CN110337426A - 碳酸钙多孔烧结体的制造方法 - Google Patents

碳酸钙多孔烧结体的制造方法 Download PDF

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CN110337426A
CN110337426A CN201880013713.8A CN201880013713A CN110337426A CN 110337426 A CN110337426 A CN 110337426A CN 201880013713 A CN201880013713 A CN 201880013713A CN 110337426 A CN110337426 A CN 110337426A
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calcium carbonate
sintered body
porous sintered
manufacturing
foaming
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田近正彦
梅本奖大
岛井骏蔵
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Shiraishi Central Laboratories Co Ltd
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Abstract

本发明提供一种能够简易地制造碳酸钙多孔烧结体的制造方法。该制造方法的特征在于，包括：制备含有碳酸钙和胶凝剂的分散液的工序；向分散液添加发泡剂后进行搅拌来使其发泡，从而制作发泡体的工序；使发泡体凝胶化的工序；和通过将凝胶化的发泡体进行烧结来制造碳酸钙多孔烧结体的工序。

Description

碳酸钙多孔烧结体的制造方法
技术领域
本发明涉及碳酸钙多孔烧结体的制造方法。
背景技术
碳酸钙烧结体被期待应用于人工珍珠的成长核、生物体用途等，对于其制造方法已有各种研究。在现有的碳酸钙烧结体的制造方法中，一般而言，将碳酸钙和烧结助剂的混合物通过静液压压制制成成型体，之后将该成型体在碳酸气体气氛中进行烧结来制造(专利文献1和非专利文献1)。
现有技术文献
专利文献
专利文献1：日本特开2007－254240号公报
非专利文献
非专利文献1：都祭聪子等“起始物质对于碳酸钙的烧结的影响”无机物质学会学术演讲会演讲要旨集Vol.105th P.46－47(2002.11.14)
发明内容
发明要解决的技术问题
通过将碳酸钙烧结体制成多孔质，能够提高碳酸钙烧结体的表面积，能够制成在生物体用途等各种用途中有用的碳酸钙烧结体。从这样的观点出发，期望开发相比于现有技术能够更简易地制造碳酸钙多孔烧结体的方法。
本发明的目的在于提供一种能够简易地制造碳酸钙多孔烧结体的制造方法。
用于解决技术问题的技术手段
本发明的制造方法的特征在于，包括：制备含有碳酸钙和胶凝剂的分散液的工序；向分散液添加发泡剂后进行搅拌而使其发泡，从而制作发泡体的工序；使发泡体凝胶化的工序；和通过将凝胶化的发泡体进行烧结来制造碳酸钙多孔烧结体的工序。
在本发明中，分散液中可以含有烧结助剂。这种情况下，作为烧结助剂，可以举出含有锂、钠和钾中的至少2种的碳酸盐或氟化物、并且熔点在600℃以下的烧结助剂。
分散液中优选含有20体积％以上的碳酸钙。
烧结的工序优选为在进行预烧结后进行正式烧结的工序。
优选预烧结的温度在200～500℃的范围内，正式烧结的温度为预烧结的温度以上并且在420～600℃的范围内。
作为碳酸钙，例如，优选使用利用透射式电子显微镜观察测定的粒径分布中的平均粒径(D50)在0.05～0.30μm的范围内的碳酸钙。碳酸钙的BET比表面积优选为5～25m2/g。
在本发明中，碳酸钙的纯度可以为99.9质量％以上。通过使用杂质含量少的高纯度碳酸钙，即使不添加烧结助剂也能够制造多孔烧结体。此时的碳酸钙的纯度优选为99.9质量％以上，更优选为99.99质量％以上。
本发明的用于制造碳酸钙多孔烧结体的碳酸钙的特征在于，纯度为99.9质量％以上。
发明效果
依据本发明，能够简易地制造碳酸钙多孔烧结体。
附图说明
图1是示出实施例1的碳酸钙多孔烧结体的扫描电子显微镜照片(倍率25倍)。
图2是示出实施例1的碳酸钙多孔烧结体的扫描电子显微镜照片(倍率150倍)。
图3是示出实施例1的碳酸钙多孔烧结体的扫描电子显微镜照片(倍率5000倍)。
图4是示出实施例1的碳酸钙多孔烧结体的扫描电子显微镜照片(倍率20000倍)。
具体实施方式
下面，对优选的实施方式进行说明。但是，以下的实施方式仅为例示，本发明不受以下的实施方式的限定。
(碳酸钙)
本发明中使用的碳酸钙只要能够用于制造碳酸钙多孔烧结体即可，没有特别限定。从能够制造具有致密的壁部的多孔烧结体的观点出发，优选为利用透射式电子显微镜观察测定的粒径分布中的平均粒径(D50)在0.05～0.30μm范围内的碳酸钙。
利用透射式电子显微镜观察测定的粒径分布中的平均粒径(D50)优选在0.05～0.30μm的范围内，更优选在0.08～0.25μm的范围内，更加优选在0.10～0.20μm的范围内。通过将平均粒径(D50)设为这样的范围内，能够制造具有致密的壁部的多孔烧结体。关于利用透射式电子显微镜观察得到的粒径分布，能够通过利用透射式电子显微镜观察对1000个以上作为测定对象的碳酸钙进行测定来求得。
本发明中使用的碳酸钙，例如能够通过普遍已知的向石灰乳中吹入碳酸气体而进行反应的碳酸气体化合法来制造。特别是平均粒径(D50)超过0.1μm的颗粒能够依据日本专利第0995926号的制造方法制造。
本发明中使用的碳酸钙的BET比表面积优选为5～25m2/g，更优选为7～20m2/g，更加优选为8～15m2/g。通过将BET比表面积设为上述的范围内，能够提高碳酸钙的烧结性。因此，能够制造具有致密的壁部的多孔烧结体。
本发明中使用的碳酸钙的纯度优选为99.0质量％以上，更优选为99.5质量％以上，更加优选为99.6质量％以上。
在本发明中，能够使用纯度为99.7质量％以上的高纯度碳酸钙。通过使用高纯度碳酸钙，能够减少烧结所需要的烧结助剂的量。另外，也能够不使用烧结助剂而进行烧结。纯度优选为99.8质量％以上，更优选为99.9质量％以上，更加优选为99.95质量％以上。这样的高纯度碳酸钙例如能够通过日本特开2012－240872号公报公开的方法制造。
此外，高纯度碳酸钙的纯度的上限值没有特别限定，一般而言为99.9999质量％。
(烧结助剂)
本发明中使用的烧结助剂只要能够使碳酸钙烧结而制造多孔烧结体即可，可以没有特别限定地使用。作为烧结助剂，例如可以举出含有锂、钠和钾中的至少2种的碳酸盐、并且熔点在600℃以下的烧结助剂。烧结助剂的熔点优选在550℃以下，更优选在530℃以下，更加优选在450～520℃的范围。通过将烧结助剂的熔点设为上述范围，能够在更低温进行烧制而制造碳酸钙多孔烧结体。烧结时，由于添加至碳酸钙中来使用，所以实际的熔点比上述的温度更低，因此能够作为烧结助剂充分地发挥功能。烧结助剂优选为碳酸钾和碳酸锂的混合物。烧结助剂的熔点例如能够从相图求得，也能够利用差示热分析(DTA)测定。
另外，可以举出含有锂、钠和钾中的至少2种的氟化物、并且熔点在600℃以下的烧结助剂。这样的烧结助剂也优选具有上述的熔点范围。作为这样的烧结助剂，例如可以举出氟化钾、氟化锂和氟化钠的混合物。具体而言，例如可以举出具有氟化钾10～60摩尔％、氟化锂30～60摩尔％和氟化钠0～30摩尔％的组成范围的混合物。通过设为这样的范围，能够在更低的温度进行烧制，来制造具有致密的壁部的碳酸钙多孔烧结体。
相对于碳酸钙和烧结助剂的合计，烧结助剂的含有比例优选在0.1～3.0质量％的范围内，更优选在0.2～2.5质量％的范围内，更加优选在0.3～2.0质量％的范围内。烧结助剂的含有比例过少时，有时碳酸钙不能充分烧结。烧结助剂的含有比例过多时，有时不能提高碳酸钙多孔烧结体的壁部的密度。
(胶凝剂)
本发明的分散液中含有胶凝剂。通过含有胶凝剂，发泡后的分散发泡体中的气泡的强度上升，能够使发泡体的形状稳定化。作为胶凝剂，可以举出甲基纤维素等多糖类、异丁烯―马来酸酐共聚物的碱水溶性聚合物等。
相对于碳酸钙100质量份，分散液中的胶凝剂的含量优选为0.1～5质量份的范围，更优选为0.5～3质量份的范围。胶凝剂的含量过少时，不能提高发泡体中的气泡的强度，有时不能使发泡体的形状稳定化。胶凝剂的含量过多时，有时不能得到与含量成比例的上述效果。
(分散液)
在本发明中，优选一边向水等分散介质缓缓地添加碳酸钙，一边利用分散机、混合机、球磨机等搅拌力强的装置将碳酸钙分散于分散介质中。在需要烧结助剂的情况下，一般添加在分散液中。碳酸钙的含量一般而言在分散液中优选为30～70质量％。此时，如有需要，可以相对于碳酸钙100质量份，添加0～3质量份左右的聚丙烯酸盐等高分子表面活性剂作为分散剂。
胶凝剂能够在碳酸钙的添加前、添加后、或者添加碳酸钙的同时添加至分散介质中。
(发泡剂)
作为本发明中使用的发泡剂，可以举出月桂基硫酸三乙醇胺等烷基硫酸酯盐、聚氧乙烯烷基醚硫酸酯盐、聚氧乙烯烷基醚乙酸盐、烷基聚葡萄糖苷等。
(发泡体的制作)
在本发明中，通过向上述分散液中添加发泡剂后进行搅拌而使其发泡，由此制作发泡体。发泡剂优选以分散液中的发泡剂的浓度达到0.01～5质量％左右的方式添加，更优选以达到0.1～3质量％左右的方式添加。搅拌优选使用手持混合机、分散机等进行。通过进行搅拌，有时分散液的温度会上升，因此如有需要，可以一边冷却分散液，一边进行搅拌。
(发泡体的凝胶化)
在本发明中，将所制得的发泡体凝胶化。通过将发泡体凝胶化，能够在烧结时保持发泡体的形状。作为进行凝胶化的方法，可以举出：通过利用分散液中的钙离子来形成交联结构，从而进行凝胶化的方法；利用胶凝剂自身的温度特性来促进凝胶化的方法等。
凝胶化后的发泡体优选在经过干燥去除至少一部分的水分后，进行烧结。干燥温度优选为30～200℃的范围。
(发泡体的烧结)
在本发明中，通过将凝胶化后的发泡体进行烧结来制造碳酸钙多孔烧结体。在本发明中，优选在进行预烧结后进行正式烧结。由此，能够防止发泡体中所含的有机成分残留、碳化而变黑或者有机成分发生剧烈分解而导致烧结体产生裂纹的情况。
预烧结的温度优选在200～500℃的范围内，更优选在300～420℃的范围内。正式烧结的温度优选在预烧结的温度以上并且在420～600℃的范围内，更优选在450～540℃的范围内。
另外，预烧结和正式烧结时的升温速度优选在2～20℃/分钟的范围内。由此，能够防止因有机成分发生剧烈分解而导致烧结体产生裂纹的情况。
烧结时的气氛优选为空气中。然而，本发明不限定于此，也可以在碳酸气体气氛中或者在氮气等不活泼气体气氛中进行烧结。依据本发明，即使在空气中进行烧结，也能够制造碳酸钙多孔烧结体。
(碳酸钙多孔烧结体)
本发明的碳酸钙多孔烧结体的气孔率优选在50体积％以上，更优选在60体积％以上，更优选在70体积％以上，更加优选在80体积％以上，特别优选在82体积％以上。由此，能够将碳酸钙多孔烧结体用于生物体用途等。此外，碳酸钙多孔烧结体的气孔率的上限值没有特别限定，一般而言为95体积％。
本发明的碳酸钙多孔烧结体中，优选形成有连通至烧结体外部的连通孔。由此，能够容易地使多孔烧结体内部的碳酸钙与外部的气氛接触。因此，能够更好地用于例如生物体用途等。
实施例
下面，对依据本发明的具体的实施例进行说明，但是本发明不受这些实施例的限定。
＜实施例1＞
(碳酸钙)
使用纯度为99.61质量％、平均粒径(D50)为0.15μm、BET比表面积为10m2/g的碳酸钙。利用透射式电子显微镜观察测定1500个作为测定对象的碳酸钙颗粒的粒径，从粒径分布求出平均粒径(D50)。使用岛津制造所制造的FlowSorb 2200，利用1点法测定BET比表面积。利用差量法导出纯度。具体而言，使用电感耦合等离子体发光分析装置，测定溶解有质量已知的试样的检测液中的杂质量，将得到的结果的和作为杂质含量，将从整体中减去杂质含量的值作为纯度。
使用上述碳酸钙，如下所述操作，制造碳酸钙多孔烧结体。
(分散液的制备)
将离子交换水55质量份、碳酸钙100质量份、甲基纤维素0.55质量份、特殊聚羧酸型高分子表面活性剂2.5质量份(有效份数1.0质量份)、碳酸钾0.32质量份和碳酸锂0.28质量份利用均匀分散机进行混合，得到分散液。甲基纤维素为胶凝剂，特殊聚羧酸型高分子表面活性剂为分散剂，碳酸钾和碳酸锂为烧结助剂。
(发泡体的制作)
向所得到的分散液中，添加作为发泡剂的月桂基硫酸三乙醇胺0.97质量份(有效份数0.39质量份)，利用手持混合机以1000rpm搅拌10分钟使其发泡，从而制作发泡体。
(发泡体的凝胶化)
将发泡体放入用纸制作的成型模具中，将成型模具移至热风干燥机中，在热风干燥机内对发泡体以80℃加热0.5小时，由此使发泡体凝胶化。将凝胶化后的发泡体在80℃加热12小时，使其干燥。
(发泡体的烧结)
将凝胶化并干燥后的发泡体以5℃/分钟的升温速度升温至预烧结温度(400℃)，在升温后进行10小时的预烧结。接着，从400℃以相同的升温速度升温至正式烧结温度(510℃)，在升温后进行3小时的正式烧结，之后以10℃/分钟的速度冷却至室温，得到碳酸钙多孔烧结体。
所得到的碳酸钙多孔烧结体的气孔率为82体积％。关于气孔率，将烧结体切成长方体块状，从块的重量和表观体积求得密度，除以碳酸钙的真密度2.711g/cm3，求得相对密度(％)，将从100％减去相对密度而得的值作为气孔率。
＜实施例2＞
除了将发泡剂的量从0.97质量份变更为0.04质量份以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结，得到碳酸钙多孔烧结体。所得碳酸钙多孔烧结体的气孔率为64体积％。
＜实施例3＞
除了作为胶凝剂使用异丁烯―马来酸酐共聚物的碱水溶性聚合物以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结，得到碳酸钙多孔烧结体。所得到的碳酸钙多孔烧结体的气孔率为78体积％。
＜比较例1＞
除了不使用胶凝剂以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结。然而，烧结时不能维持发泡体的形状，未能得到碳酸钙多孔烧结体。
＜碳酸钙多孔烧结体的扫描电子显微镜观察＞
图1～图4是实施例1中得到的碳酸钙多孔烧结体的扫描电子显微镜照片。图1为倍率25倍，图2为倍率150倍，图3为倍率5000倍，图4为倍率20000倍。从图1和图2可以明确看出，碳酸钙多孔烧结体具有连通至烧结体的外部的连通孔。另外，从图3和图4可以明确看出，碳酸钙颗粒被致密地烧结，形成了具有致密壁部的多孔烧结体。
＜实施例4＞
除了使用纯度为99.99质量％、平均粒径(D50)为0.15μm、BET比表面积为10m2/g的碳酸钙、且不向分散液中添加作为烧结助剂的碳酸钾和碳酸锂以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结，得到碳酸钙多孔烧结体。所得到的碳酸钙多孔烧结体的气孔率为84体积％。
＜实施例5＞
除了使用纯度为99.91质量％、平均粒径(D50)为0.15μm、BET比表面积为10m2/g的碳酸钙、且不向分散液中添加作为烧结助剂的碳酸钾和碳酸锂以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结，得到碳酸钙多孔烧结体。所得到的碳酸钙多孔烧结体的气孔率为81体积％。
＜参考例1＞
除了不向分散液中添加作为烧结助剂的碳酸钾和碳酸锂以外，与实施例1同样操作，制作发泡体，将制得的发泡体凝胶化后进行烧结，但未能得到碳酸钙多孔烧结体。
从实施例4和5与参考例1的比较可知，通过使用高纯度碳酸钙，能够在不使用烧结助剂的情况下，制造碳酸钙多孔烧结体。

Claims (10)

1.一种碳酸钙多孔烧结体的制造方法，其特征在于，包括：
制备含有碳酸钙和胶凝剂的分散液的工序；
向所述分散液添加发泡剂后进行搅拌而使其发泡，从而制作发泡体的工序；
使所述发泡体凝胶化的工序；和
通过将所述凝胶化的发泡体进行烧结来制造碳酸钙多孔烧结体的工序。
2.如权利要求1所述的碳酸钙多孔烧结体的制造方法，其特征在于：所述分散液含有烧结助剂。
3.如权利要求2所述的碳酸钙多孔烧结体的制造方法，其特征在于：所述烧结助剂含有锂、钠和钾中的至少2种的碳酸盐或氟化物，并且熔点为600℃以下。
4.如权利要求1～3中任一项所述的碳酸钙多孔烧结体的制造方法，其特征在于：
所述分散液含有20体积％以上的所述碳酸钙。
5.如权利要求1～4中任一项所述的碳酸钙多孔烧结体的制造方法，其特征在于：
所述烧结的工序为在进行预烧结后进行正式烧结的工序。
6.如权利要求6所述的碳酸钙多孔烧结体的制造方法，其特征在于：预烧结的温度在200～500℃的范围内，正式烧结的温度为预烧结的温度以上并且在420～600℃的范围内。
7.如权利要求1～6中任一项所述的碳酸钙多孔烧结体的制造方法，其特征在于：
所述碳酸钙的利用透射式电子显微镜观察测定的粒径分布中的平均粒径D50在0.05～0.30μm的范围内。
8.如权利要求1～7中任一项所述的碳酸钙多孔烧结体的制造方法，其特征在于：
所述碳酸钙的BET比表面积为5～25m2/g。
9.如权利要求1～8中任一项所述的碳酸钙多孔烧结体的制造方法，其特征在于：
所述碳酸钙的纯度为99.9质量％以上。
10.一种用于制造碳酸钙多孔烧结体的碳酸钙，其特征在于：
纯度为99.9质量％以上。
CN201880013713.8A 2017-02-27 2018-02-26 碳酸钙多孔烧结体的制造方法 Withdrawn CN110337426A (zh)

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JP2021037281A (ja) 2019-08-27 2021-03-11 邦夫 石川 医療用炭酸カルシウム組成物、および関連医療用組成物、ならびにこれらの製造方法
KR20210158676A (ko) 2020-06-24 2021-12-31 에스케이이노베이션 주식회사 젖산 생산능이 증가된 재조합 내산성 효모
JP2023023137A (ja) * 2021-08-04 2023-02-16 株式会社白石中央研究所 焼結体原料炭酸カルシウム、炭酸カルシウム多孔質焼結体、炭酸カルシウム緻密質焼結体ならびにそれらの製造方法

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