CN105061675A - Starch flocculant, preparation method and applications thereof - Google Patents
Starch flocculant, preparation method and applications thereof Download PDFInfo
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- CN105061675A CN105061675A CN201510127194.6A CN201510127194A CN105061675A CN 105061675 A CN105061675 A CN 105061675A CN 201510127194 A CN201510127194 A CN 201510127194A CN 105061675 A CN105061675 A CN 105061675A
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Abstract
The present invention discloses a starch flocculant, a preparation method and applications thereof, wherein starch and acrylamide are subjected to graft copolymerization to obtain the starch flocculant, the starch is pea starch, glutinous rice starch, corn starch, potato starch and sweet potato starch, preferably pea starch, and a mass ratio of the starch to the acrylamide is 1:1-1:3. According to the present invention, the starch flocculant has characteristics of low cost, green environmental protection and good flocculation effect, and is especially suitable for coal mine wastewater treatment.
Description
Technical field
The present invention relates to a kind of starch flocculant and its preparation method and application.
Background technology
In recent years, environment protection and quality of life cause people and pay close attention to greatly.It is reported, within 2012, China's discharged volume of industrial waste water is 221.6 hundred million tons, and " water resources is craved for by China " report that the Dow Chemical Company issues the same period is pointed out, the repeating utilization factor of Chinese industrial water resources is only 25%.Be waste-water from coal mine greatly in trade effluent, be often only these waste water of process and just need a large amount of flocculation agents.The a variety of flocculation agent for waste-water from coal mine process in the market, as traditional alite, copolymerization aluminum chloride, polyacrylamide, they are easy to cause secondary pollution and can not meet now for the requirement of waste-water from coal mine process.Although the flocculation agent of W-Gum, yam starch, glutinous rice starch modification has also applied waste-water from coal mine process, because amylose content in them is not high, make its water treatment effect not good.
Summary of the invention
In order to overcome the purifying water effect difference of existing flocculation agent existence and have secondary pollution problems, the present invention has better effect of settling and acrylamide and starch quality proportioning, temperature of reaction according to the graft copolymer of amylose starch and has impact to percentage of grafting, by a large amount of theories and cut-and-try work, different types of starch, acrylamide and starch quality proportioning, temperature of reaction are studied, have developed the flocculation agent being suitable for purifying waste-water from coal mine.
Implementation procedure of the present invention is as follows:
A kind of starch flocculant, obtained by starch and acrylic amide graft copolymerization, described starch is pea starch, glutinous rice starch, W-Gum, yam starch, sweet potato starch, is preferably as pea starch.The mass ratio of described starch and acrylamide is 1:1 ~ 1:3, and preferred mass is than being 1:2.
A preparation method for starch flocculant, it is obtained by starch and acrylic amide graft copolymerization, and described starch is pea starch, and the mass ratio of pea starch and acrylamide is 1:1 ~ 1:3, and temperature of reaction is 50 ~ 70 DEG C.
Starch flocculant of the present invention can be used for processing waste-water from coal mine, and during use, the add-on of flocculation agent is 35 ~ 80mg/L, and applicable pH scope is 3-11.
The present invention is with low cost, environmental protection, and flocculating effect is good, is particularly suitable for processing waste-water from coal mine.
Accompanying drawing explanation
Fig. 1 is the water treatment efficiency contrast of various different Starch synthesis flocculation agent;
Fig. 2 is the SEM before and after pea starch synthetic flocculant;
Fig. 3 is the pea starch of synthetic flocculant and the relation of AM quality proportioning and process waste-water from coal mine effect;
When Fig. 4 is synthetic flocculant, temperature of reaction is on the impact of process waste-water from coal mine transmittance;
Fig. 5 is that the dosage of novel flocculant is on the impact of process waste-water from coal mine transmittance;
Fig. 6 is the contrast of novel flocculant and polyacrylamide (PAM) water treatment efficiency;
Fig. 7 is the different pH impact on the flocculation agent process waste-water from coal mine effect of synthesis.
Embodiment
Embodiment 1: different starch conversion is on the impact of flocculation agent effect
1,500mL three-necked flask polytetrafluoroethylmixer mixer, reflux condensing tube being housed and being connected with carbonic acid gas is placed in thermostat water bath, opens thermostat water bath, bath temperature water-bath is set to 60 DEG C;
2, the 5g pea starch weighed up and 100mL dehydrated alcohol are added three-necked flask, pass into carbonic acid gas and drain air in three-necked flask, open agitator, start timing.Starch pasting is after 1 hour, adds 0.24gNaOH, 10gAM monomer and initiator toward three-necked flask, passes into carbonic acid gas and drains air in three-necked flask, carry out graft copolymerization, obtain cationic starch flocculant;
3, colloidal product is placed constant temperature, with washing with acetone several, filter, be placed in thermostatic drying chamber inner drying, after drying terminates, loaded reagent bag, and labelled, and label is 1;
4, glutinous rice starch, W-Gum, yam starch, sweet potato starch replace pea starch, repeating step 2 and step 3, the product code numbering 2,3,4,5 obtained;
5, take out the volumetric flask distilled water wash clean of 5 50ml and numbering 1,2,3,4,5, get the solution that above-mentioned five kinds of starch flocculant products are made into 0.1%;
6, take out the beaker distilled water wash clean of 5 50ml and numbering 1,2,3,4,5, pour 20ml colliery water sample into, get the solution that 1mL prepares respectively and add in the water of colliery, stir 1min, leave standstill 15min;
7, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 5 beaker supernatant liquids, to add 5 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 1.
Visible, at identical conditions, the effect of the copolymerization product process waste-water from coal mine of pea starch and AM is best.
Embodiment 2:
The flocculation agent of pea starch and obtained pea starch modification is done scanning electron microscope respectively, and scanning result is shown in Fig. 2.After can finding out grafting by scanning electron microscope, the structure of pea starch there occurs change really, and this illustrates that pea starch modified flocculant synthesizes successfully.
Embodiment 3:AM and pea starch quality proportioning are on the impact of flocculation agent effect
1,500mL three-necked flask polytetrafluoroethylmixer mixer, reflux condensing tube being housed and being connected with carbonic acid gas is placed in thermostat water bath.Open thermostat water bath, bath temperature water-bath is set to 60 DEG C;
2, the 5g pea starch weighed up and 100mL dehydrated alcohol are added three-necked flask, pass into carbonic acid gas and drain air in three-necked flask, open agitator, start timing.Starch pasting is after 1 hour, adds AM monomer and the initiator of 0.24gNaOH, 5g toward three-necked flask, passes into carbonic acid gas and drains air in three-necked flask, carry out graft copolymerization, obtain cationic starch flocculant;
3, colloidal product is placed constant temperature, with washing with acetone several, filter, be placed in thermostatic drying chamber inner drying, after drying terminates, loaded reagent bag, and labelled 1;
4, use the pea starch of 5g to react with the acrylamide (AM) of 7.5g, 10g, 12.5g, 15g respectively again, repeating step 2 and step 3, by the product code numbering 2,3,4,5 obtained;
5, take out the volumetric flask distilled water wash clean of 50ml and numbering 1,2,3,4,5, get the solution that above-mentioned five kinds of starch flocculant products are made into 0.1%;
6, take out the beaker distilled water wash clean of 5 50ml and numbering 1,2,3,4,5, pour 20ml colliery water sample into, get the solution that 1mL prepares respectively and add in the water of colliery, stir 1min, leave standstill 15min;
7, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 5 beaker supernatant liquids, to add 5 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 3.
Conclusion: at identical conditions, when pea starch and AM mass ratio are 1 ~ 3, synthetic product is good to the treatment effect of waste-water from coal mine.
Embodiment 4: temperature of reaction is on the impact of flocculation agent effect
1,500mL three-necked flask polytetrafluoroethylmixer mixer, reflux condensing tube being housed and being connected with carbonic acid gas is placed in thermostat water bath.Open thermostat water bath, bath temperature water-bath is set to 60 DEG C;
2, the 5g pea starch weighed up and 100mL dehydrated alcohol are added three-necked flask, pass into carbonic acid gas and drain air in three-necked flask, open agitator, start timing.Starch pasting is after 1 hour, adds 0.24gNaOH, 10gAM monomer and initiator toward three-necked flask, passes into carbonic acid gas and drains air in three-necked flask, carry out graft copolymerization, obtain cationic starch flocculant;
3, colloidal product is placed constant temperature, with washing with acetone several, filter, be placed in thermostatic drying chamber inner drying, after drying terminates, loaded reagent bag, and labelled 1;
4, respectively under 63 DEG C, 65 DEG C, 68 DEG C, 70 DEG C temperature of reaction, repeating step 2 and step 3, by the product code numbering 2,3,4,5 obtained;
5, take out the volumetric flask distilled water wash clean of 50ml and numbering 1,2,3,4,5, get the solution that above-mentioned five kinds of starch flocculant products are made into 0.1%;
6, take out the beaker distilled water wash clean of 5 50ml and numbering 1,2,3,4,5, pour 20ml colliery water sample into, get the solution that 1mL prepares respectively and add in the water of colliery, stir 1min, leave standstill 15min;
7, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 5 beaker supernatant liquids, to add 5 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 4.
Conclusion: at identical conditions, pea starch and AM temperature of reaction are 50 ~ 70 DEG C, and the flocculation agent of synthesis is good to the treatment effect of waste-water from coal mine, and during best treatment effect, transmittance is about 91%.
Embodiment 5: to the determination of flocculant dosage
1, get the volumetric flask of 1 50ml, clean with distilled water, be 1:2 by pea starch and AM quality proportioning, the starch flocculant reacting generation at 65 DEG C is made into the solution of 0.1%;
2, take out the beaker distilled water wash clean of 5 50ml and numbering 1,2,3,4,5, pour 20ml colliery water sample into, add different dose (20mg/L respectively, 40mg/L, 60mg/L, 80mg/L, above-mentioned starch flocculant solution 100mg/L), stirs 1min, leaves standstill 15min;
3, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 5 beaker supernatant liquids, to add 5 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 5.
Conclusion: at identical conditions, dosage is 40mg in 40mg/L(and 1L waste-water from coal mine flocculation agent usage quantity) below time, transmittance increases gradually with the increase of dosage, during more than 40mg/L, transmittance is substantially constant, consider the factors such as cost benefit, the optimum add-on choosing flocculation agent is 20 ~ 80mg/L.
Embodiment 6: the contrast of novel flocculant and PAM effect
1, get the volumetric flask of 2 50ml, clean with distilled water, novel flocculant and PAM are made into respectively the solution of 0.1%;
2, take out the beaker distilled water wash clean of 10 50ml and numbering 1,2,3,4,5,6,7,8,9,10, pour 20ml colliery water sample into, in 1-5 beaker, add different amount (20mg/L, 40mg/L, 60mg/L, 80mg/L, novel flocculation agent solution 100mg/L), different amount (20mg/L, 40mg/L, 60mg/L is added in 6-10 beaker, 80mg/L, PAM solution 100mg/L), stirs 1min, leaves standstill 15min;
3, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 10 beaker supernatant liquids, to add 10 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 6.
Conclusion: at identical conditions, when dosage is greater than 35mg/L, the successful that novel flocculant is disposed of sewage is better than PAM.
Embodiment 7:pH is on the impact of flocculation agent effect
1, take out the beaker distilled water wash clean of 6 50ml and numbering 1,2,3,4,5,6, pour 20ml colliery water sample into, and by wastewater pH furnishing 2,4,6,8,10,12 respectively, add novel flocculant and the PAC of optimum quantity, stir 1min, leave standstill 15min;
2, take out the beaker distilled water wash clean of 6 50ml and numbering 7,8,9,10,11,12, pour 20ml colliery water sample into, and by wastewater pH furnishing 2,4,6,8,10,12 respectively, add PAM and PAC of optimum quantity, stir 1min, leave standstill 15min;
3, by after spectrophotometer preheating 15min, wavelength is placed in 610nm position.Getting 12 beaker supernatant liquids, to add 12 specifications be in the cleaned glass cuvette of 722, opens the above-mentioned sample of sample chamber goalkeeper and put into sample pool, take distilled water as contrast, measures the transmittance of supernatant liquid and record data, see Fig. 7.
Conclusion: novel flocculant processes the better effects if of waste water compared with PAM, to the pH strong adaptability of waste water.
Claims (9)
1. a starch flocculant, is characterized in that: obtained by starch and acrylic amide graft copolymerization.
2. starch flocculant according to claim 1, is characterized in that: described starch is pea starch, glutinous rice starch, W-Gum, yam starch or sweet potato starch.
3. starch flocculant according to claim 2, is characterized in that: described starch is pea starch.
4. starch flocculant according to claim 3, is characterized in that: the mass ratio of described starch and acrylamide is 1:1 ~ 1:3.
5. starch flocculant according to claim 4, is characterized in that: the mass ratio of described starch and acrylamide is 1:2.
6. the preparation method of starch flocculant described in claim 1, is characterized in that: obtained by starch and acrylic amide graft copolymerization.
7. the preparation method of starch flocculant according to claim 6, it is characterized in that: described starch is pea starch, the mass ratio of pea starch and acrylamide is 1:1 ~ 1:3, and temperature of reaction is 50 ~ 70 DEG C.
8. the application of starch flocculant described in claim 1 in process waste-water from coal mine.
9. apply according to claim 8, it is characterized in that: the add-on of flocculation agent is 35 ~ 80mg/L, and applicable pH scope is 3-11.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108675426A (en) * | 2018-05-08 | 2018-10-19 | 西北大学 | A kind of flocculant and its preparation method and application based on poly- amidine |
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