝胶”包括狭义的气凝胶，干凝胶和低温凝胶。与此相关，当在临界温度以上从临界压力以上的压力开始很彻底地去除凝胶的液体时，干燥的凝胶称为狭义的气凝胶。另一方面，如果在亚临界条件下去除凝胶的液体，例如形成液气界相，形成的凝胶称为干凝胶。
制得的干凝胶与常规SiO2气凝胶相关，但与之不完全相同。
已知SiO2气凝胶具有极好的绝热作用，它们例如通过原硅酸四乙酯在乙醇中酸水解来制备。水解生成凝胶的结构由温度、PH和胶凝过程的持续时间决定。但一般湿凝胶干燥时凝胶的结构崩解，因为在干燥过程中产生的毛细管力极大。在溶剂的临界温度和临界压力以上进行干燥时，可防止凝胶的崩解。因为在此区域液/气相界消失，也不产生毛细管力，在干燥过程中凝胶无变化，即在干燥过程中凝胶也不收缩。基于此干燥技术的制备方法例如公开在EP-A-0396 076或WO92 03378中。但如使用乙醇时此技术要求温度高于240℃，压力大于40巴。虽然在干燥前用CO2代替乙醇，可将干燥温度降至约40℃，但需要80巴的压力。
现发现，当在干燥前与甲硅烷基化试剂反应时，可在亚临界条件下干燥SiO2凝胶。以下将生成的产物称为“干凝胶”。它们是极佳的绝热材料。
本发明涉及干凝胶的制备方法，其包括：
a)用酸性离子交换树脂或无机酸调节水玻璃水溶液至PH≤3.0，优选≤2.2，
b)加入碱，使由此产生的硅酸缩聚为SiO2凝胶，如果a)步中使用了无机酸，需要时用水洗涤凝胶，直至无电解质为止，
c)用与水形成冷却时分离成两相的共沸物的有机溶剂进行萃取蒸馏，从b)步所得凝胶中除去水，直至凝胶的含水量≤5％(重量)，
d)c)步所得凝胶与甲硅烷基化试剂反应，
e)在低于c)步所用有机溶剂的临界压力和/或临界温度的压力和温度下干燥d)步所得甲硅烷基化凝胶。
在a)中优选使用的特别适合于此目的的酸性离子交换树脂为含磺酸基的那些。如果使用无机酸，盐酸和硫酸特别适合。水玻璃一般使用钠和/或钾水玻璃。水玻璃的浓度优选在1-20％(重量)范围内，最优选在5-12％(重量)范围内。
在b)步优选使用的碱为NH4OH、NaOH、KOH、Al(OH)3和/或胶态硅酸。如果a)步使用无机酸，用碱产生的SiO2凝胶适当时用水洗涤，直到无电解质为止；最好持续洗涤直到流出的洗涤水与去离子水的电导率相等。
在c)步前，优选使凝胶在一般0-150℃，优选80-130℃，PH4-11，优选4-9条件下老化。老化时间一般为10秒到48小时，优选为10秒到5小时。
在c)步，用有机溶剂萃取蒸馏除去凝胶中所含水，直至凝胶中含水量不超过5％(重量)，优选≤2％(重量)。所用溶剂必须与水形成共沸物，冷却时该共沸物分成两液相，水相和溶剂相。适当溶剂的实例为甲苯、二正丁基醚或甲基异丁基酮。优选使用甲苯。
共沸物冷却时形成的溶剂相可再返回此工艺中。
a)到c)步一般在溶液的凝固点到溶剂的沸点间的温度下进行。
在d)步，含溶剂凝胶与甲硅烷基化试剂反应。所用甲硅烷基化试剂一般为式R1 4-nSiCln或R1 4-nSi(OR2)n的甲硅烷，其中n＝1-3，R1和R2相互独立地为C1-C6-烷基、环己基或苯基。硅氮烷也适用。优选使用单-、二-或三甲基氯代甲硅烷、三甲基甲氧基甲硅烷或六甲基二硅氮烷。反应一般在20-100℃，优选30-70℃进行，如果需要，在溶剂如甲苯、丙酮、正己烷、正庚烷、二正丁基醚、异丙醇或甲基异丁基酮中进行。适当时还可以在优选达25巴的压力下进行甲硅烷基化。适当时，干燥前还可以洗涤甲硅烷基化凝胶。
在e)步，甲硅烷基化凝胶在-30℃到溶剂沸点，优点在-30℃到200℃，特别优选在0-150℃的温度下干燥。用于干燥的压力优选为0.001到20巴，特别优选0.01-5巴。一般持续干燥直到溶剂残余含量小于0.1％(重量)。
为了得到特别的热性能，此干凝胶最好另外还含有IR遮光剂(如炭黑、二氧化钛、氧化铁和二氧化锆)。在此情形下，优选在b)步前加入这些IR遮光剂。
以下实施例说明本发明的方法。
实施例
让1升钠水玻璃溶液(含6％(重量)的SiO2，及Na2O∶SiO2之比为2∶3)通过一0.5升酸性离子交换树脂(带磺酸基的苯乙烯/二乙烯基苯共聚物，以Duolite 20的名称在市场上有售)填充的柱子(直径50mm，长度300mm)。流出溶液的PH为1.5。用1摩尔NH4OH溶液调节此溶液PH至5.6。形成的凝胶在50℃老化24小时，然后，在带水分离器的萃取器中于约100℃下用3升甲苯萃取水。当分离出计算量的水(约920ml)后，停止萃取。然后，此含甲苯凝胶在50℃用三甲基氯代甲硅烷(TMCS)甲硅烷基化12小时(0.05gTMCS每克含甲苯凝胶)。在大气压下N2气吹洗下在干燥器中干燥此凝胶(40℃6小时，再50℃2小时，再150℃12小时)。
这样得到的透明干凝胶的密度为0.12g/cm3。BET比表面积为920m2/g。λ值为0.016W/mK。
用热金属线法测定导热率(见，如O.Nielsson，G，Rschenpohler，J.GroB，J.Fricke，High-Temperatures High-Pressures，Vol.21.267-274(1989))。

Claims (8)

1.一种干凝胶的制备方法，其特征在于其包括：
a)用酸性离子交换树脂或无机酸调节水玻璃水溶液至PH≤3.0，
b)加入碱，使由此产生的硅酸缩聚为SiO2凝胶，如果a)步中使用了无机酸，需要时用水洗涤凝胶，直至无电解质为止，
c)用与水形成冷却时分离成两相的共沸物的有机溶剂进行萃取蒸馏，从b)步所得凝胶中除去水，直至凝胶的含水量≤5％(重量)，
d)c)步所得凝胶与甲硅烷基化试剂反应，
e)在低于c)步所用有机溶剂的临界压力和/或临界温度的压力和温度下干燥d)步所得甲硅烷基化凝胶。
2.权利要求1的方法，其中a)步中使用酸性离子交换树脂。
3.权利要求1的方法，其中使用NH3OH、NaOH、KOH、Al(OH)3和/或胶态硅酸作为b)步中的碱。
4.权利要求1的方法，其中让b)步所得SiO2凝胶在c)步除水以前于0-150℃及PH4-11老化10秒钟到48小时。
5.权利要求1的方法，其中使用甲苯、二正丁基醚或甲基异丁基酮作为c)步中的有机溶剂。
6.权利要求1的方法，其中使用单-、二-或三甲基氯代甲硅烷、三甲基甲氧基甲硅烷或六甲基二硅氮烷作为d)步中的甲硅烷基化试剂。
7.权利要求1的方法，其中在e)步中于-30℃到200℃干燥甲硅烷基化的凝胶。
8.权利要求1的方法，其中在e)步中于0.001-20巴干燥甲硅烷基化的凝胶。
CN95108111A 1994-06-30 1995-06-28 干凝胶，其制备方法和用途 Expired - Lifetime CN1048696C (zh)

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DE4422912A DE4422912A1 (de) 1994-06-30 1994-06-30 Xerogele, Verfahren zu ihrer Herstellung, sowie ihre Verwendung
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DE4422912A1 (de) 1996-01-11
EP0690023A2 (de) 1996-01-03
CA2152977A1 (en) 1995-12-31
ES2134377T3 (es) 1999-10-01
NO952618D0 (no) 1995-06-29
NO952618L (no) 1996-01-02
EP0690023B1 (de) 1999-05-12
JPH0859224A (ja) 1996-03-05
US5647962A (en) 1997-07-15
CN1124229A (zh) 1996-06-12
JP3808115B2 (ja) 2006-08-09
DE59505881D1 (de) 1999-06-17

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