CN102351992A - Preparation method of flocculation starch of grafting acrylamide - Google Patents
Preparation method of flocculation starch of grafting acrylamide Download PDFInfo
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- CN102351992A CN102351992A CN2011101947062A CN201110194706A CN102351992A CN 102351992 A CN102351992 A CN 102351992A CN 2011101947062 A CN2011101947062 A CN 2011101947062A CN 201110194706 A CN201110194706 A CN 201110194706A CN 102351992 A CN102351992 A CN 102351992A
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Abstract
The invention relates to a preparation method of a flocculation starch used in water quality purifying treatment. The preparation method of the flocculation starch of grafting acrylamide is characterized by comprising the following steps of: 1) physical initiation: sending starch to 60 Co-gamma ray radiation field, irradiating in an atmospheric environment with a radiation dose of 4-30 KGy to obtain an irradiating starch; 2) machinery mixing: adding the irradiating starch, acrylamide 50-100wt% of the irradiating starch and deionized water 100-200wt% of the irradiating starch in a mixer, stirring at a room temperature for 10-30 min to obtain a mixture; 3) graft polymerization: placing the mixture in a heat collecting constant temperature heating magnetic stirring apparatus, heating at 60-100 DEG C for 10-60 min, then washing obtained product with deionized water, drying and crushing to obtain the flocculation starch of grafting acrylamide. The flocculation starch prepared by the method has characteristics of fast sedimentation velocity, good sedimentation effect and segregative product.
Description
Technical field
The present invention relates to a kind of flocculation starch preparation method that purification of water quality is handled the preparation method, particularly a kind of graft acrylamide of flocculation starch that is used for.
Background technology
Utilizing natural macromolecular material to come the development of new flocculation agent is the problem that Chinese scholars is very paid close attention in recent years, and natural polymer has that the source is wide, price is low, degradable, characteristics such as nontoxic, in the flocculation agent industry, demonstrates bright development prospect.In numerous natural macromolecule flocculating agents, the research of starch base modified flocculant is particularly noticeable.The related patent U.S. Patent No. technology all has report both at home and abroad.
Chinese patent (200910095098.2), this invents employing
60The gamma-rays that Co produced is as source of radiation; Mixture to pasted starch and acrylamide under aerobic or oxygen free condition carries out irradiation; Produce free radical; Generate starch/acrylamide grafted copolymer; Realize that according to steps such as starch pasting, uniform mixing, radiation treatment, stabilizing treatment, modified-reactions starch/acrylamide grafted copolymer that makes by this method and derivative thereof can be widely used in papermaking, oil, mining and metallurgy, environmental protection and field of new.This directly to the method for the mixture irradiation grafting of starch and acrylamide, different fully with the grafting processing behind the independent irradiated starch remix of the present invention.
Chinese patent (200910062300.1), this invention is a raw material with starch, vinylformic acid, vinyl acetate, under the less water existence condition with three's mixture in
60Carry out irradiation under the normal temperature in the Co-γ irradiation field, with gained blend drying, pulverize, sieve binary-graft starch, it is as the textile sizing material.Compare with the present invention, not only method is different, and purposes is different.
Chinese patent (200910194176.4); This invention is initiator with potassium permanganate; Graft copolymer with starch and acrylamide polymerization in the reversed-phase emulsion that forms by whiteruss, water and composite emulsifier formation starch and acrylamide; Mainly the technical problem of Xie Jueing is the stability of emulsion system when improving the inverse emulsion polymerization reaction, and the starch that makes and the graft copolymer of acrylamide are used to handle kaolin suspension liquid, sanitary sewage, yellow mud water.This method is on the principle of preparation, and is different with the present invention.
Chinese patent (200910196533.0), the reinforced method of substep is adopted in this invention, is dissolved in starch and part non-ionic monomer, cationic monomer in the deionized water in advance; Oil mixture mixed together with oil phase solvent and emulsifying agent formation stirs then, under nitrogen protection, adds initiator then and carries out graft polymerization reaction; Behind the reaction certain hour, remaining non-ionic monomer is incorporated in continues reaction in the reaction system again, finally make cationic starch graft copolymer flocculant, products therefrom can be applicable to sewage disposal.Compare with the present invention, all inequality on preparation method and flow process.
In the above patent use is arranged
60Co-gamma-ray irradiation technology prepares graft starch, but does not directly use
60Co-gamma-ray irradiation starch, and then with the graft modification of gained irradiated starch, and reported and used the graft starch of this method preparation scarcely to be used as flocculation agent in the patent; With starch and acrylamide is the chemical method that the feedstock production flocculation agent adopts initiator to cause mostly, does not also see at present
60The Co-gamma-rays prepares irradiated starch, and then with gained irradiated starch and acrylamide graft, the patent and the bibliographical information of the flocculation starch of preparation graft acrylamide.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of flocculation starch of graft acrylamide, it is fast that the flocculation starch of this method preparation has settling velocity, and effect of settling is good, the segregative characteristics of product.
For realizing above-mentioned purpose, the technical scheme that the present invention taked is: a kind of preparation method of flocculation starch of graft acrylamide is characterized in that it comprises the steps:
1) physics causes: starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 4-30KGy, makes described starch produce free radical, obtains irradiated starch;
2) mechanically mixing: the add-on by acrylamide is the 50%-100% of irradiated starch quality, and the add-on of deionized water is the 100%-200% of irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 10-30min down, obtain mixture in normal temperature;
3) graft polymerization: mixture is placed heat collecting type thermostatically heating magnetic stirring apparatus (for existing installation); Under 60-100 ℃ of condition, heat 10-60min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, 40-60 ℃ of following vacuum-drying 2-3 hour, be crushed to the 125-400 order, the flocculation starch of graft acrylamide.
Described starch is W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch or sweet potato starch; Described acrylamide is a kind of white crystal chemical substance, is the production water treatment with one of raw material of flocculation agent.
Described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation (industrial dynamic radiation devices) for the loading of source amount.
Described atmospheric environment is meant the air conditions of normal temperature and pressure, because there is oxygen, is again that aerobic is handled, and can be described as aerobic irradiation.
Described irradiated starch is irradiation W-Gum, irradiation wheat starch, irradiation sorghum starch, irradiation Starch rice, irradiation yam starch, irradiation tapioca (flour), irradiation pueraria starch, irradiation sweet potato starch.
Compared with prior art, the present invention has following advantage:
1) the present invention uses the method that high-energy ray irradiation causes, and this method contrast conventional chemical initiation has advantages such as efficiency of initiation height, aftertreatment is simple, noresidue is pollution-free.
2) raw material that uses among the present invention all has good thermostability, and nontoxic, non-volatility helps environment protection and operator ' s health, and production efficiency is high, meets the requirement of green production.
Advantages such as 3) to have settling velocity fast for the flocculation starch of the graft acrylamide of the present invention preparation, and effect of settling is good, product is easily separated.The percentage of grafting of the flocculation starch of described graft acrylamide is at 40%-95%.
Flocculation starch of the present invention is applicable to the purifying treatment of sanitary sewage, petrochemical wastewater, paper waste.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention, should be understood that these instances only be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition that after the content of having read the present invention's instruction those skilled in the art can do work to the present invention and change or revise, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
In following examples: described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation for the loading of source amount.Described atmospheric environment is meant the air conditions of normal temperature and pressure, because there is oxygen, is again that aerobic is handled, and can be described as aerobic irradiation.
Embodiment 1:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: W-Gum is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 6KGy, makes described W-Gum produce free radical, obtains irradiated starch (being the irradiation W-Gum);
2) mechanically mixing: the add-on by acrylamide is 50% of an irradiated starch quality, and the add-on of deionized water is 100% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 20min down, obtain mixture in normal temperature;
3) graft polymerization: the mixture that stirs is placed heat collecting type thermostatically heating magnetic stirring apparatus (like DF-101 series heat collecting type thermostatically heating magnetic stirring apparatus); Under 60 ℃ of conditions, heat 30min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 50 ℃ of following vacuum-drying 2.5h, be crushed to 200 orders, percentage of grafting is 41.2% a graft acrylamide flocculation starch.
This graft acrylamide flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 15s, gets transmittance that supernatant liquid records behind the 15min greater than 85%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 2:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: pueraria starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 8KGy, makes described pueraria starch produce free radical, obtains irradiated starch (being the irradiation pueraria starch);
2) mechanically mixing: the add-on by acrylamide is 60% of an irradiated starch quality, and the add-on of deionized water is 120% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 25min down, obtain mixture in normal temperature;
3) graft polymerization: the mixture that stirs is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 80 ℃ of conditions, heat 40min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 60 ℃ of following vacuum-drying 2h, be crushed to 125 orders, percentage of grafting is the flocculation starch of 49.8% graft acrylamide.
This graft acrylamide flocculation starch is used for the processing of active dye wastewater, and settling velocity is less than 12s, gets transmittance that supernatant liquid records behind the 15min greater than 88%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 3:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: tapioca (flour) is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 8KGy, makes described tapioca (flour) produce free radical, obtains irradiated starch (being the irradiation tapioca (flour));
2) mechanically mixing: the add-on by acrylamide is 70% of an irradiated starch quality, and the add-on of deionized water is 150% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 30min down, obtain mixture in normal temperature;
3) graft polymerization: the mixture that stirs is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 70 ℃ of conditions, heat 50min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 50 ℃ of following vacuum-drying 3h, be crushed to 400 orders, percentage of grafting is the flocculation starch of 59.5% graft acrylamide.
This graft acrylamide flocculation starch is used for the processing of sanitary wastewater cupric ion, and settling velocity is less than 20s, gets transmittance that supernatant liquid records behind the 15min greater than 80%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 4:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: yam starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 10KGy, makes described yam starch produce free radical, obtains irradiated starch (being the irradiation yam starch);
2) mechanically mixing: the add-on by acrylamide is 100% of an irradiated starch quality, and the add-on of deionized water is 150% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 30min down, obtain mixture in normal temperature;
3) graft polymerization: the mixture that stirs is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 90 ℃ of conditions, heat 20min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 60 ℃ of following vacuum-drying 2h, be crushed to 125 orders, percentage of grafting is the flocculation starch of 92.2% graft acrylamide.
This graft acrylamide flocculation starch is used for the processing of kaolin suspension liquid, and settling velocity is less than 10s, gets transmittance that supernatant liquid records behind the 15min greater than 90%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 5:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: wheat starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 4KGy, makes described wheat starch produce free radical, obtains irradiated starch (being the irradiation wheat starch);
2) mechanically mixing: the add-on by acrylamide is 50% of an irradiated starch quality, and the add-on of deionized water is 100% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 10min down, obtain mixture in normal temperature;
3) graft polymerization: mixture is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 60 ℃ of conditions, heat 10min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 40 ℃ of following vacuum-drying 3h, be crushed to 200 orders, percentage of grafting is the flocculation starch of 85.3% graft acrylamide.
This graft acrylamide flocculation starch is used for the processing of acid blue dye, and settling velocity is less than 14s, gets transmittance that supernatant liquid records behind the 15min greater than 85%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 6:
A kind of preparation method of flocculation starch of graft acrylamide, it comprises the steps:
1) physics causes: sorghum starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 30KGy, makes described sorghum starch produce free radical, obtains irradiated starch (being the irradiation sorghum starch);
2) mechanically mixing: the add-on by acrylamide is 100% of an irradiated starch quality, and the add-on of deionized water is 200% of an irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 30min down, obtain mixture in normal temperature;
3) graft polymerization: mixture is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 100 ℃ of conditions, heat 60min; Heat while stirring; Carry out graft polymerization reaction; Then with products therefrom with deionized water wash, at 55 ℃ of following vacuum-drying 2h, be crushed to 400 orders, percentage of grafting is the flocculation starch of 80.5% graft acrylamide.
This graft acrylamide flocculation starch is used for the processing of sanitary wastewater hexavalent chromium, and settling velocity is less than 15s, gets transmittance that supernatant liquid records behind the 15min greater than 80%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 7:
Basic identical with embodiment 1, difference is: W-Gum substitutes with wheat starch.
Resulting flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 15s, gets transmittance that supernatant liquid records behind the 15min greater than 85%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 8:
Basic identical with embodiment 1, difference is: W-Gum substitutes with Starch rice.
Resulting flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 15s, gets transmittance that supernatant liquid records behind the 15min greater than 85%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Embodiment 9:
Basic identical with embodiment 1, difference is: W-Gum substitutes with sweet potato starch.
Resulting flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 15s, gets transmittance that supernatant liquid records behind the 15min greater than 85%.It is fast that the flocculation starch that present embodiment preparation is described has settling velocity, and effect of settling is good, the segregative characteristics of product.
Each raw material that the present invention is cited and the bound value of each raw material, and the bound value of each processing parameter can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (3)
1. the preparation method of the flocculation starch of a graft acrylamide is characterized in that it comprises the steps:
1) physics causes: starch is sent into
60In the Co-gamma-rays radiation field, under atmospheric environment, carry out irradiation, radiation dose is 4-30KGy, makes described starch produce free radical, obtains irradiated starch;
2) mechanically mixing: the add-on by acrylamide is the 50%-100% of irradiated starch quality, and the add-on of deionized water is the 100%-200% of irradiated starch quality, chooses irradiated starch, acrylamide and deionized water; Irradiated starch, acrylamide and deionized water are placed mixing tank, stir 10-30min down, obtain mixture in normal temperature;
3) graft polymerization: mixture is placed heat collecting type thermostatically heating magnetic stirring apparatus; Under 60-100 ℃ of condition, heat 10-60min, heat while stirring, carry out graft polymerization reaction; Then with products therefrom with deionized water wash, drying, pulverizing, the flocculation starch of graft acrylamide.
2. the preparation method of the flocculation starch of a kind of graft acrylamide according to claim 1, it is characterized in that: described starch is W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch or sweet potato starch.
3. the preparation method of the flocculation starch of a kind of graft acrylamide according to claim 1 is characterized in that: described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation for the loading of source amount.
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| CN107151291A (en) * | 2017-07-11 | 2017-09-12 | 武汉纺织大学 | A kind of technique of utilization dry production graft starch |
| CN107334144A (en) * | 2017-08-01 | 2017-11-10 | 肥西县金桥红薯专业合作社 | A kind of processing method of anti-mildew bean vermicelli |
| CN109912745A (en) * | 2019-03-27 | 2019-06-21 | 湖北顶新环保生物质材料有限公司 | A kind of starch-based composite flocculant and its preparation method and application |
| CN112375181A (en) * | 2020-11-03 | 2021-02-19 | 天津工业大学 | Starch ion exchange resin with carboxyl and preparation method and application thereof |
| CN113480082A (en) * | 2021-04-25 | 2021-10-08 | 内蒙古东华能源有限责任公司 | Environment-friendly process for treating coal chemical industry sewage |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107151291A (en) * | 2017-07-11 | 2017-09-12 | 武汉纺织大学 | A kind of technique of utilization dry production graft starch |
| CN107334144A (en) * | 2017-08-01 | 2017-11-10 | 肥西县金桥红薯专业合作社 | A kind of processing method of anti-mildew bean vermicelli |
| CN109912745A (en) * | 2019-03-27 | 2019-06-21 | 湖北顶新环保生物质材料有限公司 | A kind of starch-based composite flocculant and its preparation method and application |
| CN112375181A (en) * | 2020-11-03 | 2021-02-19 | 天津工业大学 | Starch ion exchange resin with carboxyl and preparation method and application thereof |
| CN112375181B (en) * | 2020-11-03 | 2022-07-19 | 天津工业大学 | Starch ion exchange resin with carboxyl and preparation method and application thereof |
| CN113480082A (en) * | 2021-04-25 | 2021-10-08 | 内蒙古东华能源有限责任公司 | Environment-friendly process for treating coal chemical industry sewage |
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Application publication date: 20120215 |