CN103304016B - A kind of method utilizing attapulgite to prepare hybrid flocculant - Google Patents
A kind of method utilizing attapulgite to prepare hybrid flocculant Download PDFInfo
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- CN103304016B CN103304016B CN201310262880.5A CN201310262880A CN103304016B CN 103304016 B CN103304016 B CN 103304016B CN 201310262880 A CN201310262880 A CN 201310262880A CN 103304016 B CN103304016 B CN 103304016B
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- flocculant
- acrylamide monomer
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Abstract
A kind of method utilizing attapulgite to prepare hybrid flocculant of the present invention, belongs to material preparation and field of water processing technology.In air atmosphere, under certain temperature condition, adopt the divalent salts FeSO of transition-metal Fe
4with NaHSO
3the binary initiator system of composition, has successfully caused acrylamide monomer (AM), on attapulgite surface, graft polymerization reaction has occurred, and had neither part nor lot in the monomer (AM) of reaction by washing with alcohol, prepared recessed native grafted polyacrylamide hybrid flocculant.Feature of the present invention is that environmental risk is little, and the hybrid flocculant cost prepared is low not containing heavy metal ion, and technique is simple, fine to the removal effect of turbidity.
Description
Technical field
The present invention relates to a kind of method utilizing attapulgite to prepare hybrid flocculant, belong to material preparation and field of water processing technology.
Background technology
In recent years, flocculence be most widely used in water technology and method, one of conventional method, in water treatment, the water factory of all earth surface water sources, flucculation process is almost one of indispensable treatment process, any one treatment stage, all can with other treatment processs with the use of, in the tertiary treatment of some trade effluents, also often adopt the method for flocculation treatment.Flocculent precipitation refers to the method by the colloid in the aqueous solution or the raw flocks of suspended particle produce.Comprise inorganics and organism, also partly can remove some deliquescent impurity simultaneously, even improve the dewatering of mud.
The sorting technique of flocculation agent has a variety of, by the difference of composition, generally can be divided into the biological flocculant of inorganic flocculating agent, organic floculant and rising in recent years.Inorganic flocculating agent also claims flocculation agent, and metal-salt kind can be divided into aluminium salt system and molysite system two class, can be divided into again hydrochloric acid system and sulfuric acid system by anionic component; Its advantage is cheap, is widely used in feeding water, the various flow processs of trade effluent and municipal effluent, becomes the main flow of flocculation agent gradually.Organic floculant mainly relies on bridging action to make particle precipitation, therefore again organic floculant is called flocculation agent or coagulant aids.Organic floculant can be divided three classes: Syn-Organic flocculants, natural organic high-molecular modified flocculant, microbial flocculant.Although inorganic flocculating agent is strong to the water treatment suitability of various complicated ingredient, the flco that the flco generated generates not as good as organic polymer coargulator is large, and dosage is large.Compared with inorganic flocculating agent, organic polymer coargulator consumption is few, and flocculation rate is fast, and the salt that coexisted, medium PH and ambient temperature effect are little, generate sludge quantity few, and organic polymer coargulator molecule can be with a COO
one, a NH-, the hydrophilic radical such as-OH, can have a various structures such as chain, ring-type, be beneficial to pollutent and enter flco, decolourising property is good.But organic polymer coargulator or its hydrolysis, degraded product is poisonous, and cost is also higher.If inorganic, organic floculant are combined to use and just in time can make up respective shortcoming, the flocculating effect forming an inorganic organic polymer composite flocculant is also more excellent.
Attapulgite is a kind of chain layer silicate mineral containing Shuifu County's magnalium, there is the duct of the multiple nanoscale be parallel to each other, it has special crystalline structure and character, a large amount of wetting ability silicone hydroxyl is there is through its surface modified, effective grafting or composite can be there is with other groups, prepare matrix material.Zhang Yue [patent No.: CN102153176] utilizes the thinking of Ballasted Flocculation Technology to design Attapulgite carrier flocculation water treatment agent, the Polyferric Sulfate salt generated with ferrous salt and oxidant reaction is for coagulating agent, adding auxiliary agent again carries out composite, prepare inorganic polymer flocculant, although effectively algae can be removed, but there is the control problem of acid in preparation feedback system, secondary pollution may be caused to environment.Graft copolymerization is carried out with acrylamide by solution polymerization process after Zhao Yijiang [patent No.: CN101342482A] adopts silane coupler modified attapulgite; But react under the protective condition of rare gas element, this adds increased cost.
Summary of the invention
The object of the invention is: provide a kind of method utilizing attapulgite to prepare hybrid flocculant, the method process is simple, prepares flocculation agent under normal temperature, air atmosphere condition, reduces production cost, reduction production technique.
Technical solution of the present invention is: the divalent salts FeSO adopting transition-metal Fe
4with NaHSO
3the binary initiator system of composition, in the middle of air, under certain temperature condition, successfully cause acrylamide monomer (AM), on recessed soil (ATP) surface, graft polymerization reaction has occurred, and the monomer (AM) of reaction is had neither part nor lot in by washing with alcohol, prepare recessed native grafted polyacrylamide hybrid flocculant.
A kind of method utilizing attapulgite to prepare hybrid flocculant, carry out according to following: acrylamide monomer (AM) is dissolved in the distilled water of certain mass, add the concave and convex rod stone powder of certain mass mark again, stirring and evenly mixing, then be placed in the water-bath of certain temperature, then add initiator divalent iron salt FeSO successively
4with NaHSO
3, polymerization for some time successfully prepares hybrid flocculant.
Wherein said attapulgite is that colloid attapulgite raw ore is soaked more than 48h, removes impurity, dries, cross 200 mesh sieve, obtain Powdered, for subsequent use.
Wherein said is dissolved in distilled water by the acrylamide monomer of certain mass, and wherein the massfraction of monomer is 10%-20%.
The addition accounting for monomer of wherein said attapulgite is 1%-15% in mass.
Wherein said initiator divalent iron salt FeSO
4with NaHSO
3the molar weight molar weight that accounts for acrylamide monomer be 7 × 10
-4-21 × 10
-4, and the molar ratio of the two is 1:5.
The system temperature of wherein said polyreaction is at 25 DEG C-45 DEG C, and polymerization reaction time is 3h.
Feature of the present invention is that environmental risk is little, and the hybrid flocculant cost prepared is low not containing heavy metal ion, and technique is simple, fine to the removal effect of turbidity.
The present invention has the following advantages:
(1) add the attapulgite of low cost in preparation process, the cost of hybrid flocculant is reduced greatly.
(2) hybrid flocculant preparation process is simple, and step is few, and initiator used is not containing heavy metal ion, free from environmental pollution.
(3) required in preparation process experiment condition is air atmosphere, does not need protection of inert gas, and meanwhile, less demanding to temperature, polymerization time is short, also reduces production cost.
(4) alumen ustum that the flocculation agent prepared produces is tiny, and settling velocity is fast, and consumption is few.
Embodiment:
Embodiment 1: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 10%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 1%, stirs and makes it to mix.Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 85%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 2: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 20%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 15%, stirs and makes it to mix.Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 87%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 3: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 17.5%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 7%, stirs and makes it to mix.Gained solution is placed in the water-bath of 25 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 84%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 4: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 17.5%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 7%, stirs and makes it to mix.Gained solution is placed in the water-bath of 45 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 78%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 5: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 17.5%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 7%, stirs and makes it to mix.Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 7 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 79%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 6: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 17.5%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 7%, stirs and makes it to mix.Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 21 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 80%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Embodiment 7: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 17.5%, adds a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 7%, stirs and makes it to mix.Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product.And use ethanol soaked in absolute ethyl alcohol, agitation as appropriate, gluey flocculation agent is fully contacted with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs.After soaking 30min, then precipitate 2 times with absolute ethanol washing.Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant.The prepared clearance of flocculation agent to turbidity reaches 95%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
Claims (1)
1. the method utilizing attapulgite to prepare hybrid flocculant, it is characterized in that carrying out according to following: accurately take a certain amount of acrylamide monomer and be placed in beaker, add a certain amount of distilled water, wherein the massfraction of acrylamide monomer is 10%, add a certain amount of concave and convex rod stone powder, the amount that its concave soil accounts for monomer is 1%, stirs and makes it to mix; Gained solution is placed in the water-bath of 35 DEG C, after temperature-stable, drip initiator ferrous sulfate-sodium sulfite solution respectively, wherein initiator concentration is 10.5 × 10
-4mol/molAM, and the two ratio is 1:5, shakes up, and leaves standstill, and after polymerization 2h, obtains gluey thick product; And by alcohol immersion, agitation as appropriate, makes gluey flocculation agent fully contact with ethanol, makes unreacted acrylamide monomer be dissolved in organic solvent ethanol, in whipping process, adularescent precipitation occurs; After soaking 30min, then precipitate 2 times with absolute ethanol washing; Dry at product after washing being placed in 60 DEG C, baking oven, grinding, obtains hybrid flocculant; The prepared clearance of flocculation agent to turbidity reaches 85%, and alumen ustum is tiny, and settling velocity is fast, and flocculant usage is few.
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| CN104448082B (en) * | 2014-11-24 | 2016-08-24 | 福建师范大学 | A kind of calcium ions modified polyacrylamide preparation method |
| CN107793001B (en) * | 2017-09-21 | 2021-01-01 | 北京工业大学 | River sludge treating agent capable of being constructed in winter and used for adsorbing and curing heavy metal ions |
| CN109232817B (en) * | 2018-09-28 | 2020-10-30 | 常州大学 | Preparation method of in-situ reaction compatibilization polypropylene/attapulgite composite material |
| CN114477398A (en) * | 2022-01-29 | 2022-05-13 | 武汉大学 | Method for strengthening coagulation denitrification of black and odorous water body by GCS compound material |
| CN116477815B (en) * | 2023-06-25 | 2023-10-31 | 湖南子宏生态科技股份有限公司 | Domestic sewage treatment method |
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