CN106083175B8 - 一种复合陶瓷蓄热基体材料的制备方法 - Google Patents
一种复合陶瓷蓄热基体材料的制备方法 Download PDFInfo
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- CN106083175B8 CN106083175B8 CN201610484277.5A CN201610484277A CN106083175B8 CN 106083175 B8 CN106083175 B8 CN 106083175B8 CN 201610484277 A CN201610484277 A CN 201610484277A CN 106083175 B8 CN106083175 B8 CN 106083175B8
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明涉及一种复合陶瓷蓄热基体材料的制备方法，属于蓄热材料制备领域。该方法将多种矿土原料共混，经菜汁发酵，微生物改性后制坯，烧结后负载光合细菌，冻干即得蓄热基体材料。本发明通过多种矿土共混弥补单一陶瓷基材料抗热震性差的缺陷，经菜汁微生物对矿土表面改性和碳酸钙共同拓宽其孔径，增加矿土负载量，再通过添加纳米二氧化钛制坯烧结后，负载光合细菌通过阿拉伯胶包覆来提高基体材料的光能利用率，又解决了传统陶瓷基蓄热材料孔隙率低导致负载量少并且光能利用率低，使其蓄热供能效率偏低的问题，具有广阔的应用前景。
Description
一种复合陶瓷蓄热基体材料的制备方法
技术领域
[0001]本发明涉及一种复合陶瓷蓄热基体材料的制备方法，属于蓄热材料制备领域。
背景技术
[0002]当代社会的快速发展消耗了大量能源，然而伴随着化石燃料的枯竭，能源的缺乏 成为了制约人类生存和发展的一大瓶颈，开发和利用新能源迫在眉睫。太阳能、风能、氢能 作为重要的新能源，具有取之不尽、用之不竭的优点，而太阳能发电作为一种清洁无污染的 能源利用方式，已经引起了全世界科研工作者的广泛关注。
[0003]太阳能发电的方式主要包括两种，即太阳能热发电和太阳能光伏发电。太阳能的 间歇性和不稳定性限制了光伏发电的应用，太阳能热发电系统针对太阳能间歇性和不稳定 性的特点专门设计了蓄热子系统，可以在光照正常时将热量储存起来，在夜间或光照不足 时保证热量供给，通过热、功、电转换系统，继续带动汽轮机正常发电，保证电站连续、稳定 工作。在太阳能热发电中使用高效的蓄热材料，可以提高太阳能的利用率，降低使用成本， 对于太阳能热发电技术具有重要意义。
[0004]蓄热材料需具备以下要求:耐高温。蓄热式热交换器的优点之一，在于能够克服常 规金属换热器不能高温下长期工作的弱点。要求蓄热介质的蓄热材料须耐高温。良好的导 热性。要求作为蓄热载体的材料必须具有良好的导热性能。导热性能越好，其体积利用率越 高，蓄热设备的体积及用材可以减少到最少，而且基体材料的抗热震性能越好。越有利于设 备的微型化，对设备的布置安装越有利。闻的抗热震性。作为蓄热载体，始终处于加热和冷 却交替循环的工作状态。由于长期处于急冷急热的工作环境，经常承受着因内外温差变化 而引起的应力作用，易引起材料破裂甚至粉碎，造成热交换器气流通道阻塞，因此对材料的 抗热震稳定性提出了较高的要求。
[0005]目前常见的陶瓷基蓄热载体材料由于成份单一，其抗热震性能差，孔隙率低导致 负载量少并且光能利用率低，使其蓄热供能效率偏低，因此研究发明一种高效蓄热供能的 蓄热载体材料具有极佳的前景。
发明内容
[0006]本发明主要解决的技术问题:针对目前常见的陶瓷基蓄热载体材料由于成份单 一，其抗热震性能差，孔隙率低导致负载量少并且光能利用率低，使其蓄热供能效率偏低的 缺陷，提供了一种复合陶瓷蓄热基体材料的制备方法，该方法将多种矿土原料共混，经菜汁 发酵，微生物改性后制坯，烧结后负载光合细菌，冻千即得蓄热基体材料。本发明通过多种 矿土共混弥补单一陶瓷基材料抗热震性差的缺陷，经菜汁微生物对矿土表面改性和碳酸钙 共同拓宽其孔径，增加矿土负载量，再通过添加纳米二氧化钛制坯烧结后，负载光合细菌通 过阿拉伯胶包覆来提高基体材料的光能利用率，解决了传统陶瓷基蓄热材料孔隙率低导致 负载量少并且光能利用率低，使其蓄热供能效率偏低的问题，具有广阔的应用前景。
[0007]为了解决上述技术问题，本发明所采用的技术方案是：
[0008] (1)称取1?〇〜l8〇g高岭土、2〇0〜300g钾长石、25〇〜3〇〇g水滑石、150〜2〇〇g赤泥 和30〜40g石英石混合均匀后放入刚玉研钵中研磨1〜2h后再移入球磨机中，向球磨罐中加 入混合物料总体积15〜20倍的氧化错球磨珠，机械球磨过夜，将球磨后的产物过25〇目标准 筛，得到混合粉末；
[0009] (2)再称取50〜60g莫来石、70〜90g沙漠砂和20〜40g堇青石一起放入气流粉碎机 粉碎后过100目不锈钢筛，将过筛后的产物和上述得到的混合粉末一起装入陶瓷发酵罐中 作为改性底物，再向罐中加入底物等质量的废弃菜汁，用搅拌棒搅拌均匀后将发酵罐放置 在30〜40°C的温室中保温发酵7〜9天；
[0010] (3)待发酵完成后，取出发酵物并加入其质量3〜5%的纳米二氧化钛粉末和10〜 15%碳酸钓，用混料机混合搅拌15〜20min后注入直径为5〜8cm，厚2〜3cm，孔径为3〜5mm的 圆形蜂窝状模具中，用液压机以3〜5MPa的压力保压压制10〜20min;
[0011] (4)压制结束后移入高温烧结炉中，先以5°C/min速率升温至500〜60(TC保温30〜 40min后再以10°C/min速率升温至1〇〇〇〜1060°C继续烧结1〜3h后待其冷却至室温，拆模得 蓄热基体粗品，备用；
[0012] (5)称取10〜15g蛋白胨、3〜5g牛肉膏、5〜7g氯化钠、3〜6g麦芽浸膏倒入1000〜 1200mL去离子水中混合均匀后的液体培养基，按接种量为1〇%将菌种号为NS〇8沼泽红假单 胞菌接入上述液体培养基中，用浓度为0 • 5mol/L氢氧化钠溶液调节pH至7 • 0〜8 • 0，在30〜 37°C恒温箱中保温培养2〜妖，用超声分散仪以200〜3〇OW功率超声分散15〜25min后得到 菌悬液；
[0013] (6)按固液比为1:5将备用的蓄热基体粗品浸入上述菌悬液中，再依次加入蓄热基 体粗品等质量的阿拉伯胶和其质量1/3的明胶，放置在摇床上振荡混合1〜2h后过滤分离得 到滤渣，用真空冻干机在-30〜-25°C下冻干，即得复合陶瓷蓄热基体材料。
[0014]本发明的物理性质:本发明制得的复合陶瓷蓄热基体材料孔隙率为25.〇〜3〇.〇%， 吸水率为10.2〜11 • 〇%，体积密度为2. l〇g/cm3，抗折强度为77〜80MPa，热震性能在400〜 800°C下热震30次不开裂，热震30次后的强度仍可达58〜60MPa。
[0015] 本发明的有益效果是：
[0016] (1)本发明制得的复合陶瓷蓄热基体材料原料易得，制备过程简单易操作，制备成 本低廉；
[0017] (2)本发明制得的复合陶瓷蓄热基体材料抗热震性能优异，在4〇〇〜8〇〇°c下执震 30次不开裂； ^
[0018] (3)本发明制得的复合陶瓷蓄热基体材料孔隙率高，负载量大，具有极佳的使用效 果。
具体实施方式
[0019] j尔取l7〇〜180g高岭土、2〇0〜3〇收钾长石、250〜3〇收水滑石、15〇〜2〇〇g赤泥和3〇 〜40g石央石混合均匀后放入刚玉研钵中研磨丨〜此后再移入球磨机中，向球磨罐中加入混 合物料总体积15〜20倍的氧化锆球磨珠，机械球磨过夜，将球磨后的产物过25〇目标准筛， 得，混合粉末;再称取50〜60g莫来石、70〜90g沙漠砂和20〜40g堇青石一起放入气流粉碎 机粉碎后过100目不锈钢筛，将过筛后的产物和上述得到的混合粉末一起装入陶瓷发酵罐 中作为改性底物，再向罐中加入底物等质量的废弃菜汁，用搅拌棒搅拌均匀后将发酵罐放 置在30〜40°C的温室中保温发酵7〜9天;待发酵完成后，取出发酵物并加入其质量3〜5%的 纳米二氧化钛粉末和10〜15%碳酸钙，用混料机混合搅拌15〜20min后注入直径为5〜8cm， 厚2〜3cm，孔径为3〜5mm的圆形蜂窝状模具中，用液压机以3〜5MPa的压力保压压制10〜 20min;压制结束后移入高温烧结炉中，先以5°C/min速率升温至500〜600°C保温30〜40min 后再以l〇°C/min速率升温至1000〜1060°C继续烧结1〜3h后待其冷却至室温，拆模得蓄热 基体粗品，备用;称取10〜15g蛋白胨、3〜5g牛肉膏、5〜7g氯化钠、3〜6g麦芽浸膏倒入1000 〜l2〇OmL去离子水中混合均匀后的液体培养基，按接种量为10%将菌种号为Ns〇8沼泽红假 单胞菌接入上述液体培养基中，用浓度为0 • 5mol/L氢氧化钠溶液调节pH至7.0〜8.0，在30 〜37°C恒温箱中保温培养2〜3天，用超声分散仪以200〜300W功率超声分散15〜25min后得 到菌悬液;按固液比为I:5将备用的蓄热基体粗品浸入上述菌悬液中，再依次加入蓄热基体 粗品等质量的阿拉伯胶和其质量1 /3的明胶，放置在摇床上振荡混合1〜2h后过滤分离得到 滤渣，用真空冻干机在_3〇〜-25°C下冻干，即得复合陶瓷蓄热基体材料。
[0020]实例 1
[0021] 称取170g高岭土、200g钾长石、250g水滑石、150g赤泥和30g石英石混合均匀后放 入刚玉研钵中研磨lh后再移入球磨机中，向球磨罐中加入混合物料总体积15倍的氧化锆球 磨珠，机械球磨过夜，将球磨后的产物过250目标准筛，得到混合粉末;再称取50g莫来石、 70g沙漠砂和20g堇青石一起放入气流粉碎机粉碎后过1〇〇目不锈钢筛，将过筛后的产物和 上述得到的混合粉末一起装入陶瓷发酵罐中作为改性底物，再向罐中加入底物等质量的废 弃菜汁，用搅拌棒搅拌均匀后将发酵罐放置在3(TC的温室中保温发酵7天;待发酵完成后， 取出发酵物并加入其质量3%的纳米二氧化钛粉末和1〇%碳酸钙，用混料机混合搅拌15min后 注入直径为5cm，厚2cm，孔径为3mm的圆形蜂窝状模具中，用液压机以3MPa的压力保压压制 lOmin;压制结束后移入高温烧结炉中，先以5°c/min速率升温至50(TC保温30min后再以10 °C/min速率升温至l^KKTC继续烧结lh后待其冷却至室温，拆模得蓄热基体粗品，备用;称取 l〇g蛋白胨、3g牛肉膏、5g氯化钠、3g麦芽浸膏倒入lOOOmL去离子水中混合均匀后的液体培 养基，按接种量为10%将菌种号为NS08沼泽红假单胞菌接入上述液体培养基中，用浓度为 0 • 5mol/L氢氧化钠溶液调节PH至7. 〇，在3〇。(：恒温箱中保温培养2天，用超声分散仪以200W 功率超声分散15min后得到菌悬液;按固液比为丨：5将备用的蓄热基体粗品浸入上述菌悬液 中，再依次加;^蓄热基体粗品等质量的阿拉伯胶和其质量丨/3的明胶，放置在摇床上振荡混 合lh后过滤分离得到滤渣，用真空冻干机在_3(rc下冻干，即得复合陶瓷蓄热基体材料。 [0022]本发明的物理性质:本发明制得的复合陶瓷蓄热基体材料孔隙率为25 •0%，吸水率 为10_2%，体积密度为2.l〇g/cm3,抗折强度为77MPa，热震性能在4〇(rc下热震30次不开裂， 热震30次后的强度仍可达58MPa。
[0023]实例 2
[0024]称取175g高岭土、250g钾长石、280g水滑石、180g赤泥和35g石英石混合均匀后放 入刚玉研钵中研磨2h后再移入球磨机中，向球磨罐中加入混合物料总体积18倍的氧化锆球 磨珠，机械球磨过夜，将球磨后的产物过25〇目标准筛，得到混合粉末;再称取55g莫来石、 8〇g沙漠砂和30g堇青石一起放入气流粉碎机粉碎后过丨⑻目不锈钢筛，将过筛后的产物和 上述得到的混合粉末一起装入陶瓷发酵罐中作为改性底物，再向罐中加入底物等质量的废 弃菜汁，用搅拌棒搅拌均匀后将发酵罐放置在35 °C的温室中保温发酵8天;待发酵完成后， 取出发酵物并加入其质量4%的纳米二氧化钛粉末和13%碳酸钙，用混料机混合搅拌18min后 注入直径为7cm，厚2cm，孔径为4mm的圆形蜂窝状模具中，用液压机以4MPa的压力保压压制 15min;压制结束后移入高温烧结炉中，先以5°C/min速率升温至550°C保温35min后再以10 tVmiri速率升温至1030°C继续烧结2h后待其冷却至室温，拆模得蓄热基体粗品，备用;称取 13g蛋白胨、4g牛肉膏、6g氯化钠、4g麦芽浸膏倒入llOOmL去离子水中混合均匀后的液体培 养基，按接种量为10%将菌种号为NS08沼泽红假单胞菌接入上述液体培养基中，用浓度为 0 • 5mol/L氢氧化钠溶液调节PH至7.5，在34°C恒温箱中保温培养2天，用超声分散仪以250W 功率超声分散20min后得到菌悬液;按固液比为1:5将备用的蓄热基体粗品浸入上述菌悬液 中，再依次加入蓄热基体粗品等质量的阿拉伯胶和其质量1/3的明胶，放置在摇床上振荡混 合2h后过滤分离得到滤渣，用真空冻干机在-28。(：下冻干，即得复合陶瓷蓄热基体材料。 [0025]本发明的物理性质:本发明制得的复合陶瓷蓄热基体材料孔隙率为28.0%，吸水率 为10 •5%，体积密度为2 • lOg/cm3，抗折强度为79MPa，热震性能在60(TC下热震30次不开裂， 热震30次后的强度仍可达59MPa。
[0026] 实例3
[0027] 称取18〇g高岭土、300g钾长石、300〖水滑石、200g赤泥和40g石英石混合均匀后放 入刚玉研钵中研磨2h后再移入球磨机中，向球磨罐中加入混合物料总体积20倍的氧化锆球 磨珠，机械球磨过夜，将球磨后的产物过250目标准筛，得到混合粉末;再称取60g莫来石、 9〇g沙漠砂和40g堇青石一起放入气流粉碎机粉碎后过丨⑻目不锈钢筛，将过筛后的产物和 上述得到的混合粉末一起装入陶瓷发酵罐中作为改性底物，再向罐中加入底物等质量的废 弃菜汁，用搅拌棒搅拌均匀后将发酵罐放置在4(TC的温室中保温发酵9天;待发酵完成后， 取出发酵物并加入其质量5%的纳米二氧化钛粉末和15%碳酸钙，用混料机混合搅拌20min后 注入直径为Scm，厚3cm，孔径为5mtn的圆形蜂窝状模具中，用液压机以5MPa的压力保压压制 20min;压制结束后移入高温烧结炉中，先以5tVmin速率升温至60(rc保温4〇min后再以1〇 °C /min速率升温至1^60°C继续烧结3h后待其冷却至室温，拆模得蓄热基体粗品，备用;称取 15g蛋白胨、5g牛肉膏、7g氯化钠、6g麦芽浸膏倒入1200mL去离子水中混合均匀后的液体培 养基，按接种量为10%将菌种号为NS〇8沼泽红假单胞菌接入上述液体培养基中，用浓度为 0 • 5mol/L氢氧化钠溶液调节PH至8. 〇，在30〜37°C恒温箱中保温培养3天，用超声分散仪以 300W功率超声分散25min后得到菌悬液;按固液比为1:5将备用的蓄热基体粗品浸入上述菌 悬液中，再依次加入^热基体粗品等质量的阿拉伯胶和其质量丨/3的明胶，放置在摇床上振 荡混合2h后过滤分离得到滤渣，用真空冻干机在_25〇C下冻干，即得复合陶瓷蓄热基体材 料。
[0028] 本发明的物理性质:本发明制得的复合陶瓷蓄热基体材料孔隙率为30.0%，吸水率 为11 • 0%，体积密度为2 • l〇g/cm3，抗折强度为8〇MPa，热震性能在8〇〇 °C下热震30次不开裂， 热震30次后的强度仍可达60MPa。
Claims (1)
1. 一种复合陶瓷蓄热基体材料的制备方法，其特征在于具体制备步骤为： (1) 称取170〜18〇g高岭土、200〜300g钾长石、250〜300g水滑石、150〜200g赤泥和30 〜40g石英石混合均匀后放入刚玉研钵中研磨1〜2h后再移入球磨机中，向球磨罐中加入混 合物料总体积15〜20倍的氧化错球磨珠，机械球磨过夜，将球磨后的产物过25〇目标准筛， 得到混合粉末； (2) 再称取50〜60g莫来石、70〜90g沙漠砂和20〜40g堇青石一起放入气流粉碎机粉碎 后过100目不锈钢筛，将过筛后的产物和上述得到的混合粉末一起装入陶瓷发酵罐中作为 改性底物，再向罐中加入底物等质量的废弃菜汁，用搅拌棒搅拌均匀后将发酵罐放置在3〇 〜40°C的温室中保温发酵7〜9天； (3) 待发酵完成后，取出发酵物并加入其质量3〜5%的纳米二氧化钛粉末和10〜15%碳 酸1¾，用混料机混合搅拌15〜20min后注入直径为5〜8cm，厚2〜3cm，孔径为3〜5mm的圆形 蜂窝状模具中，用液压机以3〜5MPa的压力保压压制10〜20min; (4) 压制结束后移入高温烧结炉中，先以5°C/min速率升温至5〇〇〜6〇〇°C保温30〜 40min后再以lOtVmin速率升温至1000〜106(TC继续烧结1〜3h，待其冷却至室温，拆模得 蓄热基体粗品，备用； (5) 称取10〜15g蛋白胨、3〜5g牛肉膏、5〜7g氯化钠、3〜6g麦芽浸膏倒入1〇〇〇〜 1200mL去离子水中混合均匀后得液体培养基，按接种量为10%将菌种号为NS08沼泽红假单 胞菌接入上述液体培养基中，用浓度为〇. 5mol/L氢氧化钠溶液调节ph至7.0〜8.0，在30〜 37°C恒温箱中保温培养2〜3天，用超声分散仪以200〜3〇OW功率超声分散15〜25min后得到 菌悬液； (6) 按固液比为1: 5将备用的蓄热基体粗品浸入上述菌悬液中，再依次加入蓄热基体粗 品等质量的阿拉伯胶和其质量1/3的明胶，放置在摇床上振荡混合1〜2h后过滤分离得到滤 渣，用真空冻干机在-30〜-25°C下冻干，即得复合陶瓷蓄热基体材料。
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