CN116462204A - 一种改性超细二氧化硅粉体及其制备方法 - Google Patents
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000077 silane Inorganic materials 0.000 claims abstract description 5
- 241001062472 Stokellia anisodon Species 0.000 claims abstract description 3
- 239000003607 modifier Substances 0.000 claims abstract description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 23
- 238000003723 Smelting Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 229910052845 zircon Inorganic materials 0.000 claims description 6
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical group [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical class Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 125000001309 chloro group Chemical class Cl* 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000009438 liyan Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
本发明属于无机新材料领域,具体涉及一种改性超细二氧化硅粉体及其制备方法。本发明是将硅酸盐在2700℃的高温下熔炼后获得气相二氧化硅,通过在烟道中喷洒硅烷改性剂对其进行改性,得到形貌完整的球型二氧化硅粉体,平均粒径在1.4~1.9μm,比表面积为:20~28m2/g。
Description
技术领域
本发明属于无机新材料领域,具体涉及一种通过碳热还原法合成球型改性超细二氧化硅粉体及方法。
背景技术
传统的方式中对产生的硅粉进行处理的方式通常是通过将烟尘冷却后进再进行分筛之后,这个过程中不可避免的会被空气中的其他物质污染,冷却后的产物粉体粒径较大、易出现团聚,出现结块现象,降低了产品的分散度,不利于副产物的深加工利用。因此,通过一种通过高温碳还原锆英砂制备的超细改性球型二氧化硅粉体及方法能有效的避免这些问题。一种无需经过粉碎加工廉价的球型二氧化硅粉体的细度:平均粒径在1.4~1.9μm,比表面积为:20~28m/g,其细度和比表面积约为水泥的80~100倍,粉煤灰的50~70倍。
CN201911408909.X一种金属锆母体原料用电熔氧化锆的制备方法与CN201910835023.7一种处理锆英砂沸腾氯化产物四氯化硅的方法中均提到通过使用电容法和锆英砂作为制备原料进行超细球型二氧化硅,但其中所用到的还原剂为氟化镁在熔炼过程中会产生有害气体有一定的危险,但本发明中所用的还原剂为石油焦能够有效避免有害气体的产生。CN202011571832.0一种矿热炉烟气制备微硅粉的方法是通过热矿机烧结原料产生烟气,再将烟气冷却收集的过程。这个过程中所产生的烟气未经改性处理,该专利并未说明产品的粒度及形貌。CN102730701A一种用电熔氧化锆尾气制备高纯气相二氧化硅的方法是通过采用夹套水冷管进行冷却硅粉,这过程中硅粉进行极冷工艺对球型硅的成型有极大的影响。
黄建辉, 林文婷, 谢丽燕. 球型多孔二氧化硅吸附剂的制备和性能[J]. 材料研究学报, 2017, 31(4):5.在异丙醇水溶液中进行正硅酸乙酯水解-缩聚反应得到二氧化硅纳米球,然后在聚乙烯吡咯烷酮保护下将其用氢氧化钠溶液刻蚀,得到球型多孔二氧化硅与本发明的电熔法相比工艺更加复杂。
发明内容
本发明需要解决的是技术问题是一种通过高温熔炼所产的超细二氧化硅粉体的制备改性方法。
本发明技术如下:
一种通过高温熔炼产生的超细改性球形二氧化硅粉体的制备工艺,包括如下步骤:
(1)将500公斤的锆英砂(ZrSiO4)投入到2750℃的高温熔炼设备中进行10 h的熔炼。
(2)熔炼得到的含少量锆杂质的气态二氧化硅经烟道进入拉瓦尔管,在拉瓦尔管的作用下使气态二氧化硅富集,同时获得能量以便于高速经过改性仓防止其过早凝华,改性仓外接气态硅烷,当气态二氧化硅经过改性仓时,利用通入的硅烷气体对其进行包覆改性,增加成球率。改性后的气体进入分离系统分离。。
(3)整个分离系统的动能由结构末端的风机提供动力,由于二者的质量差异性经过由多管陶瓷构成的分离装置后,改性的二氧化硅被变频式风机抽入到储存室内,锆杂质沉淀在多管陶瓷下方的仓储漏斗中。
本发明的有益效果如下:
1)本发明所用的无机硅酸盐为锆英砂(ZrSiO4),主要用途是生产电熔氧化锆而超细改性球型二氧化硅是生产电熔氧化锆的副产物。
2)本发明所用的二氧化硅粉体回收是通过设备一体化完成的,有效避免粉体的外泄。
3)本发明所用的改性剂为硅烷,能够优化二氧化硅颗粒的球型形貌,增加分散度。
4)本发明所使用拉瓦尔管,包括收缩管和扩张管,能够收集气体再通过改变截面面积使其不断加速,从而高速通过改性仓,避免其过早凝华成固体。
5)本发明所用的中获得的超细改性球形二氧化硅不需要进行研磨能够直接获得粒度为1.0μm-1.8μm。
6)本发明获得到改性后的斜方系球型二氧化硅粉体形貌好、纯度高,适用于在氯盐污染侵蚀、硫酸盐侵蚀、高湿度等恶劣环境下。
附图说明:
图1是例1样品的扫描电镜图谱(SEM)。
图2是实施例1样品的XRD图谱。
Claims (5)
1.一种通过高温熔炼产生的超细改性球型二氧化硅粉体的制备方法,包括如下步骤:将一种硅酸盐投入到2700℃左右的高温熔炼设备中,采用碳热还原法熔炼10-20 h,然后通过烟道内的拉瓦尔管改性装置对熔炼产生的含少量锆杂质的气态超细二氧化硅进行改性,改性后的粉体再由分离设备分离,获得超细球型二氧化硅粉体。
2.根据权利要求1所述的一种通过高温熔炼产生的超细改性球形二氧化硅粉体的制备方法,其特征在于:所述的硅酸盐为锆英砂(ZrSiO4)。
3.根据权利要求1所述的一种通过高温熔炼产生的超细改性球形二氧化硅粉体的制备方法,其特征在于:高温熔炼设备为等离子熔分炉,分离装置设备是由多根多管陶瓷组成,整个装置的动能由装置末端的风机提供,变频控制在28-42Hz,。
4.根据权利要求1所述的一种通过高温熔炼产生的超细改性球形二氧化硅粉体的制备方法,其特征在于:改性装置由烟道内特殊的拉瓦尔管和球化改性仓组成。
5.根据权利要求1所述的一种通过高温熔炼产生的超细改性球形二氧化硅粉体的制备方法,其特征在于:所述的改性剂为汽态硅烷。
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4118464A (en) * | 1977-02-07 | 1978-10-03 | University Of Utah | Process for separating silica from silicate-bearing materials |
JPH0259416A (ja) * | 1988-08-25 | 1990-02-28 | Nippon Chem Ind Co Ltd | 微細溶融球状シリカおよびその製造法 |
JPH02199013A (ja) * | 1989-01-26 | 1990-08-07 | Nippon Chem Ind Co Ltd | 微細な溶融球状シリカの製造方法 |
JPH0733427A (ja) * | 1993-07-23 | 1995-02-03 | Nissan Gaadoraa Shokubai Kk | 細孔構造を制御した球状シリカ微粉体の製造方法 |
JP2008249220A (ja) * | 2007-03-29 | 2008-10-16 | Kawasaki Plant Systems Ltd | プラズマ溶融炉 |
US20110268643A1 (en) * | 2008-10-09 | 2011-11-03 | Leblanc Johon R | Production of Silicon |
CN111057874A (zh) * | 2019-12-31 | 2020-04-24 | 三祥新材股份有限公司 | 一种金属锆母体原料用电熔氧化锆的制备方法 |
-
2022
- 2022-10-04 CN CN202211217441.8A patent/CN116462204A/zh active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4118464A (en) * | 1977-02-07 | 1978-10-03 | University Of Utah | Process for separating silica from silicate-bearing materials |
JPH0259416A (ja) * | 1988-08-25 | 1990-02-28 | Nippon Chem Ind Co Ltd | 微細溶融球状シリカおよびその製造法 |
JPH02199013A (ja) * | 1989-01-26 | 1990-08-07 | Nippon Chem Ind Co Ltd | 微細な溶融球状シリカの製造方法 |
JPH0733427A (ja) * | 1993-07-23 | 1995-02-03 | Nissan Gaadoraa Shokubai Kk | 細孔構造を制御した球状シリカ微粉体の製造方法 |
JP2008249220A (ja) * | 2007-03-29 | 2008-10-16 | Kawasaki Plant Systems Ltd | プラズマ溶融炉 |
US20110268643A1 (en) * | 2008-10-09 | 2011-11-03 | Leblanc Johon R | Production of Silicon |
CN111057874A (zh) * | 2019-12-31 | 2020-04-24 | 三祥新材股份有限公司 | 一种金属锆母体原料用电熔氧化锆的制备方法 |
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