CN101670268A - Method for preparing siliceous porous material by asbestos tailings acid leaching residue - Google Patents
Method for preparing siliceous porous material by asbestos tailings acid leaching residue Download PDFInfo
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- CN101670268A CN101670268A CN200810222081A CN200810222081A CN101670268A CN 101670268 A CN101670268 A CN 101670268A CN 200810222081 A CN200810222081 A CN 200810222081A CN 200810222081 A CN200810222081 A CN 200810222081A CN 101670268 A CN101670268 A CN 101670268A
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- CN
- China
- Prior art keywords
- porous material
- acid leaching
- siliceous porous
- asbestos tailings
- leaching residue
- 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.)
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Links
- 239000010425 asbestos Substances 0.000 title claims abstract description 28
- 229910052895 riebeckite Inorganic materials 0.000 title claims abstract description 28
- 239000002253 acid Substances 0.000 title claims abstract description 25
- 239000011148 porous material Substances 0.000 title claims abstract description 25
- 238000002386 leaching Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- -1 Cu<2+> Chemical class 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910021426 porous silicon Inorganic materials 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- Silicon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method for preparing a siliceous porous material by asbestos tailings acid leaching residue, which comprises the following steps: washing, filtering and drying a solid residue after acid leaching and filtrating of the asbestos tailings and then calcining at 400-800 DEG C for 30-120 minutes to obtain the siliceous porous material. The siliceous porous material has the SiO2 content of larger than 86 percent, the specific surface area of larger than 300m2/g and developed pores inside particles, and the pore diameter distributing range is mainly concentrated to be 0.45-2nm. The material has wide raw material source, lower production cost, good adsorbing performance on heavy metal ions, such as Cu<2+>, Pb<2+>, Ni<2+>, Cd<2+>, Cr<3+>, and the like and can be used as anadsorbing material of wastewater and waste gas containing the heavy metal ions and the relevant field.
Description
1. technical field
The present invention relates to method, belong to comprehensive utilization of resources and field of environment protection with preparing siliceous porous material by asbestos tailings acid leaching residue.
2. background technology
Asbestos tailings comprise the country rock of asbestos deposit and associated mineral and after sorting discarded seven grades short cotton, the essential mineral composition is a serpentine.Main chemical compositions is SiO
2, MgO and constitution water.Whenever selecting at present one ton of 3~5 grades of qualified asbestos need also be that 1 ton of finished product cotton of every product will produce 25~27 tons of mine tailings with 26~28 tons in asbestos ore.China's about 400,000 tons of asbestos that manufacture a finished product every year, annual newly-increased mine tailing is more than 1,000 ten thousand tons.In decades, the asbestos tailings that pile up like a mountain has not only taken a large amount of soils and covered can adopt resource, and contained powder in the mine tailing, meets wind and flies all over the sky, forms serious environmental and pollutes.Therefore, press for it is fully utilized.In recent years, asbestos tailings some comprehensive utilizating research have been carried out both at home and abroad.Wherein patent of invention ZL 03157398.3 adopts MgO, the Al in the sulfuric acid dissolution leaching asbestos tailings
2O
3, Fe
2O
3After composition and Separation of Solid and Liquid, liquid is carried out iron removal by oxidation, produces super fine magnesium hydroxide, solid (acid leaching residue) with alkali dissolve with Separation of Solid and Liquid after, adopt the acid out method to produce superfine silicon dioxide; Patent of invention CN101161591A adopts MgO, the Al in the hydrochloric acid leaching asbestos tailings
2O
3, Fe
2O
3After composition and Separation of Solid and Liquid, liquid is carried out iron removal by oxidation, produces the nano-grade super fine magnesium hydroxide, solid (acid leaching residue) with alkali dissolve with Separation of Solid and Liquid after, produce the ball shaped nano white carbon.The filter residue (abbreviation acid leaching residue) of above-mentioned two patents of invention after to the asbestos tailings acidleach carries out that alkali is molten, separation, acid out, ageing process prepare superfine silicon dioxide or Nano carbon white.Studies show that the asbestos tailings acid leaching residue is with SiO
2Be the bigger a kind of powder body material of main component, pore volume and specific area.Though the aforementioned patent method utilizes the main chemical compositions of asbestos tailings acid leaching residue to prepare the superfine silicon dioxide or the nano-level sphere white carbon of high added value preferably, technology is complicated; Particularly directly do not utilize the bigger characteristic of acid leaching residue pore volume and specific area.
The present invention is directed to the present situation of present asbestos tailings comprehensive utilization technique, particularly the present situation of asbestos tailings acid leaching residue comprehensive utilization technique provides a kind of method of directly utilizing asbestos tailings acid leaching residue pore volume and the bigger characteristic of specific area to produce siliceous porous material.This method has not only been simplified the comprehensive utilization process of asbestos tailings acid leaching residue, directly utilized asbestos tailings acid leaching residue space prosperity, pore volume and the bigger characteristic of specific area, and the preparation method of the sorbing material that a kind of absorption property is better, raw material sources extensive, production cost is lower is provided for heavy metal ion-containing waste water processing, exhaust-gas treatment and other association areas.This porous silicon material has been widely used in fields such as energy-conservation, composite filler, concrete intensifiers.
3. summary of the invention
Calcine with the asbestos tailings acidleach and after solid slag (acid leaching residue) washing, filtration and the drying after filtering, promptly obtain siliceous porous material.
Its processing step is as follows:
(1) with asbestos tailings acid leaching residue clear water cyclic washing, filtration, to remove water-soluble salts substances residual in the acid leaching residue, as MgSO
4Or MgCl
2, Al2 (SO4)
3Or AlCl
3, FeSO
4Or FeCl
2Deng, in filtrate, there is not Cl
-Detect;
(2) acid leaching residue behind the washing and filtering is carried out drying;
(3) dried acid leaching residue is calcined.To remove organic matter and constitution water in the space and the capillary water in the acid leaching residue.
The described calcining of step (3), its process conditions are 400~800 ℃ of calcining heats; Calcination time 30~120min.
With the siliceous porous material of the present invention's preparation, its SiO
2Content>86%; Specific area>300m
2/ g; The prosperity of granule interior hole, pore size distribution range mainly concentrates on 0.45~2nm.Under proper condition, this material is to Cu
2+, Pb
2+, Ni
2+, Cd
2+, Cr
3+The adsorption rate of five heavy metal species ions reaches more than 95%, is a kind of good heavy metal ion adsorbed removal material.
4. description of drawings
Accompanying drawing 1 is the graph of pore diameter distribution of the porous silicon material of embodiment of the invention preparation; Fig. 2 is pattern (SEM) figure of the siliceous material of embodiment of the invention preparation; Fig. 3 is granule interior section (TEM) figure of the porous silicon material of embodiment of the invention preparation.
5. the specific embodiment
Embodiment one:
Get asbestos tailings hydrochloric acid and leach filter residue 200g, add clear water 600mL, agitator treating 10min filters; Repeat to add the water agitator treating and filter then, in filtrate, do not have Cl
-Detect (AgNO with 0.1%
3Solution trial does not have precipitation); Filter cake dried to constant weight take out, break up with beater; Powder material after breaing up as for calcine 60min in the Muffle furnace under 600 ℃, is promptly obtained siliceous porous material.
Embodiment two:
Get asbestos tailings hydrochloric acid and leach filter residue 200kg, add clear water 600L, in dispersator, wash 10min, filter with plate and frame filter press; Filter cake adds clear water with dispersator once more and breaks up washing, and filter-press dehydration does not have Cl in filtrate then
-Detect (AgNO with 0.1%
3Solution trial does not have precipitation); Adopt the powerful breaking drier of QGS-1 type with filtration cakes torrefaction, 260 ℃ of baking temperatures (85 ℃ of drying machine outlet temperatures); (drum speed 1~2r/min) is calcined, and calcines 50min down at 600 ℃, promptly gets siliceous porous material with φ 780 * 8600 rotary kilns with dried powder.
Table 1 is the physicochemical properties check and analysis result of embodiment product.Table 2 is the siliceous porous material Adsorption of Cu of embodiment two preparations
2+, Pb
2+, Ni
2+, Cd
2+, Cr
3+Result of the test.
The physicochemical properties check and analysis result of table 1 embodiment product
Table 2 siliceous porous material absorption Gu
2+, Pb
2+, Ni
2+, Cd
2+, Cr
3+Result of the test
Claims (3)
1. method with preparing siliceous porous material by asbestos tailings acid leaching residue is characterized in that its processing step is:
Calcine with the asbestos tailings acidleach and after solid slag washing, filtration and the drying after filtering, promptly obtain siliceous porous material.
2. the preparation method of siliceous porous material according to claim 1 is characterized in that described washing, filters to be with clear water cyclic washing, filtration, does not have acid ion to detect in filtrate.
3. the preparation method of siliceous porous material according to claim 1 is characterized in that described calcining, and its process conditions are 400~800 ℃ of calcining heats; Calcination time 30~120min.
Priority Applications (1)
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CN200810222081A CN101670268A (en) | 2008-09-09 | 2008-09-09 | Method for preparing siliceous porous material by asbestos tailings acid leaching residue |
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Publication Number | Publication Date |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108298545A (en) * | 2017-01-11 | 2018-07-20 | 中国科学院过程工程研究所 | Utilize the method for sulfuric acid and metal chloride medium de_ironing refinement quartz sand |
CN111013526A (en) * | 2019-11-18 | 2020-04-17 | 昆明理工大学 | Antimony tailing based adsorption material and preparation method and application thereof |
CN111107950A (en) * | 2017-08-24 | 2020-05-05 | 蒙彼利埃大学 | Asbestos waste destruction and value-adding method |
-
2008
- 2008-09-09 CN CN200810222081A patent/CN101670268A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108298545A (en) * | 2017-01-11 | 2018-07-20 | 中国科学院过程工程研究所 | Utilize the method for sulfuric acid and metal chloride medium de_ironing refinement quartz sand |
CN108298545B (en) * | 2017-01-11 | 2021-08-10 | 中国科学院过程工程研究所 | Method for removing iron and purifying quartz sand by using sulfuric acid and metal chloride medium |
CN111107950A (en) * | 2017-08-24 | 2020-05-05 | 蒙彼利埃大学 | Asbestos waste destruction and value-adding method |
US11577112B2 (en) | 2017-08-24 | 2023-02-14 | Université De Montpellier | Asbestos waste destruction and valorization method |
CN111013526A (en) * | 2019-11-18 | 2020-04-17 | 昆明理工大学 | Antimony tailing based adsorption material and preparation method and application thereof |
CN111013526B (en) * | 2019-11-18 | 2022-02-11 | 昆明理工大学 | Antimony tailing based adsorption material and preparation method and application thereof |
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Open date: 20100317 |