CN104609450A - Process and complete industrial installation for producing highly dispersed magnalium hydrotalcite powder bodies - Google Patents
Process and complete industrial installation for producing highly dispersed magnalium hydrotalcite powder bodies Download PDFInfo
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- CN104609450A CN104609450A CN201410528456.5A CN201410528456A CN104609450A CN 104609450 A CN104609450 A CN 104609450A CN 201410528456 A CN201410528456 A CN 201410528456A CN 104609450 A CN104609450 A CN 104609450A
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- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910001051 Magnalium Inorganic materials 0.000 title 1
- 238000009434 installation Methods 0.000 title 1
- 239000002270 dispersing agent Substances 0.000 claims abstract description 79
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 71
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 71
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 71
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 69
- 238000001035 drying Methods 0.000 claims abstract description 59
- 239000012065 filter cake Substances 0.000 claims abstract description 38
- 230000004048 modification Effects 0.000 claims abstract description 33
- 238000012986 modification Methods 0.000 claims abstract description 33
- 238000000967 suction filtration Methods 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims abstract description 23
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 230000008929 regeneration Effects 0.000 claims abstract description 19
- 238000011069 regeneration method Methods 0.000 claims abstract description 19
- 230000005587 bubbling Effects 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 10
- 239000002351 wastewater Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 238000009826 distribution Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 150000001450 anions Chemical class 0.000 claims description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 5
- 238000009776 industrial production Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- -1 Inorganic acid anions Chemical class 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
- 238000001223 reverse osmosis Methods 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 3
- 229910052623 talc Inorganic materials 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 claims description 2
- 229910020366 ClO 4 Inorganic materials 0.000 claims description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims description 2
- 239000011964 heteropoly acid Substances 0.000 claims description 2
- 150000003457 sulfones Chemical class 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims 1
- IAQRGUVFOMOMEM-ONEGZZNKSA-N trans-but-2-ene Chemical group C\C=C\C IAQRGUVFOMOMEM-ONEGZZNKSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 12
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- WWGWOVMJTUUNSA-UHFFFAOYSA-N (4-formyloxyphenyl) formate Chemical compound O=COC1=CC=C(OC=O)C=C1 WWGWOVMJTUUNSA-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- C01F7/78—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- 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
- C01F7/78—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/006—Compounds containing zinc, with or without oxygen or hydrogen, and containing two or more other elements
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明公开了属于无机功能材料工业化技术领域的一种生产高分散水滑石粉体的工艺和成套工业装置。所述的装置包括浆料储罐、滤芯式抽滤机、分散剂精馏系统、洗涤水再生系统、连续盘式干燥器;将水滑石浆料由浆料储罐进入滤芯式抽滤机进行抽滤,得到水滑石滤饼,产生的废水通过洗涤水再生系统得到净化后可再利用;然后直接加入有机分散剂与水滑石滤饼混合,在机械搅拌和/或压缩空气鼓泡条件下对水滑石进行改性,改性结束后用真空泵抽滤,将滤饼转移至连续盘式干燥器中进行干燥;整个工艺流程中使用过的有机分散剂经精馏系统回收再利用,避免了有机分散剂对环境造成污染,降低成本,简化生产流程,获得分散性好、高比表面积的水滑石产品,实现了大规模生产。
The invention discloses a process and a complete set of industrial equipment for producing highly dispersed hydrotalcite powder, which belong to the technical field of industrialization of inorganic functional materials. The device includes a slurry storage tank, a filter element type suction filter, a dispersant rectification system, a washing water regeneration system, and a continuous disc dryer; the hydrotalcite slurry enters the filter element type suction filter from the slurry storage tank for Suction filtration to obtain hydrotalcite filter cake, and the waste water produced can be reused after being purified through the washing water regeneration system; then directly add organic dispersant and mix with hydrotalcite filter cake, under the condition of mechanical stirring and/or compressed air bubbling The hydrotalcite is modified, and after the modification is completed, it is filtered with a vacuum pump, and the filter cake is transferred to a continuous disc dryer for drying; the organic dispersant used in the entire process is recycled and reused by the rectification system, avoiding the organic The dispersant pollutes the environment, reduces costs, simplifies the production process, obtains hydrotalcite products with good dispersibility and high specific surface area, and realizes large-scale production.
Description
技术领域:Technical field:
本发明属于无机功能材料工业化技术领域,特别涉及一种生产高分散水滑石粉体的工艺和成套工业装置。The invention belongs to the technical field of industrialization of inorganic functional materials, and in particular relates to a process and a complete set of industrial equipment for producing highly dispersed hydrotalcite powder.
背景技术:Background technique:
层状复合金属氢氧化物(Layered Double Hydroxides,简称LDHs),又叫水滑石,是一种典型的阴离子型层状材料,其化学组成式为[M2+ 1-xM3+ x(OH)2]An- x/n·mH2O,其中M2+、M3+分别为二价及三价金属阳离子,An-是层间阴离子,x为M3+离子的摩尔分数,m为结晶水的数量。水滑石主体层板的金属元素种类及组成比例、层间客体的种类及数量和水分子的个数可以根据应用需要在较宽范围内调变,极大的丰富了其功能性,目前已被广泛的应用于紫外阻隔、红外吸收、PVC热稳定剂、新型光电材料、电化学储能等领域。Layered Double Hydroxides (LDHs for short), also known as hydrotalcite, is a typical anionic layered material, and its chemical composition formula is [M 2+ 1-x M 3+ x (OH ) 2 ]A n- x/n mH 2 O, where M 2+ and M 3+ are divalent and trivalent metal cations respectively, A n- is an interlayer anion, x is the mole fraction of M 3+ ions, m is the amount of water of crystallization. The type and composition ratio of metal elements in the main layer of hydrotalcite, the type and quantity of interlayer objects, and the number of water molecules can be adjusted in a wide range according to the application requirements, which greatly enriches its functionality. It is widely used in ultraviolet blocking, infrared absorption, PVC heat stabilizer, new photoelectric materials, electrochemical energy storage and other fields.
工业上大规模制备水滑石的传统方法为共沉淀法和成核-晶化隔离法,当水滑石的合成反应结束后,直接用纯水洗涤浆料并干燥后得到水滑石粉末产物。干燥过程中由于水滑石自身的高表面能和纯水蒸发过程中的表面张力作用,导致最终的产品团聚较严重,粒径分布不均匀,且表面积很低(约1-50m2/g),极大的限制了水滑石的应用范围。只有解决了水滑石的团聚问题,其特殊的纳米效应才会在应用中得到很好的体现,最终使其力学、光学、热学等方面的性能得到显著提升。The traditional methods for large-scale preparation of hydrotalcite in industry are co-precipitation method and nucleation-crystallization isolation method. After the synthesis reaction of hydrotalcite is completed, the slurry is directly washed with pure water and dried to obtain hydrotalcite powder product. Due to the high surface energy of hydrotalcite itself and the surface tension during the evaporation of pure water during the drying process, the final product has serious agglomeration, uneven particle size distribution, and a very low surface area (about 1-50m 2 /g). This greatly limits the scope of application of hydrotalcite. Only when the agglomeration problem of hydrotalcite is solved, its special nano-effects will be well reflected in the application, and finally its mechanical, optical, thermal and other performances will be significantly improved.
虽然在实验室制备高分散水滑石已经取得了一定进展,但若想工业化大规模生产,仍然有若干问题需要解决:①在放大过程中,当采用的改性釜体积放大至m3尺寸时,由于放大效应会导致釜内体系不均一,改性不够彻底,影响产品品质,导致其性能显著下降;②实验室改性需要用大量的有机分散剂(如得到1g水滑石需要用1L丙酮改性),且回收困难,制备成本较高;③实验室将改性后的滤饼放入托盘在鼓风干燥机中干燥,无法对挥发的分散剂进行回收利用,导致了资源浪费和VOCs污染;④实验室水洗时先利用真空泵在布氏漏斗里抽滤,然后将滤饼转移至烧瓶里,再用有机分散剂改性,最后仍然在布氏漏斗里抽滤得到滤饼,此过程较繁琐,不利于大规模连续生产。Although some progress has been made in the preparation of highly dispersed hydrotalcite in the laboratory, there are still some problems to be solved in order to industrialize large-scale production: ① During the scale-up process, when the volume of the modified kettle used is enlarged to the size of m3 , Due to the amplification effect, the system in the kettle will be inhomogeneous, and the modification is not thorough enough, which will affect the product quality and lead to a significant decline in its performance; ② laboratory modification requires a large amount of organic dispersant (such as obtaining 1g of hydrotalcite needs to be modified with 1L of acetone ), and the recovery is difficult, and the preparation cost is high; ③ the laboratory puts the modified filter cake into a tray and dries it in a blast dryer, which cannot recycle the volatilized dispersant, resulting in waste of resources and VOCs pollution; ④ When washing with water in the laboratory, first use a vacuum pump to filter in a Buchner funnel, then transfer the filter cake to a flask, then modify it with an organic dispersant, and finally filter it in a Buchner funnel to obtain a filter cake. This process is cumbersome , not conducive to large-scale continuous production.
发明内容:Invention content:
为克服大反应釜改性过程中的放大效应,将有机分散剂在使用后回收利用并避免环境污染,简化生产流程,获得分散性好、高比表面积的水滑石产品,实现大规模生产,本发明提供了一种生产高分散水滑石粉体的工艺和成套工业装置,如图1所示。In order to overcome the amplification effect in the modification process of large reactors, recycle the organic dispersant after use and avoid environmental pollution, simplify the production process, obtain hydrotalcite products with good dispersion and high specific surface area, and realize large-scale production. The invention provides a process and a complete set of industrial equipment for producing highly dispersed hydrotalcite powder, as shown in Figure 1.
本发明所述的生产高分散水滑石粉体的成套工业装置,该装置包括浆料储罐、滤芯式抽滤机、分散剂精馏系统、洗涤水再生系统、连续盘式干燥器;将水滑石浆料由浆料储罐进入滤芯式抽滤机进行抽滤,得到水滑石滤饼,产生的废水通过洗涤水再生系统得到净化后可再利用;然后直接加入有机分散剂与水滑石滤饼混合,在机械搅拌和/或压缩空气鼓泡条件下对水滑石进行改性,改性结束后抽滤,将改性后的滤饼转移至连续盘式干燥器进行干燥;整个工艺流程中使用过的有机分散剂经分散剂精馏系统回收再用。The complete industrial device for producing highly dispersed hydrotalcite powder according to the present invention, the device includes a slurry storage tank, a filter element type suction filter, a dispersant rectification system, a washing water regeneration system, and a continuous disc dryer; The talc slurry enters the filter element suction filter from the slurry storage tank for suction filtration to obtain a hydrotalcite filter cake, and the generated wastewater can be reused after being purified through the washing water regeneration system; then directly add organic dispersant and hydrotalcite filter cake Mixing, modifying the hydrotalcite under the conditions of mechanical stirring and/or compressed air bubbling, suction filtration after the modification, and transferring the modified filter cake to a continuous disc dryer for drying; used in the whole process The spent organic dispersant is recovered and reused through the dispersant rectification system.
所述的滤芯式抽滤机,其滤芯采用多孔材料制成,孔径为纳米级至微米级,孔道呈交叉分布无规则状态;抽滤时,水或有机分散剂经孔道渗出,水滑石被截留下来形成滤饼。The filter-type suction filter, the filter element is made of porous material, the pore diameter is from nanometer to micron, and the channels are in a cross distribution irregular state; during suction filtration, water or organic dispersant seeps out through the channels, and the hydrotalcite is retained to form a filter cake.
所述的连续盘式干燥器由大小干燥盘上下交替排列,每个干燥盘上带有耙叶,耙叶由耙臂控制做回转运动使耙叶连续地翻抄物料;在大干燥盘上物料向中心移动并从中心落料口落入下一层小干燥盘中,接收到物料后小干燥盘向外移动到正下方的大干燥盘外缘处,同时在小干燥盘上的物料也向外移动,并从外缘落到正下方的大干燥盘外缘;改性后的滤饼加到干燥器上部第一层干燥盘上,然后沿指数螺旋线连续流过每层干燥盘表面。The continuous disc dryer is composed of large and small drying discs arranged alternately up and down, and each drying disc has rake leaves, which are controlled by the rake arm to make a rotary motion so that the rake leaves can continuously turn over the materials; on the large drying discs, the materials Move to the center and fall into the small drying tray on the next layer from the central discharge port. After receiving the material, the small drying tray moves outward to the outer edge of the large drying tray directly below, and at the same time, the material on the small drying tray also It moves outside and falls from the outer edge to the outer edge of the large drying plate directly below; the modified filter cake is added to the first layer of drying plate in the upper part of the dryer, and then flows continuously along the exponential spiral line through the surface of each layer of drying plate.
所述的分散剂精馏系统将改性过程中使用的和干燥过程中产生的有机分散剂回收精制后进入分散剂储罐,供下一批水滑石改性使用;所述的分散剂精馏系统包括再沸器、分散剂精馏塔、换热器、冷凝器,对有机分散剂进行分离、再沸、精馏、冷凝,将含有的水及杂质除去。The dispersant rectification system recovers and refines the organic dispersant used in the modification process and the organic dispersant produced in the drying process, and enters the dispersant storage tank for the next batch of hydrotalcite modification; the dispersant rectification The system includes reboiler, dispersant rectification tower, heat exchanger and condenser, which can separate, reboil, rectify and condense organic dispersant, and remove the contained water and impurities.
所述的洗涤水再生系统,首先对抽滤后产生的废水利用酸碱中和原理进行中和,维持pH值在6.0-8.0之间,然后利用反渗透膜将水中的金属离子除掉,得到净化的水进入储水罐。In the washing water regeneration system, firstly, the waste water generated after suction filtration is neutralized using the principle of acid-base neutralization, and the pH value is maintained between 6.0-8.0, and then the metal ions in the water are removed by using the reverse osmosis membrane to obtain The purified water goes into the storage tank.
将上述成套工业装置用于高分散水滑石粉体的工业化生产工艺,其具体步骤为:The above-mentioned complete set of industrial equipment is used in the industrial production process of highly dispersed hydrotalcite powder, and its specific steps are:
A.将固含量为1-15wt%的水滑石浆料50-2000L加入滤芯式抽滤机,滤芯孔径为0.1-300μm,设置抽滤压差为0.01-0.5MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用;A. Add 50-2000L of hydrotalcite slurry with a solid content of 1-15wt% into a filter element suction filter, the filter element pore size is 0.1-300μm, set the suction filtration pressure difference to 0.01-0.5MPa, and use a vacuum pump to pump out the water. The talc filter cake is left in the filter element suction filter; the extracted water enters the washing water buffer tank, and is purified and reused through the washing water regeneration system;
B.20-150℃条件下,向滤芯式抽滤机里加入50-2000L有机分散剂,在机械搅拌和/或压缩空气鼓泡条件下对水滑石进行改性,设置搅拌转速为50-3000rpm,压缩空气鼓泡速率为0.1-1000mL/min;改性1-72小时后进行抽滤,设置抽滤压差为0.01-0.5MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为30-200℃,干燥1-48小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的有机分散剂通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用。B. Under the condition of 20-150℃, add 50-2000L organic dispersant to the filter-type suction filter, modify the hydrotalcite under the condition of mechanical stirring and/or compressed air bubbling, and set the stirring speed at 50-3000rpm , the compressed air bubbling rate is 0.1-1000mL/min; after modification for 1-72 hours, carry out suction filtration, set the pressure difference of suction filtration to 0.01-0.5MPa, transfer the obtained filter cake to a continuous disc dryer for drying, set The temperature of the disc dryer is 30-200°C, and the highly dispersed hydrotalcite powder is obtained after drying for 1-48 hours; the organic dispersant used in the modification process and produced in the drying process is recovered and refined through the dispersant rectification system Enter the dispersant storage tank for the next batch of hydrotalcite modification.
所述的水滑石的化学组成为[M2+ 1-xM3+ x(OH)2]An- x/n·mH2O;其中M2+代表二价金属阳离子Mg2+、Zn2+、Ca2+、Cu2+、Ni2+、Co2+、Fe2+、Mn2+、Cd2+、Be2+中的一种或两种,优选Mg2+、Zn2+、Ca2+、Ni2+中的一种或两种;M3+代表三价金属阳离子Al3+、Co3+、Fe3+、Mn3+、Cr3+、V3+、Ti3+、In3+、Ga3+中的一种或两种,优选Al3+、Fe3+中的一种或两种;酸根阴离子An-选自下述酸根阴离子中的一种或几种:(1)无机酸阴离子:CO3 2-、NO3 -、[B4O5(OH)4]2–、F-、Cl-、Br-、I-、ClO4 -、IO3 -、H2PO4 -、HPO4 2-、PO4 3-、SO4 2-、S2O3 2-、WO4 2-、CrO4 2-;(2)有机酸阴离子:对苯二甲酸根、对羟基苯甲酸根、丁二酸根、己二酸根、十二烷基磺酸根、苯甲酸根;(3)同多、杂多酸阴离子:Mo7O24 6-、V10O28 6-、PW11CuO39 6-、SiW9W3O40 7-;An-优选NO3 -、CO3 2-、[B4O5(OH)4]2–、SO4 2-、PO4 3-、丁二酸根、苯甲酸根中的一种;n为酸根阴离子的化合价数,n=1-7。The chemical composition of the hydrotalcite is [M 2+ 1-x M 3+ x (OH) 2 ]A n- x/n ·mH 2 O; wherein M 2+ represents divalent metal cations Mg 2+ , Zn One or two of 2+ , Ca 2+ , Cu 2+ , Ni 2+ , Co 2+ , Fe 2+ , Mn 2+ , Cd 2+ , Be 2+ , preferably Mg 2+ , Zn 2+ , Ca 2+ , Ni 2+ or both; M 3+ represents trivalent metal cations Al 3+ , Co 3+ , Fe 3+ , Mn 3+ , Cr 3+ , V 3+ , Ti 3 One or two of + , In 3+ , Ga 3+ , preferably one or both of Al 3+ , Fe 3+ ; the acid anion An- is selected from one or more of the following acid anions Species: (1) Inorganic acid anions: CO 3 2- , NO 3 - , [B 4 O 5 (OH) 4 ] 2– , F - , Cl - , Br - , I - , ClO 4 - , IO 3 - , H 2 PO 4 - , HPO 4 2- , PO 4 3- , SO 4 2- , S 2 O 3 2- , WO 4 2- , C r O 4 2- ; (2) Organic acid anion: p-phenylene Diformate, p-hydroxybenzoate, succinate, adipate, dodecylsulfonate, benzoate; (3) Isopoly and heteropoly acid anions: Mo 7 O 24 6- , V 10 O 28 6- , PW 11 CuO 39 6- , SiW 9 W 3 O 40 7- ; An- preferably NO 3 - , CO 3 2- , [B 4 O 5 (OH) 4 ] 2– , SO 4 2- , PO 4 3- , succinate, benzoate; n is the valency of the acid anion, n=1-7.
所述的水滑石粒径为30nm-5μm。The particle size of the hydrotalcite is 30nm-5μm.
所述的有机分散剂为丙酮、甲醇、乙醇、正丙醇、异丙醇、四氢呋喃、乙腈、二氧己烷、二甲亚砜、N-N二甲基甲酰胺中的一种或几种,优选丙酮、甲醇、乙醇、正丙醇、异丙醇中的一种或两种。The organic dispersant is one or more of acetone, methanol, ethanol, n-propanol, isopropanol, tetrahydrofuran, acetonitrile, dioxane, dimethyl sulfoxide, N-N dimethylformamide, preferably One or both of acetone, methanol, ethanol, n-propanol, and isopropanol.
本发明根据界面化学原理,针对水滑石的化学键类型和表面的物理化学性质,利用有机溶剂对水滑石表面或层间进行改性,设计了一种生产高分散水滑石粉体的工艺和成套工业装置。通过有机分散剂改性,可以提高水滑石的分散性,抑制粒子之间的团聚,从而使产品比表面积提高10倍以上。水滑石浆料抽去水分形成滤饼后,直接在滤芯式抽滤机中加入有机分散剂进行改性,即滤芯式抽滤机既作为抽滤装置,又作为改性装置,简化了生产流程,有利于大规模生产;此外,利用精馏和冷凝系统还可以将有机分散剂高效回收循环利用,避免了环境污染,并且显著降低了生产成本。According to the principle of interface chemistry, the present invention aims at the chemical bond type of hydrotalcite and the physical and chemical properties of the surface, and uses organic solvents to modify the surface or interlayer of hydrotalcite, and designs a process and complete set of industries for producing highly dispersed hydrotalcite powder device. By modifying the organic dispersant, the dispersibility of hydrotalcite can be improved, and the agglomeration between particles can be suppressed, so that the specific surface area of the product can be increased by more than 10 times. After the hydrotalcite slurry is dehydrated to form a filter cake, the organic dispersant is directly added to the filter element suction filter for modification, that is, the filter element suction filter is used as both a suction filtration device and a modification device, which simplifies the production process , which is conducive to large-scale production; in addition, the use of rectification and condensation systems can also efficiently recycle the organic dispersant, avoiding environmental pollution, and significantly reducing production costs.
附图说明Description of drawings
图1本发明设计的生产高分散水滑石粉体的工艺流程图;The process flow diagram of the production of highly dispersed hydrotalcite powder of Fig. 1 the present invention design;
图2是实施例1所得水滑石粉体的XRD谱图;Fig. 2 is the XRD spectrogram of embodiment 1 gained hydrotalcite powder;
图3是实施例1所得水滑石粉体的红外谱图;Fig. 3 is the infrared spectrogram of embodiment 1 gained hydrotalcite powder;
图4是实施例1所得水滑石粉体的激光粒度分布图;Fig. 4 is the laser particle size distribution figure of embodiment 1 gained hydrotalcite powder;
图5是实施例1所得水滑石粉体的TEM谱图;Fig. 5 is the TEM spectrogram of embodiment 1 gained hydrotalcite powder;
图6是实施例1所得水滑石粉体的等温吸附曲线和孔分布图。Fig. 6 is the isothermal adsorption curve and pore distribution diagram of the hydrotalcite powder obtained in Example 1.
具体实施方式Detailed ways
实施例1:Example 1:
生产高分散水滑石粉体的成套工业装置:该装置包括浆料储罐、滤芯式抽滤机、分散剂精馏系统、洗涤水再生系统、连续盘式干燥器;将水滑石浆料由浆料储罐进入滤芯式抽滤机进行抽滤,得到水滑石滤饼,产生的废水通过洗涤水再生系统得到净化再利用;然后直接加入有机分散剂与水滑石滤饼混合,在机械搅拌和/或压缩空气鼓泡条件下对水滑石进行改性,改性结束后抽滤,将改性后的滤饼转移至连续盘式干燥器进行干燥;整个工艺流程中使用过的有机分散剂经分散剂精馏系统回收再用。A complete set of industrial equipment for producing highly dispersed hydrotalcite powder: the equipment includes a slurry storage tank, a filter element suction filter, a dispersant rectification system, a washing water regeneration system, and a continuous disc dryer; The material storage tank enters the filter element suction filter for suction filtration to obtain a hydrotalcite filter cake, and the waste water generated is purified and reused through the washing water regeneration system; then directly add an organic dispersant to mix with the hydrotalcite filter cake, and mix it with mechanical stirring and/or Or modify the hydrotalcite under the condition of compressed air bubbling, suction filter after the modification, transfer the modified filter cake to a continuous disc dryer for drying; the organic dispersant used in the whole process is dispersed The solvent rectification system recycles and reuses.
所述的滤芯式抽滤机,其滤芯采用多孔材料制成,孔径为纳米级至微米级,孔道呈交叉分布无规则状态;抽滤时,水或有机分散剂经孔道渗出,水滑石被截留下来形成水滑石滤饼。The filter-type suction filter, the filter element is made of porous material, the pore diameter is from nanometer to micron, and the channels are in a cross distribution irregular state; during suction filtration, water or organic dispersant seeps out through the channels, and the hydrotalcite is Trapped to form a hydrotalcite filter cake.
所述的连续盘式干燥器由大小干燥盘上下交替排列,每个干燥盘上带有耙叶,耙叶由耙臂控制做回转运动使耙叶连续地翻抄物料;在大干燥盘上物料向中心移动并从中心落料口落入下一层小干燥盘中,接收到物料后小干燥盘向外移动到正下方的大干燥盘外缘处,同时在小干燥盘上的物料也向外移动,并从外缘落到正下方的大干燥盘外缘;改性后的滤饼加到干燥器上部第一层干燥盘上,然后沿指数螺旋线连续流过每层干燥盘表面。The continuous disc dryer is composed of large and small drying discs arranged alternately up and down, and each drying disc has rake leaves, which are controlled by the rake arm to make a rotary motion so that the rake leaves can continuously turn over the materials; on the large drying discs, the materials Move to the center and fall into the small drying tray on the next layer from the central discharge port. After receiving the material, the small drying tray moves outward to the outer edge of the large drying tray directly below, and at the same time, the material on the small drying tray also It moves outside and falls from the outer edge to the outer edge of the large drying plate directly below; the modified filter cake is added to the first layer of drying plate in the upper part of the dryer, and then flows continuously along the exponential spiral line through the surface of each layer of drying plate.
所述的分散剂精馏系统将改性过程中使用的和干燥过程中产生的有机分散剂回收精制后进入分散剂储罐,供下一批水滑石改性使用;所述的分散剂精馏系统包括再沸器、分散剂精馏塔、换热器、冷凝器,对有机分散剂进行分离、再沸、精馏、冷凝,将含有的水及杂质除去。The dispersant rectification system recovers and refines the organic dispersant used in the modification process and the organic dispersant produced in the drying process, and enters the dispersant storage tank for the next batch of hydrotalcite modification; the dispersant rectification The system includes reboiler, dispersant rectification tower, heat exchanger and condenser, which can separate, reboil, rectify and condense organic dispersant, and remove the contained water and impurities.
所述的洗涤水再生系统,首先对抽滤后产生的废水利用酸碱中和原理进行中和,维持pH值在6.0-8.0之间,然后利用反渗透膜将水中的金属离子除掉,得到净化的水进入储水罐。In the washing water regeneration system, firstly, the waste water generated after suction filtration is neutralized using the principle of acid-base neutralization, and the pH value is maintained between 6.0-8.0, and then the metal ions in the water are removed by using the reverse osmosis membrane to obtain The purified water goes into the storage tank.
使用上述的成套工业装置用于高分散水滑石粉体的工业化生产:Use the above-mentioned complete set of industrial equipment for the industrial production of highly dispersed hydrotalcite powder:
A.将固含量为6wt%、平均粒径为145.4nm、化学式为Mg6Al2(OH)16CO3·4H2O的水滑石浆料100L加入滤芯式抽滤机,滤芯孔径为0.1μm,设置抽滤压差为0.1MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 100L of hydrotalcite slurry with a solid content of 6wt%, an average particle size of 145.4nm, and a chemical formula of Mg 6 Al 2 (OH) 16 CO 3 4H 2 O into a filter-type suction filter with a pore size of 0.1 μm , set the suction filtration pressure difference to 0.1MPa, pump out the water with a vacuum pump, and leave the hydrotalcite filter cake in the filter element suction filter; the pumped out water enters the washing water buffer tank, and is purified and reused through the washing water regeneration system. and to pH=7;
B.25℃条件下,向滤芯式抽滤机里加入600L丙酮,在机械搅拌条件下对水滑石进行改性,搅拌转速为500rpm,改性48小时后进行抽滤,设置抽滤压差为0.1MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为40℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的丙酮通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,丙酮的纯度可以达到98%以上。B. Under the condition of 25°C, add 600L acetone to the cartridge type suction filter, modify the hydrotalcite under the condition of mechanical stirring, the stirring speed is 500rpm, carry out suction filtration after modification for 48 hours, set the pressure difference of suction filtration as 0.1MPa, the obtained filter cake was transferred to a continuous disc dryer for drying, and the temperature of the disc dryer was set to 40°C. After drying for 12 hours, a highly dispersed hydrotalcite powder was obtained; The produced acetone is recovered and refined by the dispersant rectification system and enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed, and the purity of the acetone can reach more than 98%.
采用日本岛津公司的XRD-6000型X-射线粉末衍射仪对产品进行晶体结构表征。图2为实施例1所得水滑石粉体的XRD谱图,从图中可以看出,在2θ=11.3°、22.7°、34.5°、60.5°和61.8°左右处出现了Mg6Al2-CO3-LDHs的特征衍射峰,且峰形尖耸,基线低平,说明产品晶体结构完整。The XRD-6000 X-ray powder diffractometer of Shimadzu Corporation was used to characterize the crystal structure of the product. Figure 2 is the XRD spectrum of the hydrotalcite powder obtained in Example 1. It can be seen from the figure that Mg 6 Al 2 -CO The characteristic diffraction peaks of 3 -LDHs are sharp and sharp, and the baseline is low and flat, indicating that the crystal structure of the product is complete.
采用德国布鲁克公司的Vector22型红外光谱仪测量样品的红外吸收光谱。图3为实施例1所得水滑石粉体的红外光谱,从图中可以看出,3486cm-1出现了层板OH的伸缩振动吸收峰,1640cm-1出现了层板OH的弯曲振动吸收峰,1570cm-1为层间CO3 2-的伸缩振动吸收峰,655cm-1为层间CO3 2-的弯曲振动吸收峰,红外光谱进一步说明产品晶体结构完整。The infrared absorption spectrum of the samples was measured by a Vector22 infrared spectrometer from Bruker, Germany. Figure 3 is the infrared spectrum of the hydrotalcite powder obtained in Example 1. It can be seen from the figure that the stretching vibration absorption peak of the laminate OH appeared at 3486cm -1 , and the bending vibration absorption peak of the laminate OH appeared at 1640cm -1 . 1570cm -1 is the stretching vibration absorption peak of interlayer CO 3 2- , and 655cm -1 is the bending vibration absorption peak of interlayer CO 3 2- . The infrared spectrum further proves that the crystal structure of the product is complete.
采用英国马尔文公司的Mastersizer2000型激光粒度仪测量样品的粒径大小。图4是实施例1所得水滑石粉体的激光粒度分布图,从图中可以看出,产物的平均粒径为145.4nm,粒径分布较均匀;无大粒径的峰出现,表明产物分散性很好,无明显团聚现象。The particle size of the samples was measured using a Mastersizer 2000 laser particle size analyzer from Malvern, UK. Figure 4 is the laser particle size distribution diagram of the hydrotalcite powder obtained in Example 1. It can be seen from the figure that the average particle size of the product is 145.4nm, and the particle size distribution is relatively uniform; no peaks with large particle sizes appear, indicating that the product is dispersed Sex is very good, no obvious reunion phenomenon.
采用日本电子仪器公司(JEOL)JEM2010型透射电镜观察晶粒尺寸和形貌。图5是实施例1所得水滑石粉体的TEM谱图,从图中可以看出水滑石颗粒为单分散,无团聚现象,粒径为50-210nm,平均粒径约为145nm。The grain size and morphology were observed by JEM2010 transmission electron microscope (JEOL). Fig. 5 is the TEM spectrogram of the hydrotalcite powder obtained in Example 1. It can be seen from the figure that the hydrotalcite particles are monodisperse, without agglomeration, with a particle size of 50-210 nm and an average particle size of about 145 nm.
采用美国Quantachrome公司Autosorb-1C-VP型分析仪测试样品的吸附等温曲线和孔径分布。图6是实施例1所得水滑石粉体的吸附等温曲线和孔分布图,从图中可以看出产品孔径分布在5-20nm之间。根据吸附等温线得出产品的比表面积为148m2/g。The adsorption isotherm curve and pore size distribution of the samples were tested by Autosorb-1C-VP analyzer from Quantachrome Company, USA. Fig. 6 is the adsorption isotherm curve and pore distribution diagram of the hydrotalcite powder obtained in Example 1. It can be seen from the figure that the pore size distribution of the product is between 5-20 nm. According to the adsorption isotherm, the specific surface area of the product is 148m 2 /g.
实施例2:Example 2:
使用实施例1设计的成套工业装置用于高分散水滑石粉体的工业化生产:The complete set of industrial equipment designed using embodiment 1 is used for the industrialized production of highly dispersed hydrotalcite powder:
A.将固含量为1wt%、平均粒径为5μm、化学式为Mg6Al2(OH)16(NO3)2·4H2O,采用成核-晶化法制得的水滑石浆料100L加入滤芯式抽滤机,滤芯孔径为300μm,设置抽滤压差为0.1MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 100L of hydrotalcite slurry with a solid content of 1wt%, an average particle size of 5μm, and a chemical formula of Mg 6 Al 2 (OH) 16 (NO 3 ) 2 ·4H 2 O, prepared by nucleation-crystallization method Cartridge-type suction filter, the pore size of the filter element is 300μm, and the suction filtration pressure difference is set to 0.1MPa. The water is pumped out with a vacuum pump, and the hydrotalcite filter cake is left in the filter-cartridge suction filter; the extracted water enters the washing water buffer tank and passes through the washing The water regeneration system is used for purification and reuse, and is set to neutralize to pH=7;
B.25℃条件下,向滤芯式抽滤机里加入600L异丙醇,在机械搅拌条件下对水滑石进行改性,搅拌转速为500rpm,改性24小时后进行抽滤,设置抽滤压差为0.1MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为40℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的异丙醇通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,异丙醇的纯度可以达到98%以上。B. Under the condition of 25°C, add 600L isopropanol to the cartridge type suction filter, modify the hydrotalcite under the condition of mechanical stirring, the stirring speed is 500rpm, carry out suction filtration after modification for 24 hours, set the suction pressure The difference is 0.1MPa, and the obtained filter cake is transferred to a continuous disc dryer for drying, and the temperature of the disc dryer is set to 40°C. After drying for 12 hours, a highly dispersed hydrotalcite powder is obtained; The isopropanol produced in the process is recovered and refined by the dispersant rectification system and enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed. The purity of isopropanol It can reach more than 98%.
实施例3:Embodiment 3:
使用实施例1设计的成套工业装置用于高分散水滑石粉体的工业化生产:The complete set of industrial equipment designed using embodiment 1 is used for the industrialized production of highly dispersed hydrotalcite powder:
A.将固含量为10wt%、平均粒径为50nm、化学式为Zn4Al2(OH)12CO3·4H2O,采用成核-晶化法制得的水滑石浆料400L加入滤芯式抽滤机,滤芯孔径为10μm,设置抽滤压差为0.1MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 400L of hydrotalcite slurry with a solid content of 10wt%, an average particle size of 50nm, and a chemical formula of Zn 4 Al 2 (OH) 12 CO 3 4H 2 O, prepared by nucleation-crystallization method into the filter element pump Filter, filter element pore size is 10μm, set suction filtration pressure difference to 0.1MPa, use vacuum pump to pump out water, hydrotalcite filter cake stays in the filter element suction filter; pumped water enters the washing water buffer tank, and passes through the washing water regeneration system Perform purification and reuse, set neutralization to pH=7;
B.25℃条件下,向滤芯式抽滤机里加入600L二甲亚砜,在机械搅拌条件下对水滑石进行改性,搅拌转速为1000rpm,改性48小时后进行抽滤,设置抽滤压差为0.1MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为80℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的二甲亚砜通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,二甲亚砜的纯度可以达到98%以上。B. Under the condition of 25°C, add 600L dimethyl sulfoxide to the filter element suction filter, modify the hydrotalcite under the condition of mechanical stirring, the stirring speed is 1000rpm, perform suction filtration after 48 hours of modification, and set the suction filtration The pressure difference is 0.1MPa, and the obtained filter cake is transferred to a continuous disc dryer for drying, and the temperature of the disc dryer is set at 80° C. After drying for 12 hours, a highly dispersed hydrotalcite powder is obtained; The dimethyl sulfoxide produced in the drying process is recovered and refined by the dispersant rectification system and then enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed, and the dimethyl sulfoxide The purity of sulfone can reach more than 98%.
实施例4:Example 4:
使用实施例1设计的成套工业装置用于高分散水滑石粉体的工业化生产:The complete set of industrial equipment designed using embodiment 1 is used for the industrialized production of highly dispersed hydrotalcite powder:
A.将固含量为15wt%、平均粒径为520nm、化学式为Zn4Al2(OH)12(NO3)2·4H2O,采用成核-晶化法制得的水滑石浆料800L加入滤芯式抽滤机,滤芯孔径为100μm,设置抽滤压差为0.1MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 800L of hydrotalcite slurry with a solid content of 15wt%, an average particle size of 520nm, and a chemical formula of Zn 4 Al 2 (OH) 12 (NO 3 ) 2 ·4H 2 O, prepared by nucleation-crystallization method Cartridge-type suction filter, the pore size of the filter element is 100μm, and the filter pressure difference is set to 0.1MPa. The water is pumped out with a vacuum pump, and the hydrotalcite filter cake is left in the filter-cartridge suction filter; the extracted water enters the washing water buffer tank and passes through the washing The water regeneration system is used for purification and reuse, and is set to neutralize to pH=7;
B.25℃条件下,向滤芯式抽滤机里加入1200L有机分散剂,在压缩空气鼓泡速率为800mL/min条件下对水滑石进行改性,改性48小时后进行抽滤,设置抽滤压差为0.1MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为40℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的有机分散剂通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,有机分散剂的纯度可以达到98%以上。所用的有机分散剂为600L丙酮和600L甲醇。B. Under the condition of 25°C, add 1200L organic dispersant to the cartridge type suction filter, modify the hydrotalcite under the condition that the compressed air bubbling rate is 800mL/min, carry out suction filtration after 48 hours of modification, set the suction The filter pressure difference is 0.1MPa, and the obtained filter cake is transferred to a continuous disc dryer for drying, and the temperature of the disc dryer is set at 40°C. After drying for 12 hours, a highly dispersed hydrotalcite powder is obtained; And the organic dispersant produced in the drying process is recovered and refined by the dispersant rectification system and enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed. The organic dispersant The purity can reach more than 98%. The organic dispersants used were 600L acetone and 600L methanol.
实施例5:Example 5:
使用实施例1设计的成套工业装置用于高分散水滑石粉体的工业化生产:The complete set of industrial equipment designed using embodiment 1 is used for the industrialized production of highly dispersed hydrotalcite powder:
A.将固含量为15wt%、平均粒径为810nm、化学式为Mg4Al2(OH)12CO3·4H2O,采用成核-晶化法制得的水滑石浆料1800L加入滤芯式抽滤机,滤芯孔径为210μm,设置抽滤压差为0.3MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 1800L of hydrotalcite slurry with a solid content of 15wt%, an average particle size of 810nm, and a chemical formula of Mg 4 Al 2 (OH) 12 CO 3 4H 2 O, prepared by nucleation-crystallization method into the filter element pump Filter, the filter core aperture is 210μm, set the suction filtration pressure difference to 0.3MPa, pump out the water with a vacuum pump, and the hydrotalcite filter cake remains in the filter core suction filter; the pumped water enters the washing water buffer tank and passes through the washing water regeneration system Perform purification and reuse, set neutralization to pH=7;
B.25℃条件下,向滤芯式抽滤机里加入2000L有机分散剂,在机械搅拌条件下对水滑石进行改性,搅拌转速为1000rpm,改性24小时后进行抽滤,设置抽滤压差为0.3MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为100℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的有机分散剂通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,有机分散剂的纯度可以达到98%以上。所用的有机分散剂为1000L丙酮和1000L四氢呋喃。B. Under the condition of 25°C, add 2000L organic dispersant to the cartridge-type suction filter, modify the hydrotalcite under the condition of mechanical stirring, the stirring speed is 1000rpm, carry out suction filtration after 24 hours of modification, set the suction pressure The difference is 0.3MPa, and the obtained filter cake is transferred to a continuous disc dryer for drying, and the temperature of the disc dryer is set to 100°C. After drying for 12 hours, a highly dispersed hydrotalcite powder is obtained; The organic dispersant produced in the process is recovered and refined by the dispersant rectification system and enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed. The purity of the organic dispersant It can reach more than 98%. The organic dispersants used were 1000L acetone and 1000L tetrahydrofuran.
实施例6:Embodiment 6:
使用实施例1设计的成套工业装置用于高分散水滑石粉体的工业化生产:The complete set of industrial equipment designed using embodiment 1 is used for the industrialized production of highly dispersed hydrotalcite powder:
A.将固含量为12wt%、平均粒径为2μm、化学式为Mg4Al2(OH)12(NO3)2·4H2O,采用成核-晶化法制得的水滑石浆料400L加入滤芯式抽滤机,滤芯孔径为250μm,设置抽滤压差为0.01MPa,用真空泵将水抽出,水滑石滤饼留在滤芯式抽滤机里;抽出的水进入洗涤水缓冲罐,通过洗涤水再生系统进行净化再利用,设置中和至pH=7;A. Add 400L of hydrotalcite slurry with a solid content of 12wt%, an average particle size of 2μm, and a chemical formula of Mg 4 Al 2 (OH) 12 (NO 3 ) 2 ·4H 2 O, prepared by nucleation-crystallization method Cartridge-type suction filter, the pore size of the filter element is 250μm, and the suction pressure difference is set to 0.01MPa. The water is pumped out with a vacuum pump, and the hydrotalcite filter cake is left in the filter-type suction filter; the extracted water enters the washing water buffer tank and passes through the washing The water regeneration system is used for purification and reuse, and is set to neutralize to pH=7;
B.100℃条件下,向滤芯式抽滤机里加入600L有机分散剂,在压缩空气鼓泡条件下对水滑石进行改性,压缩空气鼓泡速率为100mL/min,改性24小时后进行抽滤,设置抽滤压差为0.01MPa,得到的滤饼转移至连续盘式干燥器中干燥,设置盘式干燥器的温度为200℃,干燥12小时后得到高分散水滑石粉末;将改性过程中使用的和干燥过程中产生的有机分散剂通过分散剂精馏系统回收精制后进入分散剂储罐,供下一批水滑石改性使用,经过处理后99%以上的水分可被脱除,有机分散剂的纯度可以达到98%以上。所用的有机分散剂为200L丙酮,200L乙醇,200LN-N二甲基甲酰胺。B. Under the condition of 100°C, add 600L organic dispersant to the cartridge-type suction filter, and modify the hydrotalcite under the condition of compressed air bubbling. The compressed air bubbling rate is 100mL/min, and the modification is carried out after 24 hours. Suction filtration, set the pressure difference of suction filtration to 0.01MPa, transfer the obtained filter cake to a continuous disc dryer for drying, set the temperature of the disc dryer to 200°C, and obtain highly dispersed hydrotalcite powder after drying for 12 hours; The organic dispersant used in the curing process and produced in the drying process is recovered and refined by the dispersant rectification system and then enters the dispersant storage tank for the next batch of hydrotalcite modification. After treatment, more than 99% of the water can be removed In addition, the purity of the organic dispersant can reach more than 98%. The used organic dispersant is 200L acetone, 200L ethanol, 200LN-N dimethylformamide.
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