CN106102877A - 整体型分离膜结构体及其制造方法 - Google Patents
整体型分离膜结构体及其制造方法 Download PDFInfo
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- CN106102877A CN106102877A CN201580009164.3A CN201580009164A CN106102877A CN 106102877 A CN106102877 A CN 106102877A CN 201580009164 A CN201580009164 A CN 201580009164A CN 106102877 A CN106102877 A CN 106102877A
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- silica
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- 238000000926 separation method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 51
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 25
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011148 porous material Substances 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 description 15
- 238000007789 sealing Methods 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 229960005363 aluminium oxide Drugs 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 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 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000007591 painting process Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
整体型分离膜结构体(100)包括:基材(211)、第一支撑层(212)及分离膜(300)。基材(211)由多孔质材料构成,且具有多个贯通孔(TH)。第一支撑层(212)形成在多个贯通孔(TH)的内表面(211S)上。分离膜(300)配置在第一支撑层(212)的内侧。第一支撑层(212)含有骨料、无机粘结剂及烧结助剂,其中,骨料以氧化铝为主成分,无机粘结剂以二氧化钛为主成分,烧结助剂以二氧化硅和氧化镁中的至少一者为主成分。
Description
技术领域
本发明涉及整体型分离膜结构体(monolithic separation membranestructure)及其制造方法。
背景技术
目前,已知包括具有多个贯通孔的基材、形成在贯通孔的内表面的支撑层、及形成在支撑层的内表面的分离膜的整体型分离膜结构体(参见专利文献1)。专利文献1中提出了在支撑层中添加二氧化钛作为粘结剂以便改善支撑层的强度和耐化学性的方案。
现有专利文献
专利文献
专利文献1:国际公开第2013/059146号
发明内容
另一方面,为了使整体型分离膜结构体的过滤效率得到改善,有效方案是减薄支撑层的厚度而扩大分离膜的表面积。因此,为了减薄支撑层的厚度,要求进一步提高支撑层的强度。
本发明是鉴于上述情况而完成的,目的是提供能够提高支撑层的强度的整体型分离膜结构体及其制造方法。
本发明所涉及的整体型分离膜结构体包括:基材主体、第一支撑层、及分离膜。基材主体由多孔质材料构成,且具有多个贯通孔。第一支撑层形成在多个贯通孔的内表面。分离膜配置在第一支撑层的内侧。第一支撑层含有二氧化硅和氧化镁中的至少一者、以及氧化铝和二氧化钛。
根据本发明,能够提供可以提高支撑层的强度的整体型分离膜结构体及其制造方法。
附图说明
图1是整体型分离膜结构体的立体图。
图2是图1的A-A截面图。
图3是图2的B-B截面图。
具体实施方式
下面,参照附图,说明本发明的实施方式。以下的附图的记载中,对相同或类似的部分赋予相同或类似的符号。但是,附图是示意性的,各尺寸的比率等有时与现实的比率不同。因此,具体的尺寸等应该参考以下的说明进行判断。另外,附图相互之间当然也包含相互的尺寸关系、比率不同的部分。
以下的实施方式中,所谓“整体(monolithic)”,是指具有形成在长度方向的多个贯通孔的形状,是包括蜂窝形状的概念。
(整体型分离膜结构体100的构成)
图1是整体型分离膜结构体100的立体图。图2是图1的A-A截面图。图3是图2的B-B截面图。
整体型分离膜结构体100包括:整体型基材200和分离膜300。
整体型基材200具有:基材主体210、第一密封部220、及第二密封部230。
基材主体210是多孔体。基材主体210被形成为圆柱状。可以使长度方向上的基材主体210的长度为150~2000mm,可以使宽度方向上的基材主体210的直径为30~220mm,但并不限定于此。
基材主体210具有:第一端面S1、第二端面S2、及侧面S3。第一端面S1设置在第二端面S2的相反侧。侧面S3与第一端面S1和第二端面S2的外缘连接。
基材主体210包括:基材211、第一支撑层212、及第二支撑层213。
基材211被形成为圆柱状。在基材211中形成有多个贯通孔TH。贯通孔TH从第一端面S1贯通基材211至第二端面S2。贯通孔TH的截面形状为圆形,但并不限定于圆形。可以使贯通孔TH的内径为1~5mm。通过增大贯通孔TH的内径,能够扩大后述隔室C的内径。
基材211由多孔质材料构成。作为基材211的多孔质材料,可以使用陶瓷、金属、树脂等,特别优选多孔质陶瓷材料。作为多孔质陶瓷材料的骨料粒子,可以使用氧化铝(Al2O3)、二氧化钛(TiO2)、多铝红柱石(Al2O3·SiO2)、陶瓷屑及堇青石(Mg2Al4Si5O18)等,如果考虑易得性、坯土稳定性及耐腐蚀性,则特别优选氧化铝。
基材211除含有多孔质材料以外,还可以含有无机粘结剂。作为无机粘结剂,可以使用二氧化钛、多铝红柱石、易烧结性氧化铝、二氧化硅、玻璃料、粘土矿物、易烧结性堇青石中的至少一种。可以使基材211的气孔率为25%~50%。可以使基材211的平均细孔径为5μm~25μm。可以使构成基材211的多孔质材料的平均粒径为5μm~100μm。
本实施方式中,所谓“平均粒径”,是使用SEM(Scanning Electron Microscope)观察截面微结构所测得的30个待测粒子的最大直径的算术平均值。
第一支撑层212形成在基材211的贯通孔TH的内表面211S。第一支撑层212被形成为筒状。第一支撑层212由多孔质陶瓷材料构成。具体而言,第一支撑层212含有骨料、无机粘结剂及烧结助剂。
第一支撑层212的骨料含有氧化铝作为主成分。第一支撑层212的无机粘结剂含有二氧化钛作为主成分。无机粘结剂的二氧化钛粒子形成被覆骨料的氧化铝粒子中的至少一部分的粘结颈部(binding neck)。
第一支撑层212的烧结助剂含有二氧化硅和氧化镁中的至少一者作为主成分。烧结助剂中的二氧化硅、氧化镁,在烧结第一支撑层212的成型体时,促进成型体的烧结。二氧化硅成分、氧化镁成分存在于二氧化钛粒子间或二氧化钛粒子和氧化铝粒子的晶界中。由此,二氧化硅成分、氧化镁成分分布在无机粘结剂附近,从而提高了第一支撑层212的强度。
可以使第一支撑层212中的二氧化钛浓度为5重量%~40重量%,优选为10重量%~30重量%。第一支撑层212含有二氧化硅作为烧结助剂的情况下,可以使第一支撑层212中的二氧化硅浓度为0.1重量%~40重量%,优选为1重量%~30重量%,更优选为0.25重量%~6重量%。
第一支撑层212含有氧化镁作为烧结助剂的情况下,可以使第一支撑层212中的氧化镁浓度为0.1重量%~20重量%,优选为0.5重量%~5重量%。
另外,第一支撑层212含有二氧化硅和氧化镁这两者作为烧结助剂的情况下,可以使第一支撑层212中的二氧化硅浓度为0.1重量%~40重量%,使第一支撑层212中的氧化镁浓度为0.1重量%~20重量%。
本实施方式中,烧结助剂的浓度是烧结助剂重量/(骨料重量+无机粘合剂重量)×100%。本实施方式中,可以通过EDS(Energy Dispersive x-ray Spectroscopy)来测定各成分的浓度。
本实施方式中,所谓组合物X含有物质Y“作为主成分”,是指在组合物X整体中,物质Y优选占60重量%以上,更优选占70重量%以上,进一步优选占90重量%以上。
可以使与贯通孔TH的中心轴垂直的方向(以下称为“径向”。)上的第一支撑层212的厚度为100μm~300μm。本实施方式中,如上所述,因为通过添加二氧化硅和氧化镁中的至少一者使第一支撑层212的强度得到了提高,所以能够通过减薄第一支撑层212的厚度来扩大每一个过滤器的分离膜300的表面积。
可以使第一支撑层212的气孔率为5%~60%。可以使第一支撑层212的平均细孔径小于基材211的平均细孔径,达到0.005μm~5μm。
第二支撑层213形成在第一支撑层212的内表面212S上。第二支撑层213被形成为筒状。第二支撑层213由多孔质陶瓷材料构成。具体而言,第二支撑层213含有骨料和烧结助剂。第二支撑层213的骨料含有氧化铝作为主成分。第二支撑层213的烧结助剂含有二氧化硅和氧化镁中的至少一者作为主成分。二氧化硅、氧化镁,在烧结第二支撑层213的成型体时,促进成型体的烧结。烧结助剂的二氧化硅成分、氧化镁成分分布在骨料的氧化铝粒子间。
第二支撑层213含有二氧化硅作为烧结助剂的情况下,优选第二支撑层213中的二氧化硅浓度为0.01重量%~40重量%。第二支撑层213含有氧化镁作为烧结助剂的情况下,优选第二支撑层213中的氧化镁浓度为0.01重量%~40重量%。
另外,第二支撑层213含有二氧化硅和氧化镁这两者作为烧结助剂的情况下,优选第二支撑层213中的二氧化硅浓度为0.01重量%~10重量%,且第二支撑层213中的氧化镁浓度为0.01重量%~10重量%。
可以使径向上的第二支撑层213的厚度为1μm~40μm。可以使第二支撑层213的气孔率为5%~40%。可以使第二支撑层213的平均细孔径小于第一支撑层212的平均细孔径,达到0.005μm~2μm。
第一密封部220覆盖第一端面S1的整面和侧面S3的一部分。第一密封部220抑制流入贯通孔TH的待过滤混合流体从第一端面S1直接渗透到基材主体210中。以不会堵塞后述隔室C的流入口的方式形成第一密封部220。作为构成第一密封部220的材料,可以使用玻璃、金属等,但如果考虑与基材主体210的热膨胀系数的匹配性,则优选玻璃。
第二密封部230覆盖第二端面S2的整面和侧面S3的一部分。第二密封部230抑制从贯通孔TH流出的混合流体从第二端面S2直接渗透到基材主体210中。以不会堵塞隔室C的流出口的方式形成第二密封部230。第二密封部230可以由与第一密封部220同样的材料构成。
分离膜300被形成为筒状。分离膜300配置在贯通孔TH的内侧。本实施方式中,分离膜300形成在第二支撑层213的内表面213S上。在分离膜300的内表面300S的内侧形成有用于使混合流体流通的隔室C。可以使径向上的隔室C的内径为0.5mm~3.5mm。隔室C的内径会对内压强度和分离效率带来影响。可通过扩大基材211的贯通孔TH的内径或第一支撑层212的薄膜化来增大隔室C的内径。通过增大隔室C的内径,能够扩大分离膜300的表面300S的表面积。
分离膜300优选由无机材料、金属等构成。作为分离膜300的无机材料,可以举出沸石、碳、二氧化硅等。作为分离膜300的金属材料,可以举出钯等。分离膜300为沸石膜的情况下,可以使用LTA、MFI、MOR、FER、FAU、DDR、CHA、BEA等晶体结构的沸石。分离膜300为DDR型沸石膜的情况下,可以优选用作选择性地分离二氧化碳的气体分离膜。
径向上的分离膜300的厚度优选为10μm以下,更优选为5μm以下。可以使分离膜300的气孔率为0%~20%。可以使分离膜300的平均细孔径小于第一支撑层212、第二支撑层213的平均细孔径,达到0.1nm~1μm。
(整体型分离膜结构体100的制造方法)
首先,使用含有多孔质材料的坯土形成具有多个贯通孔TH的基材211的成型体。作为形成基材211的成型体的方法,除使用了真空挤压成型机的挤压成型法以外,还可以使用冲压成型法、浇铸成型法。
接着,对基材211的成型体进行烧成(例如、900℃~1600℃、0小时~100小时),由此,形成基材211。
接着,在作为骨料的氧化铝和作为无机粘结剂的二氧化钛中添加作为烧结助剂的二氧化硅和氧化镁中的至少一者、有机粘合剂、pH调整剂、表面活性剂等来制备第一支撑层用浆料。
接着,使用第一支撑层用浆料通过过滤法形成第一支撑层212的成型体。具体而言,一边将第一支撑层用浆料供给到基材211的贯通孔TH中,一边用泵从基材211的侧面S3进行抽吸,由此,使第一支撑层212的成型体沉积在贯通孔TH的内表面211S上。
接着,对第一支撑层212的成型体进行烧成(例如、900℃~1600℃、0.5小时~100小时),由此,形成第一支撑层212。
接着,在作为骨料的氧化铝中添加作为烧结助剂的二氧化硅和氧化镁中的至少一者、有机粘合剂、pH调整剂、表面活性剂等来制备第二支撑层用浆料。
接着,使用第二支撑层用浆料通过过滤法形成第一支撑层212的成型体。具体而言,一边将第二支撑层用浆料供给到筒状的第一支撑层212的内侧,一边用泵从基材211的侧面S3进行抽吸,由此,使第二支撑层213的成型体沉积在第一支撑层212的内表面212S上。
接着,对第二支撑层213的成型体进行烧成(例如、900℃~1600℃、0.5小时~100小时),由此,形成第二支撑层213。
接着,在第二支撑层213的内表面213S上形成分离膜300。作为分离膜300的形成方法,只要根据分离膜300的种类使用适当的方法即可。例如形成DDR型沸石膜作为分离膜300的情况下,依次实施:基于流下法的晶种引入工序、溶胶的水热合成工序、用于除去结构导向剂的加热工序。另外,形成二氧化硅膜作为分离膜300的情况下,依次实施:二氧化硅溶胶液的附着工序、烧成工序(150℃~800℃、0小时~100小时)。另外,形成碳膜作为分离膜300的情况下,依次实施:前驱体溶液的涂布工序、烧成工序(150℃~800℃、0小时~100小时)。
(其它实施方式)
以上说明了本发明的一个实施方式,但本发明并不限定于上述实施方式,可以在不脱离发明的主旨的范围内进行多种变更。
(A)上述实施方式中,整体型基材200具有基材主体210、第一密封部220及第二密封部230,也可以不具有第一密封部220和第二密封部230中的至少一者。
(B)上述实施方式中,基材主体210具有基材211、第一支撑层212及第二支撑层213,也可以不具有第二支撑层213。在这种情况下,分离膜300形成在第一支撑层212的内表面212S上。
(C)上述实施方式中没有特别提到,基材主体210可以在基材211和第一支撑层212之间具有第三支撑层。第三支撑层可以由与基材211同样的材料构成,但通过由与第一支撑层212同样的材料构成第三支撑层,能够使强度进一步提高。
另外,基材主体210可以在第一支撑层212和第二支撑层213之间具有第四支撑层。第四支撑层可以由与基材211同样的材料构成,但通过由与第一支撑层212同样的材料构成第四支撑层,能够使强度进一步提高。
(D)上述实施方式中,隔室C的截面形状为矩形,也可以为圆形、椭圆形或者多边形。
实施例
以下,说明本发明的实施例。但是,本发明并不限定于以下说明的实施例。
(样品No.1~14的制作)
如下制作样品No.1~14所涉及的整体型分离膜结构体。
首先,在平均粒径10μm的氧化铝100质量份中添加玻璃料10质量份,再加入水、分散剂及增稠剂,进行混炼,由此,制备出坯土。
接着,对制备的坯土进行挤压成型,由此,制作出具有多个贯通孔的基材的成型体。
接着,对基材的成型体进行烧成(1250℃、1小时)来制作基材。
接着,在作为骨料的氧化铝和作为无机粘结剂的二氧化钛中添加有机粘合剂、pH调整剂、表面活性剂等来制备第一支撑层用浆料。此时,如表1所示,样品No.3~8、10、11中,添加二氧化硅粉末作为烧结助剂,样品No.12~14中,添加二氧化硅溶胶作为烧结助剂,样品No.9中,添加氧化镁粉末作为烧结助剂。相对氧化铝和二氧化钛的总重量而言,二氧化硅粉末、二氧化硅溶胶及氧化镁粉末各自的添加量如表1所示。
接着,一边将第一支撑层用浆料供给到基材的贯通孔中,一边用泵从基材的侧面进行抽吸,由此,使第一支撑层的成型体沉积在贯通孔的内表面上。
接着,对第一支撑层的成型体进行烧成(1250℃、1小时)。
接着,在作为骨料的氧化铝中添加作为烧结助剂的醋酸镁、有机粘合剂、pH调整剂、表面活性剂等来制备第二支撑层用浆料。
接着,对第二支撑层的成型体进行烧成(1250℃、10小时)。
接着,在第二支撑层的内表面上形成DDR膜。
(强度的测定)
将各样品装入分离装置内,使加压水在DDR膜的内部(即、隔室)流通,缓慢增大加压力至各样品被破坏。表1中,记载各样品被破坏时的加压力(MPa)作为破坏强度。
【表1】
如表1所示,在第一支撑层中添加二氧化硅粉末、二氧化硅溶胶或者氧化镁粉末作为烧结助剂得到的样品No.3~14,与未在第一支撑层中添加烧结助剂的样品No.1、2相比,能够使破坏强度得到提高。特别是使第一支撑层的厚度为150μm的样品No.10、11,也能够实现充分的破坏强度。
另外,如表1所示,通过使第一支撑层中的二氧化硅浓度为0.25重量%~6重量%,能够使破坏强度进一步提高。应予说明,已经通过EDS分析确认到第一支撑层中的二氧化硅浓度与添加量一致。
另外,如表1所示,添加二氧化硅粉末作为烧结助剂的情况和添加二氧化硅溶胶作为烧结助剂的情况中,能够确认得到同样的效果。进而,添加二氧化硅作为烧结助剂的情况和添加氧化镁作为烧结助剂的情况中,也能够确认得到同样的效果。
符号说明
100 整体型分离膜结构体
200 整体型基材
210 基材主体
211 基材
212 第一支撑层
213 第二支撑层
300 分离膜
TH 贯通孔
Claims (4)
1.一种整体型分离膜结构体,包括:
基材,所述基材由多孔质材料构成,且具有多个贯通孔,
第一支撑层,所述第一支撑层形成在所述多个贯通孔的内表面,
分离膜,所述分离膜配置在所述第一支撑层的内侧;
所述第一支撑层含有二氧化硅和氧化镁中的至少一者、以及氧化铝和二氧化钛。
2.根据权利要求1所述的整体型分离膜结构体,其中,
所述第一支撑层中的二氧化硅浓度为0.25重量%~6重量%。
3.根据权利要求1或2所述的整体型分离膜结构体,其中,
包括:第二支撑层,所述第二支撑层形成在所述第一支撑层的内表面,
所述分离膜形成在所述第二支撑层的内表面,
所述第二支撑层含有二氧化硅和氧化镁中的至少一者、以及氧化铝。
4.一种整体型分离膜结构体的制造方法,包括以下工序:
使用多孔质材料形成具有多个贯通孔的基材的成型体,
对所述基材的成型体进行烧成,
使用含有骨料、无机粘结剂及烧结助剂的材料,在所述多个贯通孔的内表面形成第一支撑层的成型体,其中,骨料以氧化铝为主成分,无机粘结剂以二氧化钛为主成分,烧结助剂以二氧化硅和氧化镁中的至少一者为主成分,
对所述第一支撑层的成型体进行烧成,
在所述第一支撑层的内侧形成分离膜。
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