CN112759370A - 一种高强度陶瓷过滤膜的制备方法 - Google Patents

一种高强度陶瓷过滤膜的制备方法 Download PDF

Info

Publication number
CN112759370A
CN112759370A CN201910993045.6A CN201910993045A CN112759370A CN 112759370 A CN112759370 A CN 112759370A CN 201910993045 A CN201910993045 A CN 201910993045A CN 112759370 A CN112759370 A CN 112759370A
Authority
CN
China
Prior art keywords
support body
ceramic
drying
strength
nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910993045.6A
Other languages
English (en)
Inventor
丘助国
洪昱斌
方富林
蓝伟光
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suntar Membrane Technology Xiamen Co Ltd
Original Assignee
Suntar Membrane Technology Xiamen Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suntar Membrane Technology Xiamen Co Ltd filed Critical Suntar Membrane Technology Xiamen Co Ltd
Priority to CN201910993045.6A priority Critical patent/CN112759370A/zh
Priority to PCT/CN2020/092216 priority patent/WO2021073100A1/zh
Publication of CN112759370A publication Critical patent/CN112759370A/zh
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/0215—Silicon carbide; Silicon nitride; Silicon oxycarbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/024—Oxides
    • B01D71/027—Silicium oxide
    • 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
    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • 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
    • C04B35/14—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 silica
    • 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
    • C04B35/46—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 titanium oxides or titanates
    • 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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • 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
    • C04B35/622—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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • 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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
    • 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
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6021—Extrusion moulding
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606—Drying
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Filtering Materials (AREA)

Abstract

本发明公开了一种高强度陶瓷过滤膜的制备方法，支撑体陶瓷骨料颗粒在真空状态下升温至100‑300℃烘干24‑72h，再将预先配制分散好的纳米烧结助剂在真空状态下与陶瓷骨料颗粒进行混合、浸润，再对混合液加压至10‑20Mpa，保持压力陈腐12‑48h，将粉料从浆料中分离后烘干，加入成型助剂混合均匀后，再进行支撑体坯体成型，坯体阴干后再进行烘干烧结，后续在此支撑体上涂覆至少一层过滤膜，最终制备成陶瓷膜产品。本发明制得的高强度陶瓷膜，其抗折强度比同配方，但未经纳米烧结助剂分散液混合浸润的陶瓷膜强度可以提高20‑100％，产品强度合格率高达100％，且强度测试值偏差在±3％以内，远低于常规产品的±25％偏差，产品稳定性大幅度提高。

Description

一种高强度陶瓷过滤膜的制备方法
技术领域
本发明属于陶瓷膜制备技术领域，具体涉及一种高强度陶瓷过滤膜的制备方法。
背景技术
膜与膜过程是20世纪60年代开始快速发展起来的高新技术领域。世界各国都高度重视，将其放在科技创新和国民经济发展的重要地位。相较于传统聚合物分离膜材料，陶瓷膜具有化学稳定性好，能耐酸、耐碱、耐有机溶剂；机械强度大，可反向冲洗；抗微生物能力强；耐高温；孔径分布窄、分离效率高等优点，在食品工业、生物工程、环境工程、化学工业、石油化工、冶金工业等领域得到了广泛的应用。
陶瓷膜主要以不同规格的氧化铝、氧化锆、氧化钛和氧化硅等无机陶瓷材料作为支撑体，经表面涂膜、高温烧制而成。商品化的陶瓷膜通常具有三层结构(多孔支撑层、过渡层及分离层)，呈非对称分布，其孔径规格为0.8nm～1μm不等，过滤精度涵盖微滤、超滤、纳滤级别。
其中，陶瓷膜支撑体的制备采用实心氧化铝、碳化硅或者氧化硅等陶瓷颗粒作为骨架颗粒，并辅助添加少量金属氧化物细颗粒以及各种降低烧结温度的烧结助剂，混以成型胶体后通过各种成型方式和烧结工艺进行烧结，最终形成具有一定孔隙率和强度的陶瓷膜支撑体结构。目前市场上的作为陶瓷膜支撑体的氧化铝、碳化硅或者氧化硅等陶瓷骨料颗粒在制备过程中，都会经历破碎、筛分的过程。破碎过程中，大部分颗粒破碎为无宏观内部缺陷的独立颗粒体。但仍有一些陶瓷颗粒虽受外力冲击内部产生裂纹，但因为裂纹过短或者过小，颗粒并未沿着裂纹断裂开来，而是产生了一个带裂纹缺陷的陶瓷颗粒。受不同陶瓷原材料厂家产品不同纯度、不同制备方式、不同破碎和筛分方法的影响，这些有宏观缺陷的骨料颗粒含量从1％-50％不等。
现有的陶瓷支撑体的制备工艺中，其烧结助剂的添加方式为直接机械混合。由于上述陶瓷骨料颗粒缺陷裂纹较狭窄，且裂纹破碎后表面会吸附空气和水分，呈团聚状态的烧结助剂根本无法渗入裂纹内部，也无法进行内部裂纹表面的附着。在支撑体烧结过程中，这些骨料颗粒内部的裂纹因为没有烧结助剂覆盖，烧结温度又无法达到熔融温度，故其裂纹无法修复或者烧结在一起。由此成为支撑体成品的内部裂纹缺陷(见图1)。这些裂纹缺陷在膜管运输使用过程中，非常容易受外力震动影响产生裂纹扩展，并使陶瓷膜管断裂报废。且这些颗粒内部的裂纹缺陷在使用过程中也容易受化学腐蚀，严重影响陶瓷膜管的使用安全和使用寿命。
发明内容
本发明的目的在于克服现有技术缺陷，提供一种高强度陶瓷过滤膜的制备方法。
本发明的技术方案如下：
一种高强度陶瓷过滤膜的制备方法，包括如下步骤：
(1)将纳米烧结助剂与水混合制成纳米烧结助剂分散液；
(2)将支撑体陶瓷骨料颗粒在真空状态下升温至100-300℃，保温烘干24-72h，以将支撑体陶瓷骨料颗粒中的裂纹表面吸附的水分和气体排除；
(3)在真空状态下，将步骤(2)所得的物料与步骤(1)所得的纳米烧结助剂分散液充分混合浸润，得混合液；
(4)将上述混合液置于10-20MPa的压力下，保压陈腐12-48h至支撑体陶瓷骨料颗粒所有外表面及裂纹充分粘附纳米烧结助剂后，进行固液分离，所得固体进行烘干；
(5)将步骤(4)所得的烘干后的固体与成型助剂混合均匀后，进行支撑体坯体成型；
(6)将所得的支撑体坯体阴干后再进行烘干烧结，获得支撑体；
(7)在步骤(6)获得的支撑体上涂覆至少一层过滤膜，即得所述高强度陶瓷过滤膜。
在本发明的一个优选实施方案中，所述纳米烧结助剂的粒径为1-50nm。
在本发明的一个优选实施方案中，所述支撑体陶瓷骨料颗粒的粒径为10-60um。
在本发明的一个优选实施方案中，所述纳米烧结助剂分散液的浓度为1-10wt％。
在本发明的一个优选实施方案中，所述步骤(4)中的固液分离的方法为沉淀法或过筛网。
在本发明的一个优选实施方案中，所述步骤(5)中的支撑体坯体成型所用的方法为挤出成型法或者凝胶注模成型法。
在本发明的一个优选实施方案中，所述步骤(7)中的涂覆的方法为浸渍法或者喷涂法。
在本发明的一个优选实施方案中，所述纳米烧结助剂为纳米氧化钛或纳米氧化镁。
在本发明的一个优选实施方案中，所述支撑体陶瓷骨料颗粒为氧化硅微粉、碳化硅微粉或氧化铝微粉。
本发明的有益效果是：本发明制得的高强度陶瓷膜，其抗折强度比同配方，但未经纳米烧结助剂分散液混合浸润的陶瓷膜强度可以提高20-100％，产品强度合格率高达100％，且强度测试值偏差在±3％以内，远低于常规产品的±25％偏差，产品稳定性大幅度提高。
附图说明
图1为本发明背景技术中的陶瓷膜支撑体的扫描电镜照片。
图2为本发明实施例1制得的支撑体的扫描电镜照片。
图3为本发明实施例2制得的支撑体的扫描电镜照片。
图4为本发明实施例3制得的支撑体的扫描电镜照片。
具体实施方式
以下通过具体实施方式对本发明的技术方案进行进一步的说明和描述。
实施例1：
将氧化铝微粉(45um)在真空状态(-0.1Mpa)下升温至200℃烘干24h，然后在保持真空的状态下将预先配制的氧化钛分散液(10nm，5wt％，RO水为溶剂)与烘干后的氧化铝微粉进行充分混合、浸润，再对混合液加压至10Mpa，保持压力陈腐24h后将浆料中的粉体筛出并烘干备用。取烘干后的氧化铝与氧化钛混合粉(80wt％)，加入玉米淀粉(1um，3wt％)、PVA(1um，2wt％)用混料机混合4h，往混合好的粉料中加入RO水(13wt％)、甘油(2wt％)，再次混合4h后形成陶瓷泥料并陈腐48h。用真空练泥机对陈腐后的泥料进行真空(-0.1MPa)练泥后，采用挤出成型的方式成型陶瓷膜支撑体坯体。湿坯成型后室温阴干20h，然后用烘箱以1℃/min的速度升温至120℃烘干2h。最后采用高温烧结窑炉1750℃保温2h烧结成如图2所示的支撑体。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成陶瓷膜产品，其抗折强度提高34％至51MPa，产品强度合格率100％。
类别 强度MPa 泡压MPa 纯水通量LMH 强度合格率％
常规陶瓷膜 15-38 ≥0.30 ≥2000 89
本实施例陶瓷膜 51-52 ≥0.35 ≥2000 100
实施例2：
将碳化硅微粉(60um)在真空状态(-0.1Mpa)下升温至150℃烘干48h，然后在保持真空的状态下将预先配制的氧化钛分散液(5nm，5wt％，RO水为溶剂)与烘干后的碳化硅微粉进行充分混合、浸润，再对混合液加压至15Mpa，保持压力陈腐24h后将浆料中的粉体筛出并烘干备用。取烘干后的碳化硅与氧化钛混合粉(90wt％)、活性炭粉(20μm，3wt％)、PVA粉末(分子量2000，3wt％)、明胶粉末(纯度98％，4wt％)球磨2h混合均匀。加入RO水(混合粉末与RO水溶液的体积比为2.2∶1)，85℃水浴加温的条件下球磨分散20h制成分散均匀的浆料。浆料80℃保温状态下真空(-0.1MPa)除泡后立即浇注在模具中，坯体物理降温至20℃后原位凝固为具有一定强度的湿坯。湿坯脱模后室温阴干72h，80℃烘干72h。在空气气氛中，于1850℃保温烧结6h，制得如图3所示的支撑体。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成陶瓷膜产品，其抗折强度提高41％至65MPa，产品强度合格率100％。
类别 强度MPa 泡压MPa 纯水通量LMH 强度合格率％
常规陶瓷膜 26-46 ≥0.25 ≥2600 92
本实施例陶瓷膜 65-67 ≥0.35 ≥2800 100
实施例3：
将氧化硅微粉(30um)在真空状态(-0.1Mpa)下升温至250℃烘干72h，然后在保持真空的状态下将预先配制的氧化镁分散液(20nm，5wt％，RO水为溶剂)与烘干后的氧化硅微粉进行充分混合、浸润，再对混合液加压至20Mpa，保持压力陈腐72h后将浆料中的粉体筛出并烘干备用。取烘干后的氧化硅与氧化钛混合粉(85wt％)，加入玉米淀粉(1um，2wt％)、PVA(1um，2wt％)用混料机混合6h，往混合好的粉料中加入RO水(10wt％)、甘油(3wt％)，再次混合6h后形成陶瓷泥料并陈腐72h。用真空练泥机对陈腐后的泥料进行真空(-0.1MPa)练泥后，采用挤出成型的方式成型陶瓷膜支撑体坯体。湿坯成型后室温阴干24h，然后用烘箱以1℃/min的速度升温至105℃烘干4h。最后采用高温烧结窑炉1550℃保温6h烧结成如图4所示的支撑体。后续在此支撑体上通过浸渍或者喷涂等陶瓷过滤膜制膜工艺涂覆一层或者多层过滤膜，最终制备成陶瓷膜产品，其抗折强度提高64％至41MPa，产品强度合格率100％。
类别 强度MPa 泡压MPa 纯水通量LMH 强度合格率％
常规陶瓷膜 12-25 ≥0.20 ≥1800 73
本实施例陶瓷膜 41-42 ≥0.25 ≥1800 100
以上所述，仅为本发明的较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (9)

1.一种高强度陶瓷过滤膜的制备方法，其特征在于：包括如下步骤：
(1)将纳米烧结助剂与水混合制成纳米烧结助剂分散液；
(2)将支撑体陶瓷骨料颗粒在真空状态下升温至100-300℃，保温烘干24-72h，以将支撑体陶瓷骨料颗粒中的裂纹表面吸附的水分和气体排除；
(3)在真空状态下，将步骤(2)所得的物料与步骤(1)所得的纳米烧结助剂分散液充分混合浸润，得混合液；
(4)将上述混合液置于10-20MPa的压力下，保压陈腐12-48h至支撑体陶瓷骨料颗粒所有外表面及裂纹充分粘附纳米烧结助剂后，进行固液分离，所得固体进行烘干；
(5)将步骤(4)所得的烘干后的固体与成型助剂混合均匀后，进行支撑体坯体成型；
(6)将所得的支撑体坯体阴干后再进行烘干烧结，获得支撑体；
(7)在步骤(6)获得的支撑体上涂覆至少一层过滤膜，即得所述高强度陶瓷过滤膜。
2.如权利要求1所述的制备方法，其特征在于：所述纳米烧结助剂的粒径为1-50nm。
3.如权利要求1所述的制备方法，其特征在于：所述支撑体陶瓷骨料颗粒的粒径为10-60um。
4.如权利要求1所述的制备方法，其特征在于：所述纳米烧结助剂分散液的浓度为1-10wt％。
5.如权利要求1所述的制备方法，其特征在于：所述步骤(4)中的固液分离的方法为沉淀法或过筛网。
6.如权利要求1所述的制备方法，其特征在于：所述步骤(5)中的支撑体坯体成型所用的方法为挤出成型法或者凝胶注模成型法。
7.如权利要求1所述的制备方法，其特征在于：所述步骤(7)中的涂覆的方法为浸渍法或者喷涂法。
8.如权利要求1至7中任一权利要求所述的制备方法，其特征在于：所述纳米烧结助剂为纳米氧化钛或纳米氧化镁。
9.如权利要求1至7中任一权利要求所述的制备方法，其特征在于：所述支撑体陶瓷骨料颗粒为氧化硅微粉、碳化硅微粉或氧化铝微粉。
CN201910993045.6A 2019-10-18 2019-10-18 一种高强度陶瓷过滤膜的制备方法 Pending CN112759370A (zh)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201910993045.6A CN112759370A (zh) 2019-10-18 2019-10-18 一种高强度陶瓷过滤膜的制备方法
PCT/CN2020/092216 WO2021073100A1 (zh) 2019-10-18 2020-05-26 一种高强度陶瓷过滤膜的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910993045.6A CN112759370A (zh) 2019-10-18 2019-10-18 一种高强度陶瓷过滤膜的制备方法

Publications (1)

Publication Number Publication Date
CN112759370A true CN112759370A (zh) 2021-05-07

Family

ID=75538301

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910993045.6A Pending CN112759370A (zh) 2019-10-18 2019-10-18 一种高强度陶瓷过滤膜的制备方法

Country Status (2)

Country Link
CN (1) CN112759370A (zh)
WO (1) WO2021073100A1 (zh)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114452834A (zh) * 2022-01-18 2022-05-10 重庆兀盾纳米科技有限公司 碟式陶瓷膜
CN114920564A (zh) * 2022-05-07 2022-08-19 刘峻廷 一种高纯碳化硼管式陶瓷过滤膜制备方法
CN115231902A (zh) * 2022-07-10 2022-10-25 上海熊猫机械(集团)有限公司 W型氧化铝支撑碳化硅陶瓷膜及其制备方法
CN115894072A (zh) * 2022-12-29 2023-04-04 江苏省宜兴非金属化工机械厂有限公司 一种耐腐蚀陶瓷过滤板及其制备方法
CN116550164A (zh) * 2023-05-25 2023-08-08 江西陶瓷工艺美术职业技术学院 一种纳滤陶瓷膜的制备方法及其制得的产品

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114225715B (zh) * 2021-11-17 2022-09-20 华南理工大学 一种高性能非对称陶瓷过滤膜及其制备方法

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101913884A (zh) * 2010-07-16 2010-12-15 西安电子科技大学 利用柠檬酸盐溶胶处理铝质耐火材料颗粒的方法
CN102010187A (zh) * 2010-10-01 2011-04-13 江苏省陶瓷研究所有限公司 一种多孔陶瓷过滤管用的陶瓷膜及其改性制备方法
CN102092993A (zh) * 2010-11-25 2011-06-15 浙江大学 一种再生骨料混凝土的纳米强化方法
CN102380321A (zh) * 2011-09-07 2012-03-21 三达膜科技（厦门）有限公司 一种氧化铝陶瓷膜膜层的制备方法
CN102408250A (zh) * 2011-07-25 2012-04-11 三达膜科技（厦门）有限公司 一种陶瓷膜支撑体及其制备方法
CN102584269A (zh) * 2012-01-11 2012-07-18 浙江大学 一种有钛酸铝涂层的耐火材料颗粒及其制备方法
CN102806018A (zh) * 2012-07-12 2012-12-05 三达膜环境技术股份有限公司 一种低温烧结制备耐酸碱二氧化钛陶瓷超滤膜的方法
CN105561803A (zh) * 2015-12-29 2016-05-11 合肥创想能源环境科技有限公司 一种大通量、高精度高温凝结水除油除铁用陶瓷超滤膜的制备方法
CN106242624A (zh) * 2016-08-02 2016-12-21 山东华瓷环保设备科技有限公司 一种氧化铝多通道陶瓷膜支撑体的制备方法
CN107793158A (zh) * 2017-11-22 2018-03-13 山东华瓷环保设备科技有限公司 一种碳化硅多通道陶瓷膜的制备工艺

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19857590B4 (de) * 1998-12-14 2004-09-09 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Keramische Flachmembran und Verfahren zu ihrer Herstellung
CN104587846B (zh) * 2014-12-24 2016-05-18 长安大学 一种低温烧结制备多孔陶瓷滤膜的方法
CN107337442A (zh) * 2017-07-11 2017-11-10 芜湖市宝艺游乐科技设备有限公司 一种颗粒稳定发泡工艺制备氧化铝陶瓷支撑体及其制备方法
CN107619281B (zh) * 2017-08-03 2020-06-30 浙江理工大学 一种低温烧结耐酸碱多孔碳化硅陶瓷支撑体的制备方法
CN108392990A (zh) * 2018-02-24 2018-08-14 江苏新时高温材料股份有限公司 一种中空平板全陶瓷过滤膜元件

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101913884A (zh) * 2010-07-16 2010-12-15 西安电子科技大学 利用柠檬酸盐溶胶处理铝质耐火材料颗粒的方法
CN102010187A (zh) * 2010-10-01 2011-04-13 江苏省陶瓷研究所有限公司 一种多孔陶瓷过滤管用的陶瓷膜及其改性制备方法
CN102092993A (zh) * 2010-11-25 2011-06-15 浙江大学 一种再生骨料混凝土的纳米强化方法
CN102408250A (zh) * 2011-07-25 2012-04-11 三达膜科技（厦门）有限公司 一种陶瓷膜支撑体及其制备方法
CN102380321A (zh) * 2011-09-07 2012-03-21 三达膜科技（厦门）有限公司 一种氧化铝陶瓷膜膜层的制备方法
CN102584269A (zh) * 2012-01-11 2012-07-18 浙江大学 一种有钛酸铝涂层的耐火材料颗粒及其制备方法
CN102806018A (zh) * 2012-07-12 2012-12-05 三达膜环境技术股份有限公司 一种低温烧结制备耐酸碱二氧化钛陶瓷超滤膜的方法
CN105561803A (zh) * 2015-12-29 2016-05-11 合肥创想能源环境科技有限公司 一种大通量、高精度高温凝结水除油除铁用陶瓷超滤膜的制备方法
CN106242624A (zh) * 2016-08-02 2016-12-21 山东华瓷环保设备科技有限公司 一种氧化铝多通道陶瓷膜支撑体的制备方法
CN107793158A (zh) * 2017-11-22 2018-03-13 山东华瓷环保设备科技有限公司 一种碳化硅多通道陶瓷膜的制备工艺

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
唐钰栋等: "水处理用陶瓷平板膜制备", 《现代技术陶瓷》 *
薛云飞等: "《先进金属基复合材料》", 30 April 2019, 北京理工大学出版社 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114452834A (zh) * 2022-01-18 2022-05-10 重庆兀盾纳米科技有限公司 碟式陶瓷膜
CN114452834B (zh) * 2022-01-18 2023-11-03 重庆兀盾纳米科技有限公司 碟式陶瓷膜
CN114920564A (zh) * 2022-05-07 2022-08-19 刘峻廷 一种高纯碳化硼管式陶瓷过滤膜制备方法
CN115231902A (zh) * 2022-07-10 2022-10-25 上海熊猫机械(集团)有限公司 W型氧化铝支撑碳化硅陶瓷膜及其制备方法
CN115894072A (zh) * 2022-12-29 2023-04-04 江苏省宜兴非金属化工机械厂有限公司 一种耐腐蚀陶瓷过滤板及其制备方法
CN115894072B (zh) * 2022-12-29 2024-03-08 江苏省宜兴非金属化工机械厂有限公司 一种耐腐蚀陶瓷过滤板及其制备方法
CN116550164A (zh) * 2023-05-25 2023-08-08 江西陶瓷工艺美术职业技术学院 一种纳滤陶瓷膜的制备方法及其制得的产品

Also Published As

Publication number Publication date
WO2021073100A1 (zh) 2021-04-22

Similar Documents

Publication Publication Date Title
CN112759370A (zh) 一种高强度陶瓷过滤膜的制备方法
CN107200599B (zh) 多孔氧化铝陶瓷及其制备方法和应用
CN111545078A (zh) 平板陶瓷膜及其制备方法
CN103819219B (zh) 一种耐酸碱腐蚀的碳化硅多孔支撑体
WO2017004776A1 (zh) 多孔氧化铝陶瓷及其制备方法
CN101670244B (zh) 制备具有梯度孔陶瓷纳滤膜支撑体的方法
CN107915475B (zh) 一种梯度孔高温过滤陶瓷管及其制备方法
CN113896516B (zh) 一种石英陶瓷辊的制备方法
CN112407936B (zh) 一种多孔真空吸盘及其制备方法
US10017423B2 (en) Method for preparing support of molecular sieve membrane
CN113842787B (zh) 一种埃洛石纳米管增强的超薄陶瓷膜及其制备方法
EP3124104B1 (en) Monolithic separation membrane structure, and method for producing monolithic separation membrane structure
US20110171099A1 (en) Process for manufacturing a porous sic material
CN110981453B (zh) 一种轻质陶瓷过滤膜的制备方法
US6254822B1 (en) Production of porous mullite bodies
CN113651633B (zh) 一种莫来石纤维增强碳化硅陶瓷过滤管及其制备方法
CN109454231B (zh) 一种铁铝铜合金微孔过滤材料的制备方法
CN114307664B (zh) 一种高通量抗污染陶瓷过滤膜及其制备方法
JP2001340718A (ja) ハニカムフィルタ用基材及びその製造方法
CN115073202B (zh) 一种基于粘结剂喷射的梯度孔结构陶瓷膜及其制备方法和应用
CN107721259B (zh) 一种高性能透水砖
JP2007268463A (ja) フィルター材の製造方法
CN114133270B (zh) 中空平板陶瓷过滤膜及其制备方法
CN110898683B (zh) 一种陶瓷过滤膜的制备方法
CN116675555B (zh) 一种硅藻土基分级多孔隔热陶瓷及其制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210507