CN116639957A - 一种强耐碱的瓷球及其制备方法 - Google Patents
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- 239000003513 alkali Substances 0.000 title claims abstract description 31
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 16
- 230000032798 delamination Effects 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000004927 clay Substances 0.000 claims description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229920003257 polycarbosilane Polymers 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229960000892 attapulgite Drugs 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052625 palygorskite Inorganic materials 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims 3
- 238000005245 sintering Methods 0.000 abstract description 6
- 238000007493 shaping process Methods 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 3
- 229910018540 Si C Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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Abstract
本发明开发了一种强耐碱的瓷球及其制备方法，通过将SiO2材料层离，然后吸附聚碳硅烷，经混合混炼成型后，最后烧结，制得强耐碱性能的瓷球。
Description
技术领域
本发明涉及一种瓷球，具体为一种强耐碱的瓷球及其制备方法。
背景技术
瓷球主要应用在石油、化工、环保等行业，其作用是作为反应器中催化剂的覆盖支撑材料或塔式填料。因其在反应器中工作时，所处环境复杂，高温、高压、强酸、强碱等因素较多，所以需要根据反应特性和反应条件选择合适的瓷球。
现有技术中，由于瓷球主要成分为Al2O3，辅以一定量的SiO2材料烧结而成。其中SiO2材料的含量直接影响瓷球的耐碱性。为了提升瓷球的耐碱性，目前的主流工艺是大幅提升Al2O3用量，减少SiO2材料含量，同时提升烧结温度。
本发明开发了一种强耐碱的瓷球及其制备方法，通过将SiO2材料层离，然后吸附聚碳硅烷，经混合混炼成型后，最后烧结，制得强耐碱性能的瓷球。
发明内容
本发明开发了一种强耐碱的瓷球及其制备方法，通过将SiO2材料层离，然后吸附聚碳硅烷，经混合混炼成型后，最后烧结，制得强耐碱性能的瓷球。
一种强耐碱的瓷球的制备方法，所述制备方法具体如下：
(1)取一定量的SiO2材料，通过研磨粉碎至粒径为5μm-10μm，加入1-3倍质量的水，然后煮沸1h-2h，过滤并以乙醇清洗，得到层离SiO2材料；
(2)取一定量聚碳硅烷质量分数为1％-2％的二甲苯溶液，然后加入二甲苯溶液质量50％-80％的层离SiO2材料，混合均匀后减压蒸馏；然后与层离SiO2材料质量6-10倍的Al2O3粉末混合，加入适量水并混炼成型，得到烧制料；
(3)将烧制料入炉，通入保护气体，升温至1100℃-1200℃并保温1h-1.5h，然后继续升温至1300℃-1500℃烧制3h-4h，冷却出炉后即得强耐碱性能的瓷球。
进一步的，所述SiO2材料为粘土质硅藻土、高岭土、凹凸棒土中的一种或多种。
进一步的，第(1)步清洗用的乙醇为体积分数70％-90％的乙醇溶液。
进一步的，所述Al2O3粉末的粒径为1μm-5μm。
进一步的，第(3)步保护气体为N2或Ar。
进一步的，第(2)步混炼成型成型时，加入造孔剂。
进一步的，所述造孔剂为活性炭。
本发明的优点：本发明通过将SiO2材料层离，然后混合混炼成型，最后烧结，制得强耐碱性能的瓷球：其中，将SiO2材料层离可有效分散SiO2材料，使其被聚碳硅烷包覆，在烧结后，在表面形成Si-C保护层。
具体实施方式
实施例1
一种强耐碱的瓷球的制备方法，所述制备方法具体如下：
(1)取一定量的粘土质硅藻土，通过研磨粉碎至粒径为10μm，加入2倍质量的水，然后煮沸1h，过滤并以体积分数70％的乙醇溶液乙醇清洗，得到层离SiO2材料；
(2)取一定量聚碳硅烷质量分数为1％的二甲苯溶液，然后加入二甲苯溶液质量60％的层离SiO2材料，混合均匀后减压蒸馏；然后与层离SiO2材料质量9倍的粒径为5μm的Al2O3粉末混合，加入适量水并混炼成型，得到烧制料；
(3)将烧制料入炉，通入N2，升温至1100℃并保温1h，然后继续升温至1300℃烧制3h，冷却出炉后即得强耐碱性能的瓷球。
实施例2
第(3)步烧制工艺为升温至1300℃烧制4h，其余工艺均同实施例1。
对比例1
按照粒径为10μm的粘土质硅藻土粉:粒径为5μm的Al2O3粉末质量比为1:9的配比进行混炼成型，升温至1300℃烧制4h，制得莫来石质瓷球。
对比例2
粒径为10μm的粘土质硅藻土粉未经第(1)步层离，直接加入聚碳硅烷质量分数为1％的二甲苯溶液，其余工艺均同实施例1。
对比例3
按照粒径为10μm的粘土质硅藻土粉:粒径为5μm的Al2O3粉末质量比为1:99的配比进行混炼成型，升温至1850℃烧制4h，制得刚玉质瓷球。
对比测试：
上述实施例与对比例均烧制为φ20mm的瓷球，按照HG-T 3210-2002《耐酸陶瓷材料性能试验方法》第10项“耐碱度试验方法”进行测试，得出耐碱度RA(％)。
| 测试 | 实施例1 | 实施例2 | 对比例1 | 对比例2 | 对比例3 |
| 耐碱度RA(％) | 99.10 | 97.53 | 92.37 | 93.65 | 99.22 |
从上表可见，实施例1(90％Al2O3含量)的耐碱度接近于对比例3(99％Al2O3含量)，在扩大瓷球应用范围上效果显著，而且烧制温度大幅降低。
从对比例2可见，由于耐碱度试验方法要求将瓷球去除釉面并粉碎过筛，粘土质硅藻土粉在未经层离的情况下，其表面Si-C保护层不完整或被破坏，导致耐碱度提升不明显。
最后：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.一种强耐碱的瓷球的制备方法，其特征在于：所述制备方法具体如下：
(1)取一定量的SiO2材料，通过研磨粉碎至粒径为5μm-10μm，加入1-3倍质量的水，然后煮沸1h-2h，过滤并以乙醇清洗，得到层离SiO2材料；
(2)取一定量聚碳硅烷质量分数为1％-2％的二甲苯溶液，然后加入二甲苯溶液质量50％-80％的层离SiO2材料，混合均匀后减压蒸馏；然后与层离SiO2材料质量6-10倍的Al2O3粉末混合，加入适量水并混炼成型，得到烧制料；
(3)将烧制料入炉，通入保护气体，升温至1100℃-1200℃并保温1h-1.5h，然后继续升温至1300℃-1500℃烧制3h-4h，冷却出炉后即得强耐碱性能的瓷球。
2.根据权利要求1所述强耐碱的瓷球的制备方法，其特征在于：所述SiO2材料为粘土质硅藻土、高岭土、凹凸棒土中的一种或多种。
3.根据权利要求1所述强耐碱的瓷球的制备方法，其特征在于：第(1)步清洗用的乙醇为体积分数70％-90％的乙醇溶液。
4.根据权利要求1所述强耐碱的瓷球的制备方法，其特征在于：所述Al2O3粉末的粒径为1μm-5μm。
5.根据权利要求1所述强耐碱的瓷球的制备方法，其特征在于：第(3)步保护气体为N2或Ar。
6.根据权利要求1所述强耐碱的瓷球的制备方法，其特征在于：第(2)步混炼成型成型时，加入造孔剂。
7.根据权利要求6所述强耐碱的瓷球的制备方法，其特征在于：所述造孔剂为活性炭。
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| GB8613829D0 (en) * | 1985-06-06 | 1986-07-09 | Agency Ind Science Techn | Alumina silica sintered ceramics |
| WO2009030207A1 (de) * | 2007-09-08 | 2009-03-12 | Calsitherm Verwaltungs Gmbh | Alkaliresistente keramische erzeugnisse und schutzschichten und verfahren zu deren herstellung |
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| CN110218082A (zh) * | 2019-06-18 | 2019-09-10 | 陈彦霖 | 一种低温烧结mh型刚玉瓷球及其制备方法 |
| WO2022100282A1 (zh) * | 2020-11-12 | 2022-05-19 | 中广核研究院有限公司 | 连接钎料及其制备方法、碳化硅包壳连接方法 |
| CN115490503A (zh) * | 2022-10-25 | 2022-12-20 | 娄底市海天特种陶瓷有限公司 | 一种陶瓷复合材料及熔断器瓷管 |
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