CN103459353A - 固化成形物 - Google Patents

固化成形物 Download PDF

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CN103459353A
CN103459353A CN2012800162325A CN201280016232A CN103459353A CN 103459353 A CN103459353 A CN 103459353A CN 2012800162325 A CN2012800162325 A CN 2012800162325A CN 201280016232 A CN201280016232 A CN 201280016232A CN 103459353 A CN103459353 A CN 103459353A
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molding
weight
acid
inorganic fibre
solidifying agent
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CN103459353B (zh
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岸木智彦
三原彻也
米内山贤
石原铁也
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Nichias Corp
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Abstract

一种成形物，所述成形物由含有SiO2、碱土类金属的生物可溶性无机纤维构成，所述成形物中所述生物可溶性无机纤维的含量为20～99重量%，其中，固化剂从所述成形物的表面渗入，使得所述成形物的表面被固化，所述固化剂为胶体二氧化硅。

Description

固化成形物
技术领域
本发明涉及由进行了固化处理的无机纤维构成的成形物。
背景技术
无机纤维质量轻容易操作，而且耐热性优异，因此例如作为耐热性的封装材料使用。另一方面，近些年来，无机纤维被指出由于吸入人体而入侵肺部的问题。为此，开发了即便被吸入人体也不会引起问题或者难以引起问题的生物可溶性无机纤维。
然而，使用生物可溶性纤维制造的成形物，存在绝对强度低的缺点。
另外，在专利文献1中，公开了含有生物可溶性硅酸碱土类金属盐纤维和胶体二氧化硅的灰泥，通过将胶体二氧化硅作为粘结剂使用，从而可以发挥优异的贮藏稳定性，进一步通过含有EDTA（乙二胺四乙酸）等的螯合剂而能够进一步提高贮藏稳定性。
在专利文献2中，公开了为了抑制粉尘的发生而将硬硅钙石类硅酸钙板浸在无机粘结剂中。
现有技术文献
专利文献
专利文献1：日本特开2002-524384号公报
专利文献2：日本特开2008-13402号公报
发明内容
发明想要解决的课题
本发明是鉴于上述课题完成的发明，以提供由无机纤维构成的强度高的成形物作为其目的之一。
解决课题的手段
本发明者们通过专门研究的结果，发现用固化剂处理成形物可以提高强度从而完成了本发明。
通过本发明，可以提供以下的固化成形物及其固化方法。
1.一种成形物，其中，所述成形物由含有SiO2、碱土类金属的生物可溶性无机纤维构成，所述成形物中所述生物可溶性无机纤维的含量为20～99重量%，其中，固化剂从所述成形物的表面渗入，使得所述成形物的表面被固化，所述固化剂为胶体二氧化硅。
2.如1所述的成形物，其中，不含金属离子的螯合剂与所述固化剂一起渗入。
3.如2所述的成形物，其中，所述螯合剂为EDTA·H·3(NH4)或者EDTA·2H·2(NH4)。
4.如1所述的成形物，其中，酸与所述固化剂一起渗入。
5.如4所述的成形物，其中，所述酸为羟基酸。
6.如4所述的成形物，其中，所述酸为选自柠檬酸、苹果酸、酒石酸、水杨酸中的1种以上。
7.如1所述的成形物，其中，所述固化剂为酸性胶体二氧化硅或者阳离子型胶体二氧化硅。
8.如7所述的成形物，其中，所述酸性胶体二氧化硅的pH为2～5。
9.如1～8中任一项所述的成形物，其中，所述无机纤维为以下组成：
SiO2、ZrO2、Al2O3和TiO2的合计为50～82重量%，
碱金属氧化物和碱土类金属氧化物的合计为18～50重量%。
10.如1～8中任一项所述的成形物，其中，所述无机纤维为以下组成：
SiO2为50～82重量%，
CaO和MgO的合计为10～43重量%。
11.如1～8中任一项所述的成形物，其中，所述无机纤维为具有以下组成的镁硅酸盐纤维、或者具有以下组成的钙硅酸盐纤维，
[镁硅酸盐纤维]
SiO2   66～82重量%、
CaO   1～9重量%、
MgO   10～30重量%、
Al2O3   3重量%以下、
其它氧化物   小于2重量%；
[钙硅酸盐纤维]
SiO2   66～82重量%、
CaO   10～34重量%、
MgO   3重量%以下、
Al2O3   5重量%以下、
其它氧化物   小于2重量%。
12.一种成形物的固化方法，其中，在由含有SiO2、碱土类金属的生物可溶性无机纤维构成的成形物中，渗入含有胶体二氧化硅的固化处理液并干燥，所述成形物中所述生物可溶性无机纤维的含量为20～99重量%。
13.如12所述的成形物的固化方法，其中，所述固化处理液进一步含有螯合剂或者酸，所述螯合剂不含金属离子。
14.一种成形物，所述成形物通过12或13所述的固化方法固化得到。
通过本发明，可以提供由无机纤维构成的强度高的成形物。
附图说明
图1为实施例1的无机板的固化前后的表面的照片。
具体实施方式
本发明的固化成形物是通过使用固化剂对用含有SiO2、碱土类金属的无机纤维形成的成形物进行处理而得到的。固化剂可以使用胶体二氧化硅。胶体二氧化硅包括碱性胶体二氧化硅（pH8～10）、酸性胶体二氧化硅（pH2～6）或者阳离子型胶体二氧化硅等。
固化处理例如通过将成形物浸于固化处理液中来实施，或者通过涂布固化处理液（刷子涂布、滚筒涂布等）、喷涂（喷淋涂布、喷雾涂布等）来实施，固化处理后干燥。干燥时，溶剂从表面蒸发，因此，溶剂移动到表面上并且胶体二氧化硅也随着移动到表面。即使溶剂蒸发，胶体二氧化硅也会残留，因此，胶体二氧化硅会偏析于表面附近，其结果使得成形物的表面被固化。作为溶剂可以使用乙醇、丙醇等一元醇类、乙二醇等二元醇类等。
通过固化处理而含于成形物中的胶体二氧化硅的量，是使成形物的密度例如提高10～150%，优选为10%～100%，更加优选为10～50%的量。通常，将成形物浸于固形成分比率为10～30%的胶体二氧化硅中1秒～数分钟，不过不限定于此。也可以进行1次或者2次以上处理。进行了固化处理的成形物的水分量通常约为5重量%以下。水分量的确认通过干燥后的重量确认。
通过上述的固化处理，增大了硬度，提高了强度、操作性（持握时的手的印记、加工时的小缺损、切割时没有棱角、掉粉等的问题）。
作为固化剂如果使用碱性胶体二氧化硅来处理成形物，则固化处理液中碱土类金属离子、特别是Ca离子、Mg离子会溶出。该离子和固化剂在成形物表面反应，如果加热到800℃以上则会成为产生裂纹的原因。这被认为是因为二氧化硅和Ca离子等反应会引起体积变化。
为了抑制裂纹的产生，将成形物用不含金属离子的螯合剂和固化剂进行处理。螯合剂被认为是通过捕获溶出的碱土类金属的同时形成保护层，从而抑制碱土类金属和固化剂的反应，由此防止裂纹的产生。螯合剂由于具有2个以上的供电子基团，因而可以形成金属螯合剂化合物。在供电子基团上，具有羧基、羟基等。本发明中使用的螯合剂不含碱土类金属或者碱金属。作为螯合剂的例子，可以列举EDTA（乙二胺四乙酸）·H·3(NH4)的组成的螯合剂、EDTA·2H·2(NH4)的组成的螯合剂等。
和螯合剂并用的固化剂可以使用胶体二氧化硅，可以使用碱性胶体二氧化硅、酸性胶体二氧化硅、阳离子型胶体二氧化硅等。螯合剂的浓度可以适当设定，不过在使用碱性胶体二氧化硅作为固化剂的情况下，优选相对于固形成分为10重量%的固化处理液，碱性胶体二氧化硅的浓度为0.5重量%以上。
另外，为了抑制裂纹的产生，可以将成形物用pH为6以下（优选为pH1～6、进一步优选为2～5，特别优选为pH3～5）的固化处理液进行处理。认为通过使之为酸性，抑制碱土类金属的溶出，从而抑制碱土类金属和固化剂的反应，由此防止裂纹的产生。
具体而言，将成形物用酸和固化剂进行处理。酸可以为弱酸也可以为强酸，作为弱酸，可以列举柠檬酸、苹果酸、酒石酸、水杨酸、乙醇酸、乳酸、扁桃酸、二苯乙醇酸、香豆酸、醋酸等，作为强酸，可以列举硫酸、盐酸、硝酸等。由于弱酸没有产生气体的问题，因此优选弱酸。
另外，也可以使用酸性（例如pH1～6或者2～5）的胶体二氧化硅。作为酸性胶体二氧化硅，可以使用SILICADOL20A（日本化学工业株式会社制造，固形成分比率为20%）、CATALOID SN（日挥触媒化成株式会社制造，固形成分比率为20%）等的市售品。
作为具有螯合剂效果和使pH呈酸性这两种性质的物质，可以列举柠檬酸、苹果酸、酒石酸、水杨酸等羟基酸。
另外，作为固化剂，如果使用阳离子型胶体二氧化硅（例如，pH4～6），可以抑制碱土类金属的溶出。发明者们认为这种情况下，阳离子型胶体二氧化硅在表面形成保护膜，从而抑制碱土类金属和固化剂的反应。阳离子型胶体二氧化硅是指表面上具有正电荷的胶体二氧化硅。例如，可以列举在胶体二氧化硅的表面或者内部含有铝离子等多价金属离子的化合物或者有机阳离子性化合物，从而使二氧化硅粒子表面呈阳离子性并带电的胶体二氧化硅。作为阳离子型胶体二氧化硅，可以使用SNOWTEX AK（日产化学工业株式会社制造，固形成分比率18%）等的市售品。
本发明的成形物通过含有无机纤维而构成。例如，由20～99重量%（优选为30～95重量%）无机纤维构成，无机纤维优选为以SiO2、CaO、MgO为主要成分。主要成分是指将其合计时构成90重量%以上或者95重量%以上。
无机纤维可以是以下组成的生物可溶性纤维。
SiO2、ZrO2、Al2O3和TiO2的合计   50重量%～82重量%
碱金属氧化物和碱土类金属氧化物的合计   18重量%～50重量%
另外，无机纤维可以为以下组成的生物可溶性纤维。
SiO2   50～82重量%
CaO和MgO的合计   10～43重量%
生物可溶性纤维可以大致分为含有较多MgO的镁硅酸盐纤维、含有较多CaO的钙硅酸盐纤维。作为镁硅酸盐纤维可以例举以下的组成。
SiO2   66～82重量%
CaO   1～9重量%
MgO   10～30重量%
Al2O3   3重量%以下
其它氧化物   小于2重量%
作为钙硅酸盐纤维可以例举以下的组成。
SiO2   66～82重量%（例如，可以为68～80重量%、70～80重量%、71～80重量%或者71～76重量%。）
CaO   10～34重量%（例如，可以为18～32重量%、20～30重量%、20～27重量%或者21～26重量%。）
MgO   3重量%以下（例如，可以为1重量%以下）
Al2O3   5重量%以下（例如，可以为3.5重量%以下、3.4重量%以下或者3重量%以下。另外，可以为1重量%以上，1.1重量%以上或者2重量%以上。）
其它氧化物   小于2重量%
如果SiO2在上述范围内则耐热性优异。如果CaO和MgO在上述范围内则加热前后的生物可溶性优异。如果Al2O3在上述范围内则耐热性优异。
另外，SiO2、CaO、MgO、Al2O3的合计超过98重量%或者超过99重量%即可。
上述生物可溶性无机纤维中，作为其它成分，可以含有从碱金属氧化物（K2O、Na2O、Li2O等），选自Sc、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y或其混合物的各种氧化物，以及Fe2O3、ZrO2、TiO2、P2O5、B2O3、MnO、ZnO、SrO、BaO、Cr2O3等中选出的1种以上，也可以不含有。其它氧化物可以分别为1.0重量%以下、0.2重量%以下或者0.1重量%以下。碱金属氧化物的各氧化物可以分别为1.0重量%以下、0.2重量%以下或者0.1重量%以下。另外，碱金属氧化物的合计可以为1.0重量%以下、0.2重量%以下或者0.1重量%以下。
另外，生物可溶性纤维中，可以在SiO2和碱土类金属氧化物（例如MgO和CaO的至少一者）之上，进一步含有其它成分。例如可以进一步含有选自氧化铝（Al2O3）、氧化钛（TiO2）、氧化锆（ZrO2）、氧化铁（Fe2O3）、氧化锰（MnO）、氧化钾（K2O）中的1种或者2种以上。
生物可溶性无机纤维是，例如在40℃下生理盐水溶解率为1%以上的无机纤维。
生理盐水溶解率例如可以通过以下方式测定。具体而言，首先将无机纤维粉碎至200目以下调制得到的样品1g和150mL生理盐水装入三角烧瓶（容积为300mL）中，设置于40℃的恒温箱。接下来，对于三角烧瓶，施加每分钟120转的水平震动并持续50小时。之后，通过ICP发射光谱装置测定过滤得到的滤液中所含的各元素的浓度（mg/L）。然后基于测定的各元素的浓度和溶解前的无机纤维中各元素的含量（质量%），算出生理盐水溶解率（%）。即，例如在测定元素为硅（Si）、镁（Mg）、钙（Ca）以及铝（Al）的情况下，通过下述式子算出生理盐水的溶解率C（%）；C（%）=[滤液量（L）×（a1+a2+a3+a4）×100]／[溶解前的无机纤维的质量（mg）×（b1+b2+b3+b4）／100]。在该式子中，a1、a2、a3和a4分别是测定的硅、镁、钙以及铝的浓度（mg/L），b1、b2、b3和b4分别是溶解前的无机纤维中的硅、镁、钙和铝的含量（质量%）。
成形物是由无机纤维制作的物体，不包括灰泥等的不定型物（也可含无机和/或有机粘结剂），例如可以列举模具、毯状物、块状物、板状物、纸张、毛毡等。另外，本发明的由无机纤维构成的成形物不包括专利文献2所述的硬硅钙石类硅酸钙板。
成形物中，除了无机纤维之外还可以含有有机粘结剂、无机粘结剂、无机填料等。这些只要不损害本发明的效果都可以使用通常使用的物质，例如作为有机粘结剂可以使用淀粉、丙烯酸树脂、聚丙烯酰胺、纸浆、丙烯酸乳液等，作为无机粘结剂，可以例举阴离子性胶体二氧化硅、阳离子性胶体二氧化硅等胶体二氧化硅、氧化铝溶胶、膨润土、粘土矿物等。
本发明的固化成形物因为是通过上述的处理得到的，因此固化剂从其表面渗入。
实施例
制造例1
<有机和无机板（成形物）的制造>
由生物可溶性纤维A（其中，SiO2含量为73质量%，CaO含量为25质量%、MgO含量为0.3质量%、Al2O3含量为2质量%）90重量%、淀粉和聚丙烯酰胺（有机粘结剂）、胶体二氧化硅（无机粘结剂），制造长300mm、宽300mm、厚50mm（密度为250kg/m3）的有机板。
进一步，由生物可溶性纤维A85重量%、胶体二氧化硅和氧化铝溶胶和膨润土（无机粘结剂）、无机粉体（二氧化硅、锆石、碳酸钙、氧化锆、堇青石、硅灰石等）、丙烯酰胺（有机粘结剂）制造长300mm、宽300mm、厚50mm（密度250kg/m3）的无机板。
制造例2
<有机和无机板（成形物）的制造>
除了代替生物可溶性纤维A，使用生物可溶性纤维B（其中，SiO2含量为76质量%、CaO含量为4质量%、MgO含量为18质量%、Al2O3含量为2质量%）之外，其它都和制造例1同样，制造有机和无机板。
实施例1
<固化处理>
将在制造例1中得到的有机板和无机板（密度250kg/m3）用由碱性胶体二氧化硅构成的固化液（pH约为9，溶剂为水）处理（浸渍1～10秒），固化表面使之干燥。密度为300kg/m3。固化之后强度提高。将固化前后的无机板的表面的照片示于图1。进一步，使用硬度计（ASKER制造：Asker橡胶硬度计C型）测定固化了的有机和无机板的硬度。结果示于表1中。
比较例1
将在制造例1中得到的有机和无机板不经过固化处理进行评价。有机和无机板都很脆。和实施例1同样测定硬度。结果示于表1中。
[表1]
Figure BDA0000389779490000091
实施例2
<固化处理>
除了使用在制造例2中得到的有机板和无机板之外，和实施例1同样固化测定了硬度。结果示于表2中。
比较例2
对在制造例2中得到的有机和无机板不进行固化处理而评价。有机和无机板都很脆。和实施例1同样测定硬度。结果示于表2中。
[表2]
Figure BDA0000389779490000092
实施例3
[螯合剂和固化剂]
<固化处理>
将在制造例1中得到的有机和无机板用由EDTA二铵盐和碱性胶体二氧化硅构成的固化处理液（pH约为9，溶剂：水）处理，将表面固化干燥。相对于固形成分为10重量%的固化处理液使用1重量%的螯合剂。
<加热试验>
将固化了的有机和无机板，在800℃、900℃、1000℃、1100℃加热24小时，目视观察外观（裂纹的有无）。为了比较将实施例1中得到的固化了的有机和无机板同样加热观察。将正常的表示为◎，表面上产生小的裂纹的表示为○，产生大的裂纹的表示为▲，产生破裂的表示为×。结果示于表3中。
[表3]
800℃ 900℃ 1000℃ 1100℃
碱性胶体二氧化硅 有机板 ◎ ○ ▲ ×
碱性胶体二氧化硅 无机板 ◎ ◎ ◎ ▲
碱性胶体二氧化硅+螯合剂 有机板 ◎ ◎ ◎ ◎
碱性胶体二氧化硅+螯合剂 无机板 ◎ ◎ ◎ ◎
实施例4
[酸和固化剂]
<固化处理>
将制造例1中得到的有机和无机板，用由酸和碱性胶体二氧化硅（固化剂）构成的固化处理液处理，固化表面并干燥。作为酸，相对于固形成分为10重量%的固化处理液使用约为1重量%的柠檬酸、苹果酸、酒石酸、水杨酸，处理液的pH为3～4。
<加热试验>
和实施例3同样实施。结果示于表4、5中。
[表4]
Figure BDA0000389779490000101
[表5]
Figure BDA0000389779490000111
实施例5
[酸和固化剂]
<固化处理>
将在制造例中得到的有机和无机板，用由柠檬酸和碱性胶体二氧化硅（固化剂）构成的固化处理液进行处理，将表面固化并干燥。柠檬酸使用0.4重量%、0.6重量%、1.5重量%、8重量%，处理液的pH调节为2～5。
<加热试验>
和实施例3同样实施。结果示于表6中。
[表6]
Figure BDA0000389779490000112
Figure BDA0000389779490000121
实施例6
[酸和固化剂]
<固化处理>
除了使用在制造例2中得到的有机板和无机板之外，其它都和实施例4同样实施。
<加热试验>
和实施例4同样实施。为了比较，将实施例2中得到的固化了的有机和无机板同样加热观察。结果示于表7、8中。
[表7]
[表8]
Figure BDA0000389779490000131
实施例7
[酸性胶体二氧化硅和阳离子型胶体二氧化硅]
<固化处理>
将在制造例1中得到的有机板和无机板用酸性胶体二氧化硅（SILICADOL20A（日本化学工业株式会社制造），pH2～4）或者阳离子型胶体二氧化硅（SNOWTEX AK，日产化学工业株式会社制造）（固化剂）进行处理，固化表面并干燥。
<加热试验>
按照和实施例3同样实施。结果示于表9、10。
[表9]
Figure BDA0000389779490000132
实施例8
[酸性胶体二氧化硅和阳离子型胶体二氧化硅]
<固化处理>
除了使用在制造例2中得到的有机板和无机板之外，其它都和实施例7同样实施。
<加热试验>
和实施例7同样实施。结果示于表11、12中。
[表11]
[表12]
Figure BDA0000389779490000142
产业上的利用可能性
本发明的固化成形物可以用于通常高温用隔热材料、窑炉的顶棚、炉壁的隔热材料用内衬材料、隔热材料、支撑材料的各种用途中。
上述详细说明了本发明的几个实施方式和/或实施例，不过本领域技术人员容易在这些所例举的实施方式和/或实施例中加入更多的变化，而不实质性地偏离本发明的新颖的教导和效果。因此，这些更多的变化也包含于本发明的范围之内。
该说明书中记载的文献的内容都在此引用。

Claims (14)

1.一种成形物，其中，
所述成形物由含有SiO2、碱土类金属的生物可溶性无机纤维构成，所述成形物中所述生物可溶性无机纤维的含量为20～99重量%，其中，固化剂从所述成形物的表面渗入，使得所述成形物的表面被固化，所述固化剂为胶体二氧化硅。
2.如权利要求1所述的成形物，其中，
不含金属离子的螯合剂与所述固化剂一起渗入。
3.如权利要求2所述的成形物，其中，
所述螯合剂为EDTA·H·3(NH4)或者EDTA·2H·2(NH4)。
4.如权利要求1所述的成形物，其中，
酸与所述固化剂一起渗入。
5.如权利要求4所述的成形物，其中，
所述酸为羟基酸。
6.如权利要求4所述的成形物，其中，
所述酸为选自柠檬酸、苹果酸、酒石酸、水杨酸中的1种以上。
7.如权利要求1所述的成形物，其中，
所述固化剂为酸性胶体二氧化硅或者阳离子型胶体二氧化硅。
8.如权利要求7所述的成形物，其中，
所述酸性胶体二氧化硅的pH为2～5。
9.如权利要求1～8中任一项所述的成形物，其中，
所述无机纤维为以下组成：
SiO2、ZrO2、Al2O3和TiO2的合计为50～82重量%，
碱金属氧化物和碱土类金属氧化物的合计为18～50重量%。
10.如权利要求1～8中任一项所述的成形物，其中，
所述无机纤维为以下组成：
SiO2为50～82重量%，
CaO和MgO的合计为10～43重量%。
11.如权利要求1～8中任一项所述的成形物，其中，
所述无机纤维为具有以下组成的镁硅酸盐纤维或者具有以下组成的钙硅酸盐纤维，
镁硅酸盐纤维：
SiO2   66～82重量%、
CaO   1～9重量%、
MgO   10～30重量%、
Al2O3   3重量%以下、
其它氧化物   小于2重量%；
钙硅酸盐纤维：
SiO2   66～82重量%、
CaO   10～34重量%、
MgO   3重量%以下、
Al2O3   5重量%以下、
其它氧化物   小于2重量%。
12.一种成形物的固化方法，其中，
在由含有SiO2、碱土类金属的生物可溶性无机纤维构成的成形物中，渗入含有胶体二氧化硅的固化处理液，并干燥，所述成形物中所述生物可溶性无机纤维的含量为20～99重量%。
13.如权利要求12所述的成形物的固化方法，其中，
所述固化处理液进一步含有螯合剂或者酸，所述螯合剂不含金属离子。
14.一种成形物，其中，所述成形物通过权利要求12或13所述的固化方法固化得到。
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