CN115353134B - 一种高纯大晶粒勃姆石的制备方法 - Google Patents
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 37
- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000007524 organic acids Chemical class 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 6
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 claims description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- AWQSAIIDOMEEOD-UHFFFAOYSA-N 5,5-Dimethyl-4-(3-oxobutyl)dihydro-2(3H)-furanone Chemical compound CC(=O)CCC1CC(=O)OC1(C)C AWQSAIIDOMEEOD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229960002446 octanoic acid Drugs 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 12
- 230000001276 controlling effect Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 9
- 238000004806 packaging method and process Methods 0.000 description 6
- 238000005507 spraying Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000005643 Pelargonic acid Substances 0.000 description 1
- 241000212749 Zesius chrysomallus Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910006636 γ-AlOOH Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
- C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
本发明公开一种高纯大晶粒勃姆石的制备方法,包括以下步骤:1)将Al2O3含量为61‑65%的氢氧化铝粉加入磨机内进行研磨,得到颗粒粒径为2‑10um的氢氧化铝粉;2)将研磨后的氢氧化铝粉加入耙式干燥机中,搅拌并加入氢氧化铝粉重量的0.1‑1.0%的有机酸分散剂,并通入蒸汽,蒸汽压力为90Kpa‑1Mpa,加热至250‑300℃的温度,控制系统压力在0.8‑1.2Mpa进行高温反应,经2‑6小时反应后将反应产物放出,去离子水洗涤后烘干,得到高纯大晶粒勃姆石;本发明制得勃姆石晶体尺寸与纯度高,成本低,工艺简单。
Description
技术领域
本发明涉及材料制备技术领域,具体讲是一种高纯大晶粒勃姆石的制备方法。
背景技术
勃姆石又称一水铝石或薄水铝石,是铝土矿的主要成分,纯净的勃姆石为白色晶体,由于天然产物中含有杂质,通常带有黄色、绿色、棕色或红色斑点,并呈现玻璃或珍珠光泽。勃姆石的分子式为γ-AlOOH,属于正交晶系,具有类似于石墨烯的层状结构。勃姆石的孔隙率大、比表面积大,分散及胶溶性好,耐热度好且硬度低。
勃姆石作为添加剂也可用于涂料、陶瓷、纺织、造纸等行业中,并可作为电池隔膜涂层、催化剂载体、阻燃剂,提高橡胶、塑料的耐高温性和阻燃性。
国内制备高纯勃姆石多以高纯铝粉,异丙醇铝及铝盐等作为原料,加入有机酸碱作为助剂,在高压釜中水热反应制得,如专利号CN201710367476.2介绍了一种以纯水和高纯铝粉按一定比例混合,形成分散液;将有机碱缓慢加入到上述分散液中,在130-250℃条件下,水热处理3-12h,然后经过滤、干燥既得到勃姆石。也有部分从工业氧化铝或氢氧化铝出发制备纳米级的勃姆石,如专利号CN201810073336.9以普通工业氧化铝粉体(γ-氧化铝)为原料来制备纳米勃姆石粉的生产工艺,其将工业氧化铝粉(D=10μm左右)与水按一定比例混合搅拌均匀后转移到反应釜中,调节反应釜内压力,保压1h后在保压的压力下将浆料直接放出,冷却到室温后进行抽滤,水洗,烘干,得到粒度小于100nm的勃姆石纳米粉。专利号CN201710534602.9介绍了将氢氧化铝粉体置于水中,调节体系的pH值为6-10,于不低于170℃的温度下水热反应7h~10h,冷却并固液分离,所得固相经洗涤、干燥获得勃姆石纳米晶。
现有技术生产勃姆石的方法,所制备的勃姆石晶体尺寸不高,纯度低,成本较高,工艺较复杂。
发明内容
本发明旨在至少部分地克服现有技术中存在的上述和/或其他潜在的问题:提供一种制得勃姆石晶体尺寸与纯度高,成本低,工艺简单的高纯大晶粒勃姆石的制备方法。
本发明的技术解决方案如下:一种高纯大晶粒勃姆石的制备方法,包括以下步骤:
1)将Al2O3含量为61-65%的氢氧化铝粉加入磨机内进行研磨,得到颗粒粒径为2-10um的氢氧化铝粉;
2)将研磨后的氢氧化铝粉加入耙式干燥机中,搅拌并加入氢氧化铝粉重量的0.1-1.0%的有机酸分散剂,并通入蒸汽,蒸汽压力为90Kpa-1Mpa,加热至250-300℃的温度,控制系统压力在0.8-1.2Mpa进行高温反应,经2-6小时反应后将反应产物放出,去离子水洗涤后烘干,得到高纯大晶粒勃姆石。
作为优化,步骤1)中,磨机的入口温度150-200℃,进料压力0.2-0.3Mpa,研磨压力在0.6-1.0Mpa。
作为优化,步骤1)中,磨机的入口温度200℃,进料压力0.2Mpa,研磨压力在1.0Mpa。
作为优化,步骤2)中,将研磨后的氢氧化铝粉加入耙式干燥机中,搅拌并加入氢氧化铝粉重量的1.0%的有机酸分散剂,并通入压力为1Mpa蒸汽,加热至300℃的温度下,控制压力在1.2Mpa的条件下进行高温反应,经6小时高温反应后放出。
作为优化,所述有机酸分散剂为C1-C9有机酸分散剂。
作为优化,所述有机酸分散剂为甲酸、醋酸、丙酸、正丁酸、异丁酸、正戊酸、异戊酸、己酸、庚酸、辛酸与壬酸中的一种或多种。
本发明的有益效果是:本发明提供一种新的高纯大晶粒勃姆石的制造方法, 适合于工业化生产的一步法制高纯大晶粒勃姆石产品。工艺简单,易实现工业化生产,摒弃液相法合成,采取氢铝直接加热,并通入蒸汽,实现勃姆石的转相及合成,加入C1-C9有机酸分散剂,抑制杂相生成,避免粒径变粗,对设备投入要求较低,减少了洗涤用水,节约了成本,有利于节能环保;制备的晶体尺寸高达80nm,纯度高达99.9%。
附图说明
图1为本发明的工艺流程示意图。
图2为实施例3制备的产品XRD图。
具体实施方式
下面用具体实施例对本发明做进一步详细说明,但本发明不仅局限于以下具体实施例。
实施例1
如图1工艺流程图所示,将Al2O3含量为61%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度200℃,进料压力0.2Mpa,研磨压力1.0Mpa,得到颗粒尺寸为4um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,搅拌过程中喷入10克正丁酸,并通入压力为90Kpa蒸汽,加热至250℃的温度下,控制压力在0.8Mpa的条件下进行高温反应,经2小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在40nm,纯度99.5%的勃姆石产品,收集包装。
实施例2
如图1工艺流程图所示,将Al2O3含量为61%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度150℃,进料压力0.2Mpa,研磨压力0.6Mpa,得到颗粒尺寸为10um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,搅拌过程中喷入100克异丁酸,并通入压力为1Mpa蒸汽,加热至280℃的温度下,控制压力在1Mpa的条件下进行高温反应,经6小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在61nm,纯度99.7%的勃姆石产品,收集包装。
实施例3
如图1工艺流程图所示,将Al2O3含量为64%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度200℃,进料压力0.2Mpa,研磨压力1.0Mpa,得到颗粒尺寸为2um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,搅拌过程中喷入100克正戊酸,并通入压力为1Mpa蒸汽,加热至300℃的温度下,控制压力在1.2Mpa的条件下进行高温反应,经6小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在80nm,纯度99.9%的勃姆石产品,收集包装;产品XRD图见附图2。
实施例4
如图1工艺流程图所示,将Al2O3含量为64%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度200℃,进料压力0.3Mpa,研磨压力1.0Mpa,得到颗粒尺寸为7um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,搅拌过程中喷入20克有正戊酸,并通入压力为0.2Mpa蒸汽,加热至250℃的温度下,控制压力在1.2Mpa的条件下进行高温反应,经6小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在47nm,纯度99.5%的勃姆石产品,收集包装。
实施例5
如图1工艺流程图所示,将Al2O3含量为64%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度200℃,进料压力0.3Mpa,研磨压力1.0Mpa,得到颗粒尺寸为5um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,搅拌过程中喷入50克壬酸,并通入压力为0.2Mpa蒸汽,加热至290℃的温度下,控制压力在1Mpa的条件下进行高温反应,经6小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在76nm,纯度99.8%的勃姆石产品,收集包装。
对比例1
将Al2O3含量为64%的氢氧化铝粉加入磨机内进行研磨,控制磨机入口温度200℃,进料压力0.2Mpa,研磨压力1.0Mpa,得到颗粒尺寸为2um的氢氧化铝粉;
将10千克研磨后的氢氧化铝粉加入耙式干燥机中,并通入压力为1Mpa蒸汽,加热至300℃的温度下,控制压力在1.2Mpa的条件下进行高温反应,经6小时高温反应后放出,去离子水洗涤,烘干,得到晶体尺寸在80nm,纯度99.0%的勃姆石产品,收集包装。
以上仅是本发明的特征实施范例,对本发明保护范围不构成任何限制。凡采用同等交换或者等效替换而形成的技术方案,均落在本发明权利保护范围之内。
Claims (4)
1.一种高纯大晶粒勃姆石的制备方法,其特征在于,包括以下步骤:
1)将Al2O3含量为61-65%的氢氧化铝粉加入磨机内进行研磨,得到颗粒粒径为2-10um的氢氧化铝粉;
2)将研磨后的氢氧化铝粉加入耙式干燥机中,搅拌并加入氢氧化铝粉重量的0.1-1.0%的有机酸分散剂,并通入蒸汽,蒸汽压力为90Kpa-1Mpa,加热至250-300℃的温度,控制系统压力在0.8-1.2Mpa进行高温反应,经2-6小时反应后将反应产物放出,去离子水洗涤后烘干,得到高纯大晶粒勃姆石;
步骤1)中,磨机的入口温度150-200℃,进料压力0.2-0.3Mpa,研磨压力在0.6-1.0Mpa;
所述有机酸分散剂为C1-C9有机酸分散剂。
2.根据权利要求1所述的高纯大晶粒勃姆石的制备方法,其特征在于,步骤1)中,磨机的入口温度200℃,进料压力0.2Mpa,研磨压力在1.0Mpa。
3.根据权利要求1所述的高纯大晶粒勃姆石的制备方法,其特征在于,步骤2)中,将研磨后的氢氧化铝粉加入耙式干燥机中,搅拌并加入氢氧化铝粉重量的1.0%的有机酸分散剂,并通入压力为1Mpa蒸汽,加热至300℃的温度下,控制压力在1.2Mpa的条件下进行高温反应,经6小时高温反应后放出。
4.根据权利要求1所述的高纯大晶粒勃姆石的制备方法,其特征在于,所述有机酸分散剂为甲酸、醋酸、丙酸、正丁酸、异丁酸、正戊酸、异戊酸、己酸、庚酸、辛酸与壬酸中的一种或多种。
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