CN100443159C - Cation flocculant of surface modified attapulgite, and preparation method - Google Patents
Cation flocculant of surface modified attapulgite, and preparation method Download PDFInfo
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- CN100443159C CN100443159C CNB2006100430109A CN200610043010A CN100443159C CN 100443159 C CN100443159 C CN 100443159C CN B2006100430109 A CNB2006100430109 A CN B2006100430109A CN 200610043010 A CN200610043010 A CN 200610043010A CN 100443159 C CN100443159 C CN 100443159C
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- flocculant
- concavo
- surface modified
- modified attapulgite
- convex rod
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Abstract
The present invention provides a flocculant of surface modified attapulgite. A silicon coupling agent is used to carry out surface functionalization to attapulgite, then a cation etherifying agent is used to carry out cationization, and the flocculant of surface modified attapulgite is obtained. The flocculant of the present invention has the super-strong adsorption of nano attapulgite and simultaneously has high surface activity, cation property and strong flocculating performance, the flocculant can be used for a sludge flocculating and dehydrating process in sewage treatment as well as a coagulating sedimentation process in the sewage treatment, and can partially remove pollutants in sewage, such as COD, NH4<+>-N, heavy metal, etc., and meanwhile, the flocculant of the present invention has the advantages of high flocculation speed, high settling speed, low cost and low price without residual matter and pollution to water bodies after water is treated.
Description
Technical field
The invention belongs to water-treatment technology field, relate to a kind of flocculant that is used to flocculate with the coagulation water treatment procedure, relate in particular to a kind of cation flocculant of surface modified attapulgite and preparation method thereof.
Background technology
Flocculation is the important technical links of sewage disposal process with coagulation, only just can finish wastewater treatment alone with flocculation and coagulation process under some situation.Therefore, flocculant and coagulant are the importances of new process for treating waste water and new material development exploitation, and corresponding product quantity is huge, various in style.Because modernization industry and modernization life improve the content of organic matter in the draining greatly, and the particulate that contains in the aqueous systems of organic matter or colloid has negative electrical charge mostly, use cationic flocculant to handle to this class waste water, can play charge neutrality and adsorption bridging effect with the particulate in the water simultaneously, thereby the particulate in the water is taken off surely, help sedimentation and filtering means dehydration, generally can play the effect of direct Separation of Solid and Liquid.Nano particle is widely used in polymer modification because of nano effects such as its quantum size effect, small-size effect, skin effect and macro quanta tunnel effects, and has formed the series of new techniques high performance material.There is hydroxyl and the unique crystal pore passage structure of different residual bonds to be in different bonding states in the nano-attapulgite surface, has very big specific area, strong adsorption bleaching characteristic.Along with cationic flocculant has occupied more and more important position in water treatment, its synthetic method is also more and more.
A kind of concavo-convex excellent sewage-treating agent and production method are disclosed among the Chinese patent application CN200410041493.X, this sewage-treating agent is a raw material with concavo-convex rod, after acidification, dry, add alum and modified starch and grind jointly, obtain concavo-convex excellent sewage-treating agent.Though this patent has small investment, low, the simple characteristics of cost, alum has behind water purification and residual there is secondary pollution in water body.
Disclose a kind of " nanometer ultra-high efficiency flocculating agent " among the Chinese patent application CN1303821A, this flocculant is with SiOx and Al
2O
3Be scattered in the various polyacrylamide flocculants in the mechanical agitation mode Deng metal oxide nanoparticles.Because SiOx and Al
2O
3Deng the agglomeration of metal oxide nanoparticles, make its dispersion effect in high polymer coagulant relatively poor.
Summary of the invention
The purpose of this invention is to provide that a kind of cost is low, flocculating property is strong, free of contamination cation flocculant of surface modified attapulgite.
Another object of the present invention provides the preparation method of this cation flocculant of surface modified attapulgite.
Cation flocculant of surface modified attapulgite of the present invention is concavo-convex rod to be carried out earlier surface-functionalized with silicone couplet, carries out cationization with cationic etherifying agent again and gets.
The preparation method of cation flocculant of surface modified attapulgite of the present invention may further comprise the steps:
1. in concavo-convex rod, add the absolute alcohol kind solvent by 1: 3～1: 5 volume ratio and soak 6～12h, in the alcoholic solution of concavo-convex rod, add silicone couplet then with 1: 1～1: 3 volume ratio, ultrasonic dispersion 1～4 hour, oven dry obtains the concavo-convex rod of surface-functional with toluene extracting in apparatus,Soxhlet's;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 1～1: 3 volume ratio and soak 1～4h, stirring is carried out expanded under 20～60 ℃ again, in solution, add cationic etherifying agent with 1: 3～1: 10 mass ratio then, at 30-80 ℃ of following constant temperature stirring reaction 2～6h, discharging, filtration, filter cake spends deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets.
The silicone couplet that the present invention adopts is a gamma-aminopropyl-triethoxy-silane.
The cationic etherifying agent that the present invention adopts is 2,3-epoxypropyl trimethylammonium chloride ammonium.
The absolute alcohol kind solvent that the present invention adopts can be methyl alcohol, ethanol or propyl alcohol, also can be ethylene glycol etc.
The flocculating property of cation flocculant of surface modified attapulgite of the present invention can be confirmed by the coagulation experiment to the campus life composite wastewater:
Gather the campus composite wastewater, outward appearance: faint yellow, there is the canescence suspension to exist; Pungent stench is arranged, and whole water body has certain viscosity.
Drop into the gained cation flocculant of surface modified attapulgite of the present invention of sewage quality 0.05%～0.5%, stirred 3～8 minutes, detect the coagulating treatment result.See Table 1.
The coagulating treatment result of table 1 city domestic sewage
| Index | Turbidity (NTU) | SS(mg/L) | COD(mg/L) | NH 4 +-N(mg/L) |
| Former water | 184 | 491 | 264 | 75.8 |
| Handle water | 5 | 18 | 125 | 60.9 |
| Clearance (%) | 97.3 | 96.3 | 52.7％ | 19.7 |
Show that from the experimental result of table 1 flocculation rate of cation flocculant of surface modified attapulgite of the present invention is fast, higher to the clearance of the suspension in the waste water, SS, and can partly remove COD and NH in the waste water
4 +-N demonstrates good coagulation property.
Of the present invention have following advantage compared to existing technology:
1, cation flocculant of surface modified attapulgite of the present invention is to carry out surface-functionalized with silicone couplet earlier to concavo-convex rod, carry out cationization with cationic etherifying agent again and get, superpower adsorptivity with nano-attapulgite, have again simultaneously very high surface-active and cationic characteristic are arranged, integrate adsorption bridging and the charging neutrality net is caught, improved absorption and the bridge formation function of flocculant exponentially, constituted effectively collaborative flocculation system and improved flocculating property suspended particles in the water body and dissolved organic matter.
2, cation flocculant of surface modified attapulgite of the present invention can be used for the mud flocculation dewatering process of sewage disposal, also can be used for the precipitation process of coagulation of sewage disposal, and can partly remove COD in the sewage, NH
4 +Pollutant such as-N, heavy metal.
3, the flocculation rate of cation flocculant of surface modified attapulgite of the present invention is fast, sinking speed is fast, can with organic flocculant, the composite use of inorganic flocculating agent, the scope of application is wide.
4, it is abundant, cheap that the present invention prepares the concavo-convex excellent reserves of raw material of cation flocculant of surface modified attapulgite, and preparation technology is simple, and cost is low.
5, of the present invention modified attapulgite cationic flocculant noresidue material after water treatment can not pollute water body.
The specific embodiment
The preparation of embodiment 1, a kind of cation flocculant of surface modified attapulgite:
1. the volume ratio of pressing 1: 3 adds soaked in absolute ethyl alcohol 12h in concavo-convex rod, in the ethanolic solution of concavo-convex rod, add gamma-aminopropyl-triethoxy-silane then with 1: 1 volume ratio, ultrasonic dispersion 4 hours, oven dry obtains the concavo-convex rod of surface-functional with the toluene extracting;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 1 volume ratio and soak 4h, stirring is carried out expanded under 20 ℃ again, in solution, add 2 with 1: 3 mass ratio then, 3-epoxypropyl trimethylammonium chloride ammonium, at 30 ℃ of following constant temperature stirring reaction 6h, discharging, filtration, filter cake spend deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets.
The preparation of embodiment 2, a kind of cation flocculant of surface modified attapulgite:
1. in concavo-convex rod, add no water glycol by 1: 4 volume ratio and soak 10h, in the ethylene glycol solution of concavo-convex rod, add gamma-aminopropyl-triethoxy-silane then with 1: 2 volume ratio, ultrasonic dispersion 3 hours, oven dry obtains the concavo-convex rod of surface-functional with the toluene extracting;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 2 volume ratio and soak 3h, stirring is carried out expanded under 30 ℃ again, in solution, add 2 with 1: 5 mass ratio then, 3-epoxypropyl trimethylammonium chloride ammonium, at 50 ℃ of following constant temperature stirring reaction 4h, discharging, filtration, filter cake spend deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets.
The preparation of embodiment 3, a kind of cation flocculant of surface modified attapulgite:
1. in concavo-convex rod, add anhydrous propyl alcohol by 1: 5 volume ratio and soak 8h, in the alcoholic solution of concavo-convex rod, add gamma-aminopropyl-triethoxy-silane then with 1: 3 volume ratio, ultrasonic dispersion 1 hour, oven dry obtains the concavo-convex rod of surface-functional with the toluene extracting;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 3 volume ratio and soak 4h, stirring is carried out expanded under 40 ℃ again, in solution, add 2 with 1: 8 mass ratio then, 3-epoxypropyl trimethylammonium chloride ammonium, at 70 ℃ of following constant temperature stirring reaction 3h, discharging, filtration, filter cake spend deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets.
The preparation of embodiment 4, a kind of cation flocculant of surface modified attapulgite:
1. in concavo-convex rod, add absolute methanol by 1: 3.5 volume ratio and soak 6h, in the methanol solution of concavo-convex rod, add gamma-aminopropyl-triethoxy-silane then with 1: 2.5 volume ratio, ultrasonic dispersion 2 hours, oven dry obtains the concavo-convex rod of surface-functional with the toluene extracting;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 1 volume ratio and soak 1h, stirring is carried out expanded under 60 ℃ again, in solution, add 2 with 1: 10 mass ratio then, 3-epoxypropyl trimethylammonium chloride ammonium, at 80 ℃ of following constant temperature stirring reaction 2h, discharging, filtration, filter cake spend deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets.
Claims (2)
1, a kind of preparation method of cation flocculant of surface modified attapulgite may further comprise the steps:
1. in concavo-convex rod, add the absolute alcohol kind solvent by 1: 3～1: 5 volume ratio and soak 6～12h, in the alcoholic solution of concavo-convex rod, add silicone couplet then with 1: 1～1: 3 volume ratio, ultrasonic dispersion 1～4 hour, oven dry obtains the concavo-convex rod of surface-functional with toluene extracting in apparatus,Soxhlet's; Described silicone couplet is a gamma-aminopropyl-triethoxy-silane;
2. in the concavo-convex rod of above-mentioned surface-functional, add deionized water by 1: 1～1: 3 volume ratio and soak 1～4h, stirring is carried out expanded under 20～60 ℃ again, in solution, add cationic etherifying agent with 1: 3～1: 10 mass ratio then, at 30～80 ℃ of following constant temperature stirring reaction 2～6h, discharging, filtration, filter cake spends deionised water, suction filtration, the dry surface modified attapulgite flocculant that gets; Described cationic etherifying agent is 2,3-epoxypropyl trimethylammonium chloride ammonium.
2, the cation flocculant of surface modified attapulgite of the method for claim 1 preparation.
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| CN100443159C true CN100443159C (en) | 2008-12-17 |
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| CN101973616B (en) * | 2010-10-29 | 2012-07-25 | 淮阴工学院 | Method for preparing composite coagulant used for treating slightly polluted raw water |
Citations (5)
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|---|---|---|---|---|
| WO2001090000A1 (en) * | 2000-05-19 | 2001-11-29 | Commonwealth Scientific And Industrial Research Organisation | Removal of toxins from water |
| US20020011447A1 (en) * | 1999-09-30 | 2002-01-31 | Waldmann John J. | Chemical composition for treatment of nitrate and odors from water streams and process wastewater treatment |
| CN1363515A (en) * | 2002-01-28 | 2002-08-14 | 国家非金属矿深加工工程技术研究中心 | Process for preparing natural magnesium aluminium silicate gel |
| CN1597541A (en) * | 2004-07-27 | 2005-03-23 | 许庆华 | Concave convex rod sewage treatment agent and its production method |
| WO2005075362A1 (en) * | 2004-02-04 | 2005-08-18 | Ciba Speciality Chemicals Water Treatments Limited | Production of a fermentation product |
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2006
- 2006-06-15 CN CNB2006100430109A patent/CN100443159C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020011447A1 (en) * | 1999-09-30 | 2002-01-31 | Waldmann John J. | Chemical composition for treatment of nitrate and odors from water streams and process wastewater treatment |
| WO2001090000A1 (en) * | 2000-05-19 | 2001-11-29 | Commonwealth Scientific And Industrial Research Organisation | Removal of toxins from water |
| CN1363515A (en) * | 2002-01-28 | 2002-08-14 | 国家非金属矿深加工工程技术研究中心 | Process for preparing natural magnesium aluminium silicate gel |
| WO2005075362A1 (en) * | 2004-02-04 | 2005-08-18 | Ciba Speciality Chemicals Water Treatments Limited | Production of a fermentation product |
| CN1597541A (en) * | 2004-07-27 | 2005-03-23 | 许庆华 | Concave convex rod sewage treatment agent and its production method |
Non-Patent Citations (4)
| Title |
|---|
| 凹凸棒石改性机理研究进展. 赵娣芳等.硅酸盐通报，第3期. 2005 |
| 凹凸棒石改性机理研究进展. 赵娣芳等.硅酸盐通报，第3期. 2005 * |
| 纳米凹凸棒土的表面修饰及表征. 宋仁峰等.硅酸盐通报，第3期. 2003 |
| 纳米凹凸棒土的表面修饰及表征. 宋仁峰等.硅酸盐通报，第3期. 2003 * |
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