CN102380346B - Organic/inorganic flaky adsorbing material and application thereof in acidic printing and dyeing wastewater - Google Patents
Organic/inorganic flaky adsorbing material and application thereof in acidic printing and dyeing wastewater Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 239000002351 wastewater Substances 0.000 title claims abstract description 12
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- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 39
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 23
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 229910001868 water Inorganic materials 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 25
- 239000000725 suspension Substances 0.000 claims description 23
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 17
- 229910052708 sodium Inorganic materials 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
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- 230000032683 aging Effects 0.000 claims description 10
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- 238000000926 separation method Methods 0.000 abstract description 6
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- 239000003795 chemical substances by application Substances 0.000 abstract 3
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 abstract 2
- 238000009396 hybridization Methods 0.000 abstract 1
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- 229910021641 deionized water Inorganic materials 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- YYYARFHFWYKNLF-UHFFFAOYSA-N 4-[(2,4-dimethylphenyl)diazenyl]-3-hydroxynaphthalene-2,7-disulfonic acid Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C(S(O)(=O)=O)=CC2=CC(S(O)(=O)=O)=CC=C12 YYYARFHFWYKNLF-UHFFFAOYSA-N 0.000 description 5
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- 238000002360 preparation method Methods 0.000 description 5
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- 229920001661 Chitosan Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
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- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
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- 238000004062 sedimentation Methods 0.000 description 2
- -1 surfactant-modified organo montmorillonite Chemical compound 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
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- 125000000129 anionic group Chemical group 0.000 description 1
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- 239000000440 bentonite Substances 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 238000004065 wastewater treatment Methods 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an organic/inorganic flaky adsorbing material and an application thereof to acidic printing and dyeing wastewater. The organic/inorganic hybridization flaky adsorbing material is synthesized by the following method that: Na-montmorillonite is taken and is uniformly dispersed in water to obtain montmorillonite suspending liquid; organic silane coupling agents are uniformly dispersed in absolute ethyl alcohol, in addition, the mixed materials are slowly added into the montmorillonite suspending liquid and are uniformly stirred, and the organic silane coupling agents are ethyl orthosilicate or 1,6-bi-trimethoxy silica-based hexane; acid is used for regulating the pH value of the mixed liquid to 1 to 3, and the mixed liquid is continuously stirred for a certain time at 20 to 50 DEG C to form uniform milk-white gel; the milk-white gel is aged until the solvent is completely volatilized; and the organic/inorganic flaky adsorbing material is obtained through drying. The adsorbing agent can be applied to the acidic printing and dyeing wastewater. Because the adsorbing agent has the paper type structure feature, the adsorbing agent can be fast extracted from the adsorbing liquid in the adsorption separation, and the settlement separation is not needed.
Description
(1) technical field
The present invention relates to the application of hydridization sheet adsorbent and the absorption acid dyes thereof of a kind of novel hybrid adsorbent and application, particularly a kind of organosilan/imvite in dyeing waste water absorption.
(2) background technology
Imvite is the silicate clay mineral of a class stratiform, because its aboundresources, interlayer cation interchangeability, such mineral have the ability of Liquidity limit and polarity organic molecule, is used as adsorbent and flocculant in the wastewater treatment of being everlasting.Studies show that in recent years, through surfactant-modified organo montmorillonite, organic wastewater had been demonstrated adsorption bleaching effect preferably.(the Wang Hongmei such as Wang Hongmei, Zheng Zhenhui, the processing research [J] of the gorgeous .PDMDAAC-bentonite of Yue Qin to active dye wastewater. water technology, 2005,31 (12): 16-19.) utilize the imvite of PDDA (PDMDAAC) blending and modifying, and be used for the decolouring of active dye wastewater, studies show that, under the same conditions, the absorption property outline of PDMDAAC-imvite is better than active carbon.(the Wang Li such as Wang Li, Wang Aiqin. the preparation of Chitosan/Montmorillonite Hybrid Nanocomposite reaches the absorption property [J] to dyestuff. polymer material science and engineering, 2007,23 (5): 104-107.) use the chitosan intercalation modified montmorillonoid, prepared Chitosan/Montmorillonite Hybrid Nanocomposite, the impact of preparation condition on composite structure has been discussed, and studied the absorption of this composite for congo red.Result shows, along with the increase of shitosan amount, the structure of composite by intercal type to exfoliated transformation.When shitosan and imvite mol ratio surpassed 5: 1, organic degree did not almost change, and illustrates that the intercalation of shitosan and imvite has reached balance.The increase along with organic degree, the also corresponding increase of adsorbance that nano composite material is Congo red to anionic dye are found in research.But because the grain diameter of montmorillonite composite material is less, easily disperse in the aqueous solution, the characteristic such as suspension, make its effect when processing waste water not satisfactory, particularly Separation of Solid and Liquid speed is slow, flocculate costs and poor dehydration results, adsorbent be free settling etc. not, has affected its practical application.Therefore, research and develop the clay-based sorbing material that is easy to separate and be still problem demanding prompt solution.
The at present existing organosilane-modified imvite of bibliographical information, hydroxyl in imvite can be divided into non-reacted hydroxyl and reactable hydroxyl, the aluminium hydroxyl that wherein is enclosed in silicon-oxy tetrahedron is non-reacted hydroxyl, and the hydroxyl that is positioned at the montmorillonite layer edge is the reactable hydroxyl.Organosilane-modified dose can with the reactable hydroxyl reaction on imvite surface, thereby be grafted in imvite.Reaction mechanism can be expressed as:
RSiX
3+H
2O→RSi(OH)
3+HX (1-2)
Clay|-OH+RSi(OH)
3→Clay|-O-Si-R+H
2O (1-3)
Li Jisen [Li Jisen. the research of methyl orange in the preparation of organic modification montmonrillonite and adsorbed water. the master thesis .2007 of University Of Yantai] use octadecyl trichlorosilane alkane modified montmorillonoid, and take methyl orange solution as dye wastewater, investigated the absorption property of modified montmorillonoid composite to methyl orange.
But above-mentioned research, the imvite based composites of preparation is mainly to carry out modification between cheating engaging layer, organic modifiers is introduced the interlayer of imvite by methods such as ion-exchanges, obtain organically-modified composite, and the material that obtains is granular, can scatter fast in solution, must adopt sedimentation separation.
(3) summary of the invention
The technical problem to be solved in the present invention is to provide a kind of organic/inorganic flaky adsorbent, and this adsorbent has " scraps of paper shape " architectural feature, can extract fast adsorbent from adsorption liquid in adsorbing separation, and not need sedimentation separation.
For solving the problems of the technologies described above, the concrete technical scheme that the present invention adopts is as follows:
A kind of organic/inorganic flaky adsorbing material, synthetic by the following method: as to get sodium-based montmorillonite and be dispersed in water, obtain montmorillonite suspension liquid; Organo silane coupling agent is dispersed in absolute ethyl alcohol, and slowly joins in montmorillonite suspension liquid, stir, described organo silane coupling agent is the two silica-based hexanes of trimethoxy of ethyl orthosilicate or 1,6-; Regulate the pH value to 1 of mixed liquor～3 with acid, at 20～50 ℃ of lower continuous stirring certain hours until form even milky gel; The milky gel is carried out ageing to solvent to volatilize fully; Drying namely obtains described organic/inorganic flaky adsorbing material again.
In the present invention, be 1: 10～40 samplings according to the mass ratio of sodium-based montmorillonite and water, sodium-based montmorillonite is dispersed in water, obtain montmorillonite suspension liquid.For obtaining finely dispersed suspension, can be by conventional methods such as ultrasonic or stirrings.
In the present invention, be 1: 2～20 samplings according to the mass ratio of organosilan and ethanolic solution, organo silane coupling agent is dispersed in absolute ethyl alcohol.Be uniformly dispersed for making, can be by conventional methods such as ultrasonic or stirrings.
In the present invention, the mixing quality of described sodium-based montmorillonite and organo silane coupling agent ratio is 1: 1～10, be preferably 1: 1～and 5, most preferably be 1: 1.
Regulate the pH value of mixed liquor in the present invention with acid, described acid is hydrochloric acid, and the present invention does not have special requirement for concentration of hydrochloric acid, generally can select 0-5mol/L hydrochloric acid.
The present invention preferably regulates the pH to 2 of mixed liquor.
After the present invention regulates the pH of mixed value, preferably formed even milky gel in 2～72 hours 20～50 ℃ of (more preferably at 25 ℃) continuous stirring, the preferred continuous stirring time is 2～30 hours, and more preferably the continuous stirring time is 2～5 hours.
In the present invention, the digestion time of milky gel is generally about 5 days, until solvent volatilizees fully.
In the present invention, described drying condition is: baking temperature is 50～90 ℃, and be 24～72 hours drying time.
The present invention is concrete recommends described organic/inorganic flaky adsorbing material specifically synthetic in accordance with the following steps: the mass ratio according to sodium-based montmorillonite and water is 1: 10～40 samplings, and sodium-based montmorillonite is dispersed in water, obtains montmorillonite suspension liquid; Mass ratio according to organo silane coupling agent and absolute ethyl alcohol is 1: 2～20 samplings, organo silane coupling agent is dispersed in absolute ethyl alcohol, and slowly join in montmorillonite suspension liquid, stir, described organo silane coupling agent is ethyl orthosilicate or 1, the two silica-based hexanes of trimethoxy of 6-, the mixing quality ratio of described sodium-based montmorillonite and organo silane coupling agent is 1: 1～5; Regulate the pH value to 2 of mixed liquor with hydrochloric acid, formed even milky gel in 2～5 hours 25 ℃ of lower continuous stirring; The milky gel is carried out ageing to solvent to volatilize fully; 50～90 ℃ of dryings are 24～72 hours again, namely obtain described organic/inorganic flaky adsorbing material.
The organic/inorganic flaky adsorbing material that the present invention makes can be applicable in acid dyeing waste water.Its absorption property can detect by the following method: get acid scarlet 25mg (0.025g), insert in conical flask, add 500ml distilled water, shake up, make 50mg/L acid scarlet solution.Regulate the pH value to 0.5 of adsorption liquid～10 with 1mol/L HCl or NaOH solution, add 0.01～0.5g composite material adsorbent, at 20 ± 2 ℃ of lower adsorption reaction 8-72h.
Compared with prior art, beneficial effect of the present invention is:
(1) new adsorbent has strip-like features.Synthetic adsorbent is the sheet adsorbent that end face connects, and does not disperse in reaction solution.Adsorbent can extract from reactant liquor in use fast.
(2) the absorbent preparation method is simple.
(4) description of drawings
Fig. 1: the SEM figure that (a)～(g) is respectively the organic/inorganic flaky material that embodiment 1～7 makes;
The absorption property result of the organic/inorganic flaky material that Fig. 2: embodiment 1～7 makes to acid scarlet G.
Fig. 3: the photo of organic/inorganic flaky material.
(5) specific embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described further, but protection scope of the present invention is not limited to this.
Get sodium-based montmorillonite (Changxing County, Zhejiang Province Chang'an, Zhejiang Province benevolence permanent Science and Technology Co., Ltd. produces, lower with) 0.5g in beaker, add the 10ml deionized water, ultrasonic wave disperses to make imvite after 30min and stirring at room 2h and disperses suspension preferably.Get 0.5g ethyl orthosilicate (TEOS) and be dispersed in the 10ml absolute ethyl alcohol, slowly join montmorillonite suspension liquid.The mass ratio of clay and TEOS is 1: 1.Regulate the pH value to 2 of mixed liquor with 1mol/L HCl, at 25 ℃ of lower continuous stirring 4h, form even milky gel.With gel ageing 5 days, volatilize fully to solvent, then be placed under 60 ℃, baking oven and dry 48h, namely obtain product.The SEM figure of product is as shown in Fig. 1 (a).
Embodiment 2
Get sodium-based montmorillonite 0.5g in beaker, add the 10ml deionized water, make imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 1.0g ethyl orthosilicate (TEOS) and be dispersed in the 10ml absolute ethyl alcohol, slowly join montmorillonite suspension liquid.The mass ratio of clay and TEOS is 1: 2.Regulate the pH value to 2 of mixed liquor with 1mol/L HCl, at 25 ℃ of lower continuous stirring 3h, form even milky gel.With gel ageing 5 days, volatilize fully to solvent, then be placed under 60 ℃, baking oven and dry 48h, namely obtain product.The SEM figure of product is as shown in Fig. 1 (b).
Embodiment 3
Get sodium-based montmorillonite 0.5g in beaker, add the 10ml deionized water, make imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 2.5g ethyl orthosilicate (TEOS) and be dispersed in the 10ml absolute ethyl alcohol, slowly join montmorillonite suspension liquid.The mass ratio of clay and TEOS is 1: 5.Regulate the pH value to 2 of mixed liquor with 1mol/L HCl, at 25 ℃ of lower continuous stirring 2h, form even milky gel.With gel ageing 5 days, volatilize fully to solvent, then be placed under 60 ℃, baking oven and dry 48h, namely obtain product.The SEM figure of product is as shown in Fig. 1 (c).
Embodiment 4
Get sodium-based montmorillonite 0.5g in beaker, add the 10ml deionized water, make imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 0.5g ethyl orthosilicate (TEOS) and be dispersed in the 10ml ethanolic solution, slowly join montmorillonite suspension liquid.The mass ratio of clay and TEOS is 1: 1.At 25 ℃ of lower continuous stirring 30h, form even milky gel.With gel ageing 5 days, volatilize fully to solvent, then be placed under 60 ℃, baking oven and dry 48h, namely obtain product.The SEM figure of product is as shown in Fig. 1 (d).
Get sodium-based montmorillonite 0.5g in beaker, add the 10ml deionized water, make imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 1.0g ethyl orthosilicate (TEOS) and be dispersed in the 10ml absolute ethyl alcohol, slowly join montmorillonite suspension liquid.The mass ratio of clay and TEOS is 1: 2.At 25 ℃ of lower continuous stirring 20h, form even milky gel.With gel ageing 5 days, volatilize fully to solvent, then be placed under 60 ℃, baking oven and dry 48h, namely obtain product.The SEM figure of product is as shown in Fig. 1 (e).
Embodiment 6
Get sodium-based montmorillonite 0.5g in beaker, add the 20ml deionized water, obtain imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 0.5g 1, the two silica-based hexanes of trimethoxy of 6-are dispersed in the 20ml absolute ethyl alcohol, then slowly join montmorillonite suspension liquid.The mass ratio of the two silica-based hexanes of trimethoxy of clay and 1,6-is 1: 1.Regulate the pH value to 2 of mixed liquor with 1mol/L HCl, at 25 ℃ of lower continuous stirring 2h, obtain even milky gel.With gel ageing 5 days, to volatilize fully to solvent, then be placed in baking oven 24h, 60 ℃ of oven dry namely obtain product.The SEM figure of product is as shown in Fig. 1 (f).
Get sodium-based montmorillonite 0.5g in beaker, add the 20ml deionized water, obtain imvite after ultrasonic wave dispersion 30min and stirring at room 2h and disperse suspension preferably.Get 0.5g 1, the two silica-based hexanes of trimethoxy of 6-are dispersed in the 20ml absolute ethyl alcohol, then slowly join montmorillonite suspension liquid.The mass ratio of the two silica-based hexanes of trimethoxy of clay and 1,6-is 1: 1.At 25 ℃ of lower continuous stirring 24h, obtain even milky gel.With gel ageing 5 days, to volatilize fully to solvent, then be placed in baking oven 24h, 60 ℃ of oven dry namely obtain product.The SEM figure of product is as shown in Fig. 1 (g).
Embodiment 8
Get acid scarlet 25mg (0.025g), insert in conical flask, add 500ml distilled water, shake up, make 50mg/L acid scarlet G solution.Regulate the pH value to 1 of adsorption liquid with 1mol/L HCl solution, the sorbing material that adds 0.1g embodiment 1～7 to make is at 20 ± 2 ℃ of lower adsorption reaction 10h.The absorption property result of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, embodiment 7 gained samples as shown in Figure 2.
Claims (2)
1. organic/inorganic flaky adsorbing material, it is characterized in that: described organic/inorganic flaky adsorbing material is specifically synthetic in accordance with the following steps: the mass ratio according to sodium-based montmorillonite and water is 1:10～40 samplings, sodium-based montmorillonite is dispersed in water, obtains montmorillonite suspension liquid; Mass ratio according to organo silane coupling agent and absolute ethyl alcohol is 1:2～20 samplings, organo silane coupling agent is dispersed in absolute ethyl alcohol, and slowly join in montmorillonite suspension liquid, stir, described organo silane coupling agent is ethyl orthosilicate or 1, the two silica-based hexanes of trimethoxy of 6-, the mixing quality of described sodium-based montmorillonite and organo silane coupling agent is than being 1:1～5; Regulate the pH value to 2 of mixed liquor with hydrochloric acid, formed even milky gel in 2～5 hours 25 ℃ of lower continuous stirring; The milky gel is carried out ageing to solvent to volatilize fully; 50～90 ℃ of dryings 24～72 hours, namely obtain described organic/inorganic flaky adsorbing material.
2. the application of organic/inorganic flaky adsorbing material as claimed in claim 1 in acid dyeing waste water.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1579938A (en) * | 2004-05-21 | 2005-02-16 | 浙江工业大学 | Method for preparing mesoporous silicon metal layer-column clay material |
| CN101003374A (en) * | 2006-11-27 | 2007-07-25 | 浙江大学 | Method for synthesizing composite material of organic - inorganic bentonite |
| CN101735667A (en) * | 2009-12-04 | 2010-06-16 | 浙江丰虹新材料股份有限公司 | Sol-gel modified organic montmorillonoid and organic silicon sol-gel for modification |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1579938A (en) * | 2004-05-21 | 2005-02-16 | 浙江工业大学 | Method for preparing mesoporous silicon metal layer-column clay material |
| CN101003374A (en) * | 2006-11-27 | 2007-07-25 | 浙江大学 | Method for synthesizing composite material of organic - inorganic bentonite |
| CN101735667A (en) * | 2009-12-04 | 2010-06-16 | 浙江丰虹新材料股份有限公司 | Sol-gel modified organic montmorillonoid and organic silicon sol-gel for modification |
Non-Patent Citations (2)
| Title |
|---|
| 于志纲等.蒙脱土改性的研究进展.《精细石油化工进展》.2005,第6卷(第8期),第5-8页. |
| 蒙脱土改性的研究进展;于志纲等;《精细石油化工进展》;20050830;第6卷(第8期);第5-8页 * |
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