CN102211804A - Preparation method of starch-based flocculating agent - Google Patents
Preparation method of starch-based flocculating agent Download PDFInfo
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- CN102211804A CN102211804A CN 201110059248 CN201110059248A CN102211804A CN 102211804 A CN102211804 A CN 102211804A CN 201110059248 CN201110059248 CN 201110059248 CN 201110059248 A CN201110059248 A CN 201110059248A CN 102211804 A CN102211804 A CN 102211804A
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Abstract
The invention relates to a preparation method of a starch-based flocculating agent. The preparation method of the starch-based flocculating agent is characterized by comprising the following steps of: 1) irradiating starch in a 60Co-gamma irradiation field to obtain pre-irradiated starch; 2) putting the pre-irradiated starch and a grafting monomer into a mixer, adding water into the mixer, and starting the mixer to stir so as to obtain a mixture, wherein the added amount of the grafting monomer is 50 to 100 percent of the mass of the pre-irradiated starch, and the mass ratio of the pre-irradiated starch to the water is 1:1-1:3; 3) putting the uniformly stirred mixture into a microwave oven, and applying intermittent microwaves to the mixture for 1 to 3 minutes to ensure that starch free radicals react with active groups on the grafting monomer to generate grafting starch; and 4) baking the grafting starch after microwave treatment for 5 to 10 hours at 80 to 140 DEG C, and crushing to obtain the starch-based flocculating agent. The preparation method is simple in process, less in investment equipment and low in cost, and can obtain a good flocculating effect; besides, a flocculation is easy to separate and does not cause secondary pollution to the environment.
Description
Technical field
The invention belongs to the natural macromolecule flocculating agent technical field, particularly relate to a kind of preparation method of starch base flocculation agent.
Background technology
Along with the quick growth of domestic economy, industrial water consumption constantly increases, and trade effluent also produces in a large number, according to statistics, only calendar year 2001 whole nation industry and urban life wastewater emission amount just are 428.4 hundred million tons, and wherein discharged volume of industrial waste water is 200.7 hundred million tons, accounts for 46.7% of wastewater emission amount.National discharged volume of industrial waste water was 241.7 hundred million tons in 2008, unprocessed rivers,lakes and seas that directly enter of the waste water more than 30% wherein, the utilization of reuse water (sewage is through recovering the water of its functions of use after the purifying treatment) in industry also only is equivalent to 0.4% of water withdrawal.Industrial development to people bring economically growth and material on plentiful the time, also the non-renewable water resources of depending on for existence to the mankind causes huge pressure, and, people's living environment and life security caused great harm without the direct discharging of the sewage of purifying treatment.To become one of main difficult problem that China and even the world faces in from now on several years water supply getses and sewage purification, so the research of the flocculation agent of high-efficiency environment friendly seems particularly important.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of starch base flocculation agent, this method has that technology is simple, investment goods is few, cost is lower, and can obtain good flocculating effect.
For achieving the above object, the technical solution adopted in the present invention is: a kind of preparation method of starch base flocculation agent is characterized in that comprising the following steps:
1) starch is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 4～10KGy, makes starch produce free radical, obtains pre-irradiation starch;
2) add-on by grafted monomer is the 50%-100% of pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water is 1: 1～1: 3, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac (acrylyl oxy-ethyl-trimethyl salmiac is DAC), and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 3: 7～7: 3;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) mixture that stirs is placed microwave oven discontinuous microwave 1～3min (each microwave time is 10～22.5s, 5～15s intermittently, microwave is 4～8 times altogether), make the active group reaction on starch free radical and the grafted monomer, the generation graft starch;
4) graft starch behind the microwave was cured 5～10 hours under 80～140 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
The described starch of step 1) is any one in W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch, the sweet potato starch etc.
Described starch water ratio is 12～16wt%.
Described acrylamide is a kind of white crystal chemical substance, is one of raw material of production water treatment usefulness flocculation agent.
Described acrylyl oxy-ethyl-trimethyl salmiac (Aacryloxyethyltrimethyl Ammonium Chloride) (acrylyl oxy-ethyl-trimethyl salmiac is DAC) is a kind of quaternary ammonium cationic monomer, itself has positive charge, and the negatively charged ion in the water is had very strong adsorption effect.
Described
60Co-γ irradiation field is loading of source amount 400,000 Curie's an industrial dynamic radiation devices, is the concrete chamber of radiation source irradiates sample.
The power of described microwave is 500～1000W.
Natural macromolecule flocculating agent of the present invention is applicable to waste water from dyestuff, petrochemical wastewater, paper waste field of purification.
Beneficial effect of the present invention: 1) utilize radiation-microwave method that natural polymer is carried out physically modified, preparation starch base flocculation agent.This method has that technology is simple, investment goods is few, cost is lower, and can obtain good flocculating effect, and flocculation is easily separated, can not cause secondary pollution to environment.
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 the production efficiency height meets the requirement of green production.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention, should be understood that these examples only are used to the present invention is described and are not used in to limit the scope of the 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.
Embodiment 1:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch (W-Gum) is placed
60In the Co-γ irradiation field, (under at air conditions) carries out irradiation under aerobic conditions, and irradiation dose is 6KGy (radiation dose is fixed, and then the time all is fixed), makes starch produce free radical, obtains pre-irradiation starch; Described starch is W-Gum, viscosity 46mps, water ratio 13.14wt%;
2) add-on by grafted monomer is 100% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water (deionized water) is 1: 1, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac, and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 5: 5;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) (each microwave time is 20s, intermittently 5s the mixture that stirs to be placed microwave oven discontinuous microwave 2.0min; Microwave is 6 times altogether, and the microwave time is 2.0min altogether), make the active group reaction on starch free radical and the grafted monomer, generate graft starch;
4) graft starch behind the microwave was cured 7 hours under 100 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 87.5% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 95.8%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Embodiment 2:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch is placed
60In the Co-γ irradiation field, (under at air conditions) carries out irradiation under aerobic conditions, and irradiation dose is 8KGy, makes starch produce free radical, obtains pre-irradiation starch; Described starch is W-Gum, viscosity 46mps, water ratio 13.14wt%;
2) add-on by grafted monomer is 100% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water (deionized water) is 1: 1.5, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac, and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 5: 5;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) mixture that stirs being placed microwave oven discontinuous microwave 140s[each microwave time is 20s, intermittently 10s; Microwave is 7 times altogether, and the microwave time is 140s (being batch microwave 140s) altogether], make the active group reaction on starch free radical and the grafted monomer, generate graft starch;
4) graft starch behind the microwave was cured 10 hours under 80 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 89.7% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 97.4%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Embodiment 3:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 6KGy, makes starch produce free radical, obtains pre-irradiation starch; Described starch is W-Gum, viscosity 46mps, water ratio 13.14wt%;
2) add-on by grafted monomer is 70% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water (deionized water) is 1: 2, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac, and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 5: 5;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) mixture that stirs being placed microwave oven discontinuous microwave 140s[each microwave time is 20s, intermittently 8s; Microwave is 7 times altogether, and the microwave time is 140s (being batch microwave 140s) altogether], make the active group reaction on starch free radical and the grafted monomer, generate graft starch;
4) graft starch behind the microwave was cured 5 hours under 140 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 86.4% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 95.2%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Embodiment 4:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 10KGy, makes starch produce free radical, obtains pre-irradiation starch; Described starch is W-Gum, viscosity 46mps, water ratio 13.14wt%;
2) add-on by grafted monomer is 100% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water (deionized water) is 1: 2.5, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac, and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 4: 6;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) (each microwave time is 20s, intermittently 5s the mixture that stirs to be placed microwave oven discontinuous microwave 140s; Microwave is 7 times altogether), make the active group reaction on starch free radical and the grafted monomer, generate graft starch;
4) graft starch behind the microwave was cured 10 hours under 140 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 87.7% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 97.9%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Embodiment 5:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch (wheat starch) is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 4KGy, makes starch produce free radical, obtains pre-irradiation starch;
2) add-on by grafted monomer is 50% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water is 1: 1, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac (acrylyl oxy-ethyl-trimethyl salmiac is DAC), and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 3: 7;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) mixture that stirs is placed microwave oven discontinuous microwave 1min (each microwave time is 10s, 5s intermittently, microwave is 6 times altogether), make the active group reaction on starch free radical and the grafted monomer, the generation graft starch;
4) graft starch behind the microwave was cured 5 hours under 80 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 86.0% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 96.0%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Embodiment 6:
A kind of preparation method of starch base flocculation agent comprises the following steps:
1) starch (yam starch) is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 10KGy, makes starch produce free radical, obtains pre-irradiation starch;
2) add-on by grafted monomer is 60% of a pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water is 1: 3, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac (acrylyl oxy-ethyl-trimethyl salmiac is DAC), and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 7: 3;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry (deionized water), the stirring of machining until stirring, obtains mixture;
3) mixture that stirs is placed microwave oven discontinuous microwave 3min (each microwave time is 22.5s, 15s intermittently, microwave is 8 times altogether), make the active group reaction on starch free radical and the grafted monomer, the generation graft starch;
4) graft starch behind the microwave was cured 6 hours under 90 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
Gained starch base flocculation agent is used for the active red dye that concentration of treatment is 200mg/l, and its chroma removal rate can reach 87.0% in 5min, and along with the prolongation of action time, the highest clearance of its colourity can reach 97.0%.Illustrate that the starch base flocculation agent that present embodiment obtains has good flocculating effect.
Other kinds kind of starch also can be realized by the present invention, in this not operation one by one.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 a starch base flocculation agent is characterized in that comprising the following steps:
1) starch is placed
60In the Co-γ irradiation field, carry out irradiation under aerobic conditions, irradiation dose is 4～10KGy, obtains pre-irradiation starch;
2) add-on by grafted monomer is the 50%-100% of pre-irradiation starch quality, chooses pre-irradiation starch and grafted monomer; Mass ratio by pre-irradiation starch and water is 1: 1～1: 3, chooses water; Wherein, grafted monomer is acrylamide and acrylyl oxy-ethyl-trimethyl salmiac, and the mass ratio of acrylamide and acrylyl oxy-ethyl-trimethyl salmiac is 3: 7～7: 3;
Pre-irradiation starch is placed in the mixing tank, grafted monomer is placed in the mixing tank, and add entry, the stirring of machining until stirring, obtains mixture;
3) mixture that stirs is placed microwave oven discontinuous microwave 1～3min, make the active group reaction on starch free radical and the grafted monomer, generate graft starch;
4) graft starch behind the microwave was cured 5～10 hours under 80～140 ℃ of conditions,, obtain the starch base flocculation agent through pulverizing.
2. the preparation method of a kind of starch base flocculation agent according to claim 1 is characterized in that: the described starch of step 1) is any one in W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch, the sweet potato starch.
3. the preparation method of a kind of starch base flocculation agent according to claim 1 is characterized in that described batch microwave: each microwave time is 10～22.5s, 5～15s intermittently, and microwave is 4～8 times altogether.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045649A (en) * | 2013-01-11 | 2013-04-17 | 甘肃农业大学 | Method for preparing microbial flocculant form potato starch wastewater as raw material |
| CN103849010A (en) * | 2014-02-23 | 2014-06-11 | 江苏省农业科学院 | Irradiated corn starch-based biodegradable particles and thin film thereof |
| CN104781196A (en) * | 2012-11-16 | 2015-07-15 | 罗盖特公司 | Potabilization process |
| CN107189015A (en) * | 2017-07-11 | 2017-09-22 | 武汉纺织大学 | A kind of preparation method of non-ionic acrylamide flocculating agent |
| CN109569523A (en) * | 2018-10-27 | 2019-04-05 | 嘉兴珠韵服装有限公司 | The preparation of modified bean pulp adsorbent and the application in treatment of dyeing wastewater |
| CN109880009A (en) * | 2019-03-27 | 2019-06-14 | 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 |
| CN109880010A (en) * | 2019-03-27 | 2019-06-14 | 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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104781196A (en) * | 2012-11-16 | 2015-07-15 | 罗盖特公司 | Potabilization process |
| CN103045649A (en) * | 2013-01-11 | 2013-04-17 | 甘肃农业大学 | Method for preparing microbial flocculant form potato starch wastewater as raw material |
| CN103045649B (en) * | 2013-01-11 | 2014-05-21 | 甘肃农业大学 | Method for preparing microbial flocculant form potato starch wastewater as raw material |
| CN103849010A (en) * | 2014-02-23 | 2014-06-11 | 江苏省农业科学院 | Irradiated corn starch-based biodegradable particles and thin film thereof |
| CN107189015A (en) * | 2017-07-11 | 2017-09-22 | 武汉纺织大学 | A kind of preparation method of non-ionic acrylamide flocculating agent |
| CN109569523A (en) * | 2018-10-27 | 2019-04-05 | 嘉兴珠韵服装有限公司 | The preparation of modified bean pulp adsorbent and the application in treatment of dyeing wastewater |
| CN109880009A (en) * | 2019-03-27 | 2019-06-14 | 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 |
| CN109880010A (en) * | 2019-03-27 | 2019-06-14 | 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 |
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Effective date of registration: 20170527 Address after: 435216, No. 1, Golden Village, Wei Town, Yangxin County, Huangshi City, Hubei Province Patentee after: Hubei new green biomass materials Co. Ltd. Address before: 430073 textile school, No. 1 Textile Road, Hongshan District, Wuhan, Hubei, Wuhan Patentee before: Wuhan Textile University |
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