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CN1057039A - 多孔结晶合成材料，其合成和应用 - Google Patents

多孔结晶合成材料，其合成和应用 Download PDF

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CN1057039A
CN1057039A CN90103973A CN90103973A CN1057039A CN 1057039 A CN1057039 A CN 1057039A CN 90103973 A CN90103973 A CN 90103973A CN 90103973 A CN90103973 A CN 90103973A CN 1057039 A CN1057039 A CN 1057039A
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波琴(Nmn)丘
梅柯尼希鲁宾
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Abstract

一种多孔结晶的合成材料，其特征是X射线衍 射谱显示的值基本上是本说明书表1中所提出的值， 系从含钠阳离子，含至少30％重量比的固体氧化硅 石、氧化铝、水和六甲撑亚胺的反应混合物制备而 成。

Description

本发明是关于多孔结晶合成材料，其制备方法和其在有机化合物的催化转化中的应用。
无论是天然还是合成的沸石，在此之前都已显示出对各种烃的转化具有催化的性质。某些沸石是一些有序的多孔结晶的铝硅酸盐，具有由X射线衍射法所测定的确定的结晶结构，结晶体内有大量的较小的空穴，空穴可能被许多更小的槽或细孔彼此连系起来。就专门的沸石来说，这些空穴和细孔在大小上是一致的。由于这些细孔的大小能容纳某些大小的被吸附的分子而同时拒绝了大尺寸的分子，故这些物质已习惯于被称作“分子筛”，以各种方式应用在能发挥其长处的地方。
无论是天然还是合成的分子筛都包含各种正离子的结晶硅酸盐。这些硅酸盐可以表述为SiO4和周期表ⅢA族元素氧化物，例如AlO4的三维刚性骨架，在这种骨架结构中，四面体由于氧原子的共享而交联起来，其中ⅢA族元素，例如铝原子和硅原子的总和与氧原子的比为1∶2。含ⅢA族元素，例如铝的四面体的电子价被其中所夹杂的阳离子-例如碱金属或碱土金属阳离子-的结晶所平衡。这种四面体可以表达如下，即其中，ⅢA族元素，例如铝，对各种阳离子数，例如Ca/2，Sr/2，Na，K或Li的比例等于1。利用离子交换技术，以通用的方式可以使一种阳离子部分或全部被另一种阳离子所取代。通过这种阳离子交换法以及选择适当的阳离子已经能够改变给定的硅酸盐的一些性质。
已有技术已经导致形成了各种各样的合成沸石。这些沸石的许多种已经习惯于用字母或其它传统符号来表示。例如沸石A（美国专利2，882，243），沸石X（美国专利2，882，244），沸石Y（美国专利3，130，007），沸石ZK-5（美国专利3，247，195），沸石ZK-4（美国专利3，314，752），沸石Z  SM-5（美国专利3702，886），沸石Z  SM-11（美国专利3，709，979），沸石Z  SM-12（美国专利3，832，449），沸石Z  SM-20（美国专利3，972，983），Z  SM-35（美国专利4，016，245）和沸石Z  SM-23（美国专利4，076，842）。
给定的沸石的Si O2/Al2O3比常常是可变的。例如，沸石X可以2至3的Si O2/Al2O3比来合成;沸石Y可以3至6合成。在某些沸石中，Si O2/Al2O3比的上限是不限定的。Z SM-5是其例之一，其中的Si O2/Al2O3比至少为5，高可以高至现有分析测定技术的上限。美国专利3，941，871（Re，29，948）披露了一个多孔结晶的硅酸盐，其由含不精确加入的氧化铝和显示Z SM-5特征X射线衍射谱的反应混合物所制备。美国专利4，061，724，4，073，865和4，104，294都阐述了各种氧化铝和金属含量的结晶硅酸盐。
首先，本发明是关于多孔结晶的合成材料，其特征是利用X射线衍射，其谱线包含了基本上是本发明专利说明书中表Ⅰ列出的各个值，并具有大于10重量%水蒸汽、大于4.5重量%环己烷蒸气和大于10重量%正己烷蒸气的平衡吸附力。
本发明的多孔结晶材料看起来与美国专利4，439，409中阐述的名为“P  SH-3”的构成物有关。但本结晶物质看来并不含有所有在P  SH-3构成物中明显存在的成分。尤其是，本发明的构成物没有受到其它结晶-例如Z  SM-12或Z  SM-5-结晶的玷污，与按美国专利4，439，409合成出来的P  SH-3构成物相比较，显示出不寻常的吸附力和独特的催化应用性。
本发明的结晶物可以利用含所需氧化物的原料与六甲撑亚胺定向剂一起的反应混合物的结晶作用而合成。但已发现，尤其是当本发明的结晶物是硅酸盐时，采用固体含量相对较高的氧化硅原料是很重要的。
其次，本发明的第二个方面是关于按本发明的一个方面来制备合成结晶物的方法，本发明由制备反应混合物（反应混合物能在结晶后形成所述的物质，所述的反应混合物含足够量的碱金属或碱土金属阳离子，含至少约30重量%固体YO2的四价氧化物YO2的原料，三价氧化物X2O3的原料，水和六甲撑亚胺）以及将所述的反应混合物保持在足够结晶化的条件中直至所述物质的结晶形成为止。
本发明的结晶物具有下面的构成，包括相应的摩尔比例关系：
式中X是三价元素，例如铝，硼，铁和/或镓，最好是铝，Y是四价元素，例如硅和/或锗，最好是硅，n至少是10，通常从10至150，较好是10到60，最好是20至40。物质在合成形态下，按照无水物的计算法和每n个摩尔的YO2具有的氧化物的摩尔数，具有下列分子式：
式中R是有机体部分，Na和R组分作为它们在结晶时存在的结果而与该物质联系在一起，并易于用后结晶方法（于后面细述）除去。
本发明的结晶物质是热稳定的，具有很高的表面积（大于400m2/g）与有类似结晶结构的相比较有不同寻常的吸附力。从上面的结构式已可看出，本发明的结晶物合成时几乎无Na阳离子。因此，它可用作具有酸活性而无交换步骤的催化剂。然而，根据需要，合成材料中有原有钠阳离子可以现有技术中所熟知的工艺手段来取代，至少可用离子交换法用其它阳离子部分取代。推荐取代的阳离子包括金属离子，氢离子，氢产物母体一例如铵，离子和其混合物。最好是采用对某种烃转化反应具有催化活性的那些阳离子。这些阳离子包括氢，稀土金属和元素周期表中ⅡA，ⅢA，ⅣA，ⅠB，ⅡB，ⅢB，ⅣB和Ⅷ族的金属。
就其灼烧的形式而言，本发明的结晶物看来是由单晶相（带少量的或测不到的杂质晶相）所组成，具有下面表Ⅰ中所列示的X射线衍射谱，这些谱图与其它已知的结晶物的谱图有所不同：
表Ⅰ
晶面间的d-间距（A）  相对强度I/Io×100
30.0±2.2  W-M
22.1±1.3  W
更为特定的是下面表Ⅱ所列：
表Ⅱ
晶面间的d-间距（A）  相对强度I/Io×100
30.0±2.2  W-M
22.1±1.3  W
3.91±0.07  M-VS
至目前为止更为特定的是下面表Ⅲ所列：
表Ⅲ
晶面间的d-间距（A）  相对强度I/Io×100
30.0±2.2  W-M
22.1±1.3  W
6.00±0.10  W-M
4.64±0.08  W
4.06±0.07  W-S
3.91±0.07  M-VS
最特别的是本发明的灼烧过的结晶材料的X射线衍射谱图包括在下面表Ⅳ中所列的谱图。
表Ⅳ
晶面间的d-间距（A）  相对强度I/Io×100
30.0±2.2  W-M
22.1±1.3  W
12.36±0.2  M-VS
11.03±0.2  M-S
8.83±0.14  M-VS
6.86±0.14  W-M
6.18±0.12  M-VS
6.00±0.10  W-M
5.54±0.10  W-M
4.92±0.09  W
4.64±0.08  W
4.41±0.08  W-M
4.25±0.08  W
4.10±0.07  W-S
4.06±0.07  W-S
3.91±0.07  M-VS
3.75±0.06  W-M
3.56±0.06  W-M
3.42±0.06  VS
3.30±0.05  W-M
3.20±0.05  W-M
3.14±0.05  W-M
3.07±0.05  W
2.99±0.05  W
2.82±0.05  W
2.78±0.05  W
2.68±0.05  W
2.59±0.05  W
上述这些数值都用标准技术来确定的。辐射线是铜的K-阿尔法双线，衍射仪装备闪烁计数器和采用联机。峰高，I，和位置（它们是2θ的函数，θ是Bragg角），都是通过与衍射仪连通的计算机进行算术运算后确定的。从这些值中确定出与各记录线相对应的各个相对强度，100I/Io（式中Io是最强线的强度或峰值）和以
Figure 90103973X_IMG1
单位表示的d（观察值）晶面间的间距。在表Ⅰ-Ⅳ中，相对强度以符号W＝弱，M＝中，S＝强和VS＝甚强来表示。强度符号一般是指：
W＝0-20
M＝20-40
S＝40-60
VS＝60-100
应该了解，此X射线衍射谱对现有所有结晶构成物都是特征性的。钠形式和其它阳离子形式实质上显露出相同的谱图，只是在晶面间距上有少许偏移，相对强度上有些变化。还可能发生其它一些少许变化，这取决于特定试样中的Y和X的比例，例如硅对铝的比例，以及取决于它们的热处理的程度。
本发明的结晶物质可以从含有碱金属或碱土金属（M），例如钠阳离子或钾阳离子、三价元素X（例如铝）的氧化物、四价元素Y（例如硅）的氧化物原料，以及下面还要详谈的有机定向剂（R），和水的反应混合物中制得，所述的反应混合物，其中各氧化物的摩尔比例位于下列范围之内，其构成如下：
反应物  有用  最好为
YO2/X2O310-80 10-60
H2O/YO25-100 10-50
OH-/YO20.01-1.0 0.1-0.5
M/YO20.01-2.0 0.1-1.0
R/YO20.05-1.0 0.1-0.5
已经发现，如YO2反应原料含至少30重量%固体YO2，尤其当YO2是氧化硅时，本发明物质的结晶状态就很好，可以得到的适宜的氧化硅原料Ultrasil（一种沉淀成的、喷雾干燥的氧化硅，含约90重量%硅石）和Hi Sil（一种沉淀成的水合的SiO2，含约87重量%氧化硅，约6重量%游离水和约4.5重量%的水合水，粒径约0.02微米）。如用其它Si O2原料，例如用Q-Brand（由约28.8重量%Si O2，8.9重量%Na2O和62.3重量%H2O组成的硅酸钠），就会发现结晶后很少产生本发明中要求的结晶物或根本就没有产生，而代之以形成其它结晶结构，例如Z SM-12的各个杂质相。因此，YO2原料最好含有至少30重量%的固体YO2，最好是氧化硅，更好的是至少含40重量%固体YO2。
从上述反应混合物合成现在结晶物所用的有机定向剂（R）是六甲撑亚胺，它具有下列结构式：
本结晶物可在适当的反应器，例如在聚丙烯罐或聚四氟乙烯衬里釜或不锈钢釜中，在静态或搅拌条件下进行结晶。结晶通常在80℃至225℃温度下，进行24小时至60天。此后，将晶体与液体分离并加以回收。
如能在至少0.01%，最好是0.10%，更佳的是在1%的所需结晶产物的晶种（以总重量计算）的存在下进行结晶，效果更好。
在用作催化剂或吸附剂之前，应将合成得到的结晶物加以灼烧以部分或全部除去任何有机成份。
本发明的结晶物可用作催化剂，用在与氢化组份密切关联的金属上，例如钨、钒、钼、铼、镍、钴、铬、锰、或铂或钯一类贵金属上，这些金属常常起着加氢或脱氢的作用。这类组份可以共结晶的方式存在于结构物中，本质已交换到结构物中，浸渍在其中或在其中密切地进行物理掺混。举铂为例，这样的组分可以浸渍于结构物内，例如，将硅酸盐用含铂金属离子的溶液加以处理。适用于这种用途的铂化合物包括氯铂酸，氯化铂和各种含铂胺配位化合物的化合物。
本发明的结晶物的粒子可分为各种大小。一般而言，其粒子可以是粉末，颗粒或模塑品，例如挤塑物。若是后者，那么结晶物可在干燥前挤塑或部分干燥后再挤塑。
本发明的结晶物，在其作为吸附剂或催化剂用于有机化合物的转化工艺时应先脱水，至少部分脱水。通过在空气或氮气等氛围气中，在大气压，低于大气压或高于大气压的压力之下，加热到温度达到200℃到595℃范围内达30分钟到48小时而做到这一点。也可将硅酸盐放在真空中，仅在室温下进行脱水，但需要化较长的时间，以便使脱水充分。
本发明的结晶物可用于催化各种有机转化工艺，举例来说，C2-C7烯烃，例如聚丙烯水合成醇类和醚类，其反应条件包括50到300℃，最好是90到250℃温度，至少5kg/cm2，最好至少20kg/cm2的压力以及水/烯烃的摩尔比为0.1-30，最好是0.2-15。
在许多催化剂的例子中，常常可将本发明的结晶物与在有机转化工艺中所用的能耐受温度和其它条件的另一些物质一起并用。这些物质包括有活性和惰性物质，合成和天然沸石以及诸如粘土，氧化硅和/或氧化铝一类金属氧化物类无机物。后者既可以是天然产生的物质也可以是凝胶沉淀物或胶体的形态，包括氧化硅和金属氧化物的混合物。将这种物质与新结晶并用，亦即在新结晶合成时存在着或与其结合在一起，这种新结晶是活性的，趋向于改变某些有机转化工艺中催化剂的转化率和/或选择性。惰性物质适宜用作稀释剂以控制某一给定工艺中的转化量使得能够经济有序地获得产物，不需要使用其它手段来控制反应的速率。这些物质也可以并用到天然产生的各种粘土中，如膨润土和高岭土中，改进工业操作条件下催化剂的抗破碎强度。所述物质，即粘土，氧化物等对催化剂起到粘合剂的作用，希望催化剂在工业使用时具有良好的抗破碎强度，防止催化剂碎裂成粉状物质。这些粘土粘结剂已经使用，但通常只是用来改进催化剂的抗破碎强度。
与新结晶配伍使用的天然粘土计有蒙脱土和高岭土家族，这个大家族计有次膨润土和通常作为Dixie，Mc  Namee，Georgia，和Florida粘土群的高岭土或其它（其主要矿石成份是多水高岭土，高岭土，地开石，珍珠陶土或富硅高岭石）粘土。这些粘土以原始矿物开采出来的状态使用，也可以经灼烧，酸处理或化学改性的初加工后使用。与本结晶配伍使用的粘合剂还包括无机氧化物，特别是氧化铝。
除了上述物质之外，新结晶还可与多孔型物质，例如氧化硅-氧化铝，氧化硅-氧化镁，氧化硅-氧化锆，氧化硅-氧化钍，氧化硅-氧化铍，氧化硅-二氧化钛以及三元组分，例如氧化硅-氧化铝-氧化钍，氧化硅-氧化铝-氧化锆，氧化硅-氧化铝-氧化镁和氧化硅-氧化镁-氧化锆并用。
细分结晶物和无机氧化物的相对比例变动很大，就晶体的含量而言，从1到90重量%都有，尤其是当构成物以珠粒形状制备时是如此，其更为常用的范围是取组成物的2至80重量%。
现以实施例和附图对本发明作更详尽的说明，图1-5各为实施例1，3，4，5和9的灼烧产物的X射线衍射图谱。在实施例中，凡有吸附值数据的均是提出来与水、环己烷和/或正己烷的吸附值作比较，它们都是一些用以下方法测得的平衡吸附值：
称量一份灼烧吸附剂的试样使与所要求的纯吸附蒸汽在吸附室中接触，抽真空至1mm，与12乇水蒸汽和40乇正己烷或环己烷蒸气接触，压力小于在90℃下的各吸附剂的气一液平衡压力。压力通过在吸附期内加入由稳压器控制的吸附剂蒸气而保持稳定（在约±0.5mm之内），吸附期不超过8小时。当吸附剂被新晶体吸附后，压力的下降引起稳压器打开凡尔，以使更多的吸附剂蒸气进入室内重新使上面的控制压力得以恢复。当压力的变化不足使稳压器有所动作时便告吸附完成。重量上的增加以每100克灼烧过的吸附剂中试样的吸附力为多少克计算出来的。
本发明的合成材料的平衡吸附值总是显示出大于水蒸汽的10重量%，大于环己烷蒸气的4.5重量%，一般是7重量%，大于正己烷蒸气的10重量%。
当阿尔法值已予确定时，应注意到阿尔法值是约略指示出与标准催化剂相比较的催化剂的催化裂解活性，它给出的是与取作1的阿尔法（速率常数＝0.016秒-1）的高活性氧化硅-氧化铝裂解催化剂相比较而言的相对速率常数（每单位体积催化剂每单位时间内的正己烷的转化率）。阿尔法测试已在美国专利3，354，078和在催化剂杂志（Journal of Catalysis）Vol，Ⅳ，pp，522-529（1965年8月）上阐说过。需注意的是，许多酸催化的反应的固有速率常数是与特定的结晶化硅酸盐催化剂的阿尔法值呈正比的，对甲苯而言是不成比例的，对二甲苯异构物，烯烃转化和甲醇转化也不成比例（见“自然”杂志Vo 1，309，No，5969，pp，589-591，1984年6月14日的“酸性铝硅酸盐催化剂的活性位置”）
实施例1
将铝酸钠（43.5%Al2O3，32.2%Na2O，25.6%H2O）12.86克溶于含12.8克50%NaOH溶液和1320克H2O的溶液中，再加入57.6克六甲撑亚胺。将配好的溶液加入到109.4克的Ultrasil中（一种沉淀的喷雾干燥的氧化硅，含约90%SiO2）。
反应混合物具有下述组成，组成以摩尔比表示：
SiO2/Al2O3＝30.0
OH-/SiO2＝0.18
H2O/SiO2＝44.9
Na/SiO2＝0.18
R/SiO2＝0.35
式中R是六甲撑亚胺。
混合物被放在一只带搅拌的不锈钢反应釜中结晶，在150℃，结晶7天。将结晶物过滤，用水洗涤，在120℃干燥。在538℃下灼烧20小时后，X射线衍射谱具有表Ⅴ所列的主线。图1为灼烧产物的X射线衍射谱。灼烧产物的吸附能力经测定为：
H2O（12乇） 15.2重量%
环己烷（40乇）  14.6重量%
正己烷（40乇）  16.7重量%
灼烧过的结晶物的表面积经测定为494m2/g。
灼烧物的化学组成经测定为：
成份  重量%
SiO266.9
Al2O35.40
Na  0.03
N  2.27
    76.3
Al2O3摩尔比＝21.1
表Ⅴ
2θ度  晶面d-间距（A）  I/Io
2.80  31.55  25
4.02  21.98  10
7.10  12.45  96
7.95  11.12  47
10.00  8.85  51
12.90  6.86  11
14.34  6.18  42
14.72  6.02  15
15.90  5.57  20
17.81  4.98  5
19.08  4.65  2
20.20  4.40  20
20.91  4.25  5
21.59  4.12  20
21.92  4.06  13
22.67  3.92  30
23.70  3.75  13
25.01  3.56  20
26.00  3.43  100
26.96  3.31  14
27.75  3.21  15
28.52  3.13  10
29.01  3.08  5
29.71  3.01  5
31.61  2.830  5
32.21  2.779  5
33.35  2.687  5
34.61  2.592  5
实施例2
取部分实施例1的灼烧过的结晶物用阿尔法测试法加以测定，发现阿尔法值为224。
实施例3-5
将3份分开的合成反应混合物按表Ⅵ所列的组分比例加以制备。混合物用铝酸钠，氢氧化钠，UItrasil，六甲撑亚胺（R）和水加以制备。将混合物在150℃、143℃和150℃下各保持7，8和6天，保持在自动压力下搅拌着的一只不锈钢热压釜中，搅拌速度为350转/分。用过滤将固体与任何未反应的组分分开来，然后用水洗涤，继之在120℃干燥。结晶物用X射线衍射法，吸附法，表面积法和化学分析法加以分析，产物被发现是本发明中的新结晶物质。将吸附、表面积和化学分析的结果也列于表Ⅵ中。实施例3，4和5灼烧产物（在538℃灼烧3小时）的X射线衍射谱分别列在图2，3和4上。吸附和表面积测定都是用灼烧产物。
表Ⅵ
实施例数  3  4  5
合成混合物，摩尔比
SiO2/Al2O330.0 30.0 30.0
OH-/SiO20.18 0.18 0.18
H2O/SiO219.4 19.4 44.9
Na/SiO20.18 0.18 0.18
R/SiO20.35 0.35 0.35
产物组成，重量%
SiO264.3 68.5 74.5
Al2O34.85 5.58 4.87
Na  0.08  0.05  0.01
N  2.40  2.33  2.12
灰份  77.1  77.3  78.2
SiO2/Al2O3，摩尔比 22.5 20.9 26.0
吸附率，重量%
H2O 14.9 13.6 14.6
环己烷  12.5  12.2  13.6
正己烷  14.6  16.2  19.0
表面积，m2/g 481 492 487
实施例6
将几份实施例3，4和5的灼烧过的（538℃烘3小时）结晶硅酸盐产物用阿尔法测试法加以测定，得到其阿尔法值各为227，180和187。
实施例7
将实施例4的灼烧过的结晶硅酸盐试样用Pt（NH3）4Cl2溶液浸渍到约1（重量）%Pt，然后将此物质在空气中在349℃加热3小时。
实施例8
将从实施例7获得的产物1克作为催化剂被加入到一只有预加热器和插入热电偶的小反应器中。然后在482℃加热催化剂通以流动氢气以使Pt组分还原。以癸烷和氢/烃的摩尔比为100/1地将正癸烷和氢通过催化剂获得0.4小时-1重量时空速度（WHSV）。反应是在温度范围为130-250℃，和1大气压下进行。
此实验的结果汇集于表Ⅶ中，与同样实验的一些结果汇集在一起。但变换为Z  SM-5（美国专利3，702，886）和Z  SM-11（美国专利3，709，979）和β沸石（美国专利3，308，069）的结晶物乃是用作对比的。可看到本发明的结晶硅酸盐对正癸烷加氢转化是很佳活性的催化剂并具有良好的异构活性。在表Ⅶ中，“5MN/2MN”是5-甲基壬烷/2-甲基壬烷的摩尔比。由于它们的甲基基团的位置不同，5-甲基壬烷对进入沸石孔的过程给予了稍高的空间位阻阻力。5MN/2MN之比提供了被测沸石的孔隙率方面的情况。
表Ⅶ
沸石  沸石的  50%转化率  在50%  5MN/2MN
催化剂 SiO2/Al2O3的温度 转化率时 5% 20%
摩尔比  的异构物%  异构物异构物
实施例7  20.9  174  70  0.15  0.24
Z  SM-5  50  187  65  0.11  0.15
Z  SM-11  40  187  94  0.36  0.41
Z  SM-23  85  211  90  0.27  0.28
β  30  189  76  0.68  0.59
实施例9
为了表明大量制备本发明的结晶材料，将1，200克的六甲撑亚胺加到含有268克的铝酸钠;267克的50%氢氧化钠溶液和11，800克的水的溶液中。再加2，280克Ultrasil氧化硅到该混合溶液中，使此混合物在5加仑大小反应器中在145℃下搅拌结晶，搅拌速度为200转/分，结晶时间是59小时。产物用水洗涤并在120℃下干燥。
灼烧（538℃）结晶物的X射线衍射谱示于图5并表明该产物是本发明的结晶物。产物的化学成分、表面积和吸附分析的结果如下：
表Ⅷ
产物成分
C  12.1重量%
N  1.98重量%
Na  640ppm
Al2O35.0重量%
SiO274.9重量%
SiO2/Al2O3摩尔比 25.4
吸附重量%
环己烷  9.1
正己烷  14.9
H2O 16.8
表面积m2/g 479
实施例10
取实施例9的25克数量的固体结晶物放在538℃氮气流中灼烧5小时，继之用5%氧气（其余是氮气）在538℃吹扫另外16小时。
将每个有3克灼烧物的试样各自用100ml的0.1N TEABr，TPABr和La Cl3溶液进行离子交换。每次交换都在常温下进行24小时并重复三次。交换后的试样通过过滤收集。水洗到无卤化物并干燥，交换后的试样的组成列于下表，表明本结晶硅酸盐对不同离子的交换能力。
交换离子  TEA  TPA  La
离子的组成，重量%
Na  0.095  0.0089  0.063
N  0.30  0.38  0.03
C  2.89  3.63  -
La  -  -  1.04
实施例11
将上面用La交换过的试样用14到25目筛过筛，将14到15目之间的粒子在空气中在538℃灼烧3小时，灼烘物具有阿尔法值173。
实施例12
将实施例11中用La交换过的物质的灼烧过的试样被在100%蒸汽中通入649℃温度下的剧热蒸汽达2小时之久。通过蒸汽的试样具有阿尔法值22，表明由此得到的结晶硅酸盐在严格的水热处理的条件下具有良好的稳定性。
实施例13
为了制备具有X组分为硼的本结晶，将17.5克的硼酸加入到含6.75克45%  KOH溶液和290克水的溶液中，再往其中加入57.8克Ultrasil氧化硅，将此混合物充分搅匀，往此混合物中加入26.2克的六甲撑亚胺。
反应混合物具有下面以摩尔比表示的如下组成：
SiO2/B2O3＝6.1
OH-/SiO2＝0.06
H2O/SiO2＝19.0
K/SiO2＝0.06
R/SiO2＝0.30
式中R是六甲撑亚胺。
将混合物放在一只带搅拌的不锈钢反应釜中，在150℃下结晶8天。结晶物被过滤，水洗，在120℃干燥。部分结晶在540℃下灼烧6小时后，测得有下面的吸附力：
H2O（12乇） 11.7重量%
环己烷（40乇）  7.5重量%
正己烷（40乇）  11.4重量%
灼烧过的结晶物的表面积经测定为405m2/g。
灼烧物的化学组成经测定如下：
N  1.94重量%
Na  175ppm
K  0.60重量%
硼  1.04重量%
Al2O3920ppm
SiO275.9重量%
灰份  74.11重量%
SiO2/Al2O3，摩尔比 ＝1406
SiO2/（Al+B）2O3，摩尔比 ＝25.8
实施例14
将实施例13的部分灼烧过的结晶产物用NH4Cl处理后再灼烧，最后的结晶产物用阿尔法测试法进行测试，发现阿尔法值为1。
实施例15
为制备具有X组分为硼的本结晶物，将35.0克硼酸加入到由15.7克50%NaOH溶液和1160克水组成的溶液中，往此溶液加入240克Hisil氧化硅，继之加入105克六甲撑亚胺。反应混合物具有以摩尔比表示的如下组成
SiO2/B2O3＝12.3
OH/SiO  ＝0.056
H2O/SiO2＝18.6
Na/SiO2＝0.056
R/SiO2＝0.30
式中R是六甲撑亚胺
将混合物放在一只带搅拌的不锈钢釜中，在300℃下结晶9天。结晶物经过滤，水洗，在120℃干燥。灼烧物（540℃下6小时）的吸附力经测定为：
H2O（12乇） 14.4重量%
环己烷（40乇）  4.6重量%
正己烷（40乇）  14.0重量%
灼烧过的结晶物的表面积经测量为438m2/g
灼烧物的化学组成经测定为：
成份  重量%
N  2.48
Na  0.06
硼  0.83
Al2O30.50
SiO273.4
SiO2/Al2O3摩尔比＝249
SiO2/（Al+B）2O3摩尔比＝28.2
实施例16
将实施例15的部分灼烧过的结晶物用阿尔法测试进行测定，其阿尔法值为5。
实施例17
为了说明在本发明的方法中使用含至少30%固体氧化硅作氧化硅原料的重要性，将实施例3加以重复，只是将Q-Brand硅酸钠（仅含约29重量%固体硅）用作氧化硅原料。在本实施例中，将67.6克硫酸铝溶解在38.1克H2SO4（96.1%）和400克水的溶液中，将配成的溶液与120克六甲撑亚胺混合后加入由712.5克Q-Brand硅酸钠（28.8%SiO2和8.9%Na2O）和351克水组成的混合物中，配成的混合物具有以摩尔比表示的下列组成：
SiO2/Al2O3＝30.0
OH-/SiO2＝0.18
H2O/SiO2＝19.4
Na/SiO2＝0.60
R/SiO2＝0.35
经充分混合后，边搅拌边在一只不锈钢釜中，在246℃下结晶8天。产物的固体用过滤与未反应部分分离，水洗后在120℃干燥。产物用X射线衍射法分析，发现其是地定形物质，Magadiite和发光沸石的混合物。没有发现有本发明中的结晶物质。
实施例18
本实施例中，将本发明的结晶物的丙烯水合物的性能与按美国专利4439409实施例4中制备的Z  SM-12和P  SH-3的同类物加以比较。
本发明的结晶物制备如下，将15.9重量份的六甲撑亚胺加入到含3.5份50%NaOH，3.5份硅酸钠，30.1份Ultrasil VN3氧化硅和156份去离子水的混合物中。将反应混合物放在一只反应釜中在搅拌下直接加热到290°F（143℃），在那个温度下进行结晶。结晶充分完成后，将生成的结晶用过滤将其与残液分离。水洗后干燥。部分结晶与氧化铝合并以形成由沸石65重量份和氧化铝35重量份的混合物，往此混合物中加入足量的水，使得最后形成的催化剂能被成形为挤塑品。此催化剂通过在氮气中在1000°F（540℃）下灼烧。继之用含水的1.0N硝酸铵交换，再在空气中在1000-1200°F（540-650℃）灼烧，使之活化。
通过将1重量份的Z  SM-12晶种到含41.5份Hi-sil233氧化硅，67.7份50%四乙基溴化胺，7.0份50%NaOH和165.4份去离子水的混合物中制得Z  SM-12。反应混合物放在一只反应釜中在搅拌下直接加热到280°F（138℃），在那个温度下进行结晶，待完全结晶之后，将形成的结晶用过滤与残液分离，水洗后干燥。部分结晶与氧化铝合并形成由65重量份沸石和35份氧化铝的混合物。往此混合物中加入足量的水，使得形成的催化剂能够成形为挤塑品。将此催化剂先在氮气中1000°F（540℃）灼烧，继之用含水的1.0N硝酸胺交换，再在1200°F（650℃）下灼烧使之活化。
在温度330°F（166℃），压力1000psig（7000kpa）和丙烯的重量时空速度为0.6下导入丙烯水合物，将形成物放在蒸汽中2天后与下面表Ⅸ的进行比较。
表Ⅸ
P  SH-3  本发明的材料  Z  SM-12
%丙烯转化率  1.9  27.8  10.8
%水转化率  5.7  33.7  8.1
IPA选择性  88.7  76.7  74.6
DIPE选择性  2.9  22.3  23.1
齐聚物选择性  8.4  1.2  2.3
IPA＝异丙醇  DIPE＝二异丙醚
上述结果清楚表明，本发明的物质与P  SH-3和Z  SM-12两者比较，在达到高转化率方面，在对二异丙苯的良好选择性，在对丙烯齐聚物的低产率方面均显示出优良的性能。

Claims (10)

1、一种合成的多孔结晶物质，其特征是，其X射线衍射谱基本上包括了本专利说明书中表Ⅰ提出的诸值，而且具有大于10重量%水蒸汽，大于4.5重量%环已烷蒸气和大于10重量%正已烷蒸气的平衡吸附能力。
2、按权利要求1中提出的合成多孔结晶物质，其特征是，其X射线衍射谱基本上包括了本专利说明书中表Ⅱ提出的诸值。
3、按权利要求1中提出的合成多孔结晶物质，其特征是，其X射线衍射谱基本上包括了本专利说明书中表Ⅲ提出的诸值。
4、按权利要求1中提出的合成多孔结晶物质，其特征是，其X射线衍射谱基本上包括了本专利说明书中表Ⅳ提出的诸值。
5、按上述任一权利项中的结晶物质，其具有下述摩尔比例的组成物
X2O3＝（n）YO2，
式中n至少10，X是三价元素，Y是四价元素。
6、按权利要求5的结晶物质，其中X由铝组成，Y由硅组成。
7、按权利要求6的结晶物质，其中n从20至40。
8、一种制备权利要求5的合成结晶物质的方法，所述方法其构成为：制备能在结晶后形成所述物质的反应混合物（所述的反应混合物含足量的碱或碱土金属阳离子，含至少30重量%固体YO2的四价Y氧化物的原料，三价X氧化物的原料，水和六甲撑亚胺）以及将所述的反应混合物保持在能满足结晶的诸条件下，直至所述的物质的结晶形成为止。
9、按权利要求8的方法，其中所述的反应混合物的摩尔比具有下述的组成范围。
YO2/X2O3＝10至80
H2O/YO2＝5至100
OH-/YO2＝0.01至1.0
M/YO2＝0.01至2.0
R/YO2＝0.05至1.0
式中R表示六甲撑亚胺，M表示碱或碱土金属。
10、按权利要求8的方法，其所述的反应混合物的摩尔比例具有下述的组成范围：
YO2/X2O3＝10至60
H2O/YO ＝10至60
OH-/YO2＝0.1至0.5
M/YO2＝0.1至1.0
R/YO2＝0.1至0.5
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CN101384366B (zh) * 2006-02-14 2011-12-14 埃克森美孚化学专利公司 一种用于制造分子筛的高生产量的方法
CN101495234B (zh) * 2006-07-28 2012-06-27 埃克森美孚化学专利公司 新型分子筛组合物，它的制造方法和使用方法
CN101489675B (zh) * 2006-07-28 2012-07-11 埃克森美孚化学专利公司 分子筛组合物（emm-10），其制造方法和用于烃转化的用途
CN101489677B (zh) * 2006-07-28 2012-12-26 埃克森美孚化学专利公司 Mcm-22家族分子筛组合物，其制造方法和用于烃转化的用途

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