CN108658199A - Polyferric Sulfate-cornstarch graft composite flocculant and its preparation method and application - Google Patents
Polyferric Sulfate-cornstarch graft composite flocculant and its preparation method and application Download PDFInfo
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- CN108658199A CN108658199A CN201810415048.7A CN201810415048A CN108658199A CN 108658199 A CN108658199 A CN 108658199A CN 201810415048 A CN201810415048 A CN 201810415048A CN 108658199 A CN108658199 A CN 108658199A
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- polyferric sulfate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The present invention relates to a kind of Polyferric Sulfate cornstarch graft composite flocculants and its preparation method and application, specifically using cornstarch as raw material, after oxidation-treated respectively with styrene, acrylic amide graft copolymerization, it is compounded by graft obtained and by the Polyferric Sulfate of Material synthesis of ferrous sulfate heptahydrate, and is used for raw water and sewage disposal.The present invention is by comparative study ferric trichloride, the flocculating property of Polyferric Sulfate, maize oxidized starch styrene-grafted object, maize oxidized starch acrylamide graft object and composite flocculant, prove the compound product of Polyferric Sulfate and the maize oxidized starch graft of grafting rate 100~200, there is better treatment effect to raw water and sanitary sewage, dosage range is big, sinking speed is fast, there is stronger adaptability to acid-base value variation, is a kind of flocculant of broad-spectrum high efficacy.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of Polyferric Sulfate-compound wadding of cornstarch graft
Solidifying agent and its preparation method and application.
Background technology
Flocculation is raw water and the important link of sewage disposal, and common inorganic flocculating agent has aluminium salt, molysite and kaolin etc.；
Organic flocculant is organic high molecular compound, such as polyacrylamide, maleic acid aggressiveness salt mostly.Polyferric flocculant, again
Claim glue bodied ferric sulfate, be a kind of slag high price iron macromolecular inorganic polymer, there is stronger temperature and pH adaptability, water
It is smaller to solve product iron hydroxide solubility, does not influence the transparency of water within the scope of larger dosage, therefore have in water treatment field
There is good application prospect.However, polyferric flocculant, when dosage is 40.0mgL-1When, it can only to the COD removal rates of raw water
Up to 75.6%, concentration of suspension is up to 1.3mgL-1。
Cornstarch is natural biodegradable polymer compound, has the characteristics that large specific surface area, may modify, thus is being had
It is used widely in the synthesis of machine high molecular material.Therefore, we synthesize some cornstarch graft products, and wad a quilt with cotton with Polyferric Sulfate
Solidifying agent compounding, makes the absorption property of the two generate collaboration, is desirably to obtain a kind of higher compound wadding of the COD removal rates to raw water
Solidifying agent.
Invention content
The object of the present invention is to provide a kind of Polyferric Sulfate-cornstarch graft composite flocculants.
It is a further object of the present invention to provide a kind of preparation methods of Polyferric Sulfate-cornstarch graft composite flocculant.
It is a further object of the present invention to provide a kind of Polyferric Sulfate-cornstarch graft composite flocculants in raw water and sewage
Application in processing.
The technical solution adopted by the present invention is：A kind of Polyferric Sulfate-cornstarch graft composite flocculant, with cornstarch
For raw material, oxidation-treated rear and graft copolymerization monomer graft copolymerization, by graft copolymer obtained and with ferrous sulfate heptahydrate
It compounds to obtain for the polyferric flocculant of Material synthesis.
A kind of preparation method of Polyferric Sulfate-cornstarch graft composite flocculant, specifically comprises the following steps：
Step 1：The oxidation of cornstarch：Cornstarch and deionized water are pressed 1：1.5-1：2 solid-liquid mass ratio mixing
After be beaten, add hydrogen peroxide oxidation 30-40min, obtain maize oxidized starch；
The preparation of step 2, maize oxidized starch graft copolymer：Emulsification is added in step 1 gained maize oxidized starch
Agent is added initiator, reacts 1.5-2h under reflux conditions for the first time after stirring evenly, graft copolymerization monomer, the is then added
Secondary addition initiator is warming up to 88-90 DEG C, reacts 0.5-1h, and cooling, filtering, drying obtain maize oxidized starch graft copolymerization
Object；
The preparation of step 3, Polyferric Sulfate-cornstarch graft composite flocculant：Step 2 gained maize oxidized starch is connect
Graft copolymer is with polyferric flocculant with 1:1-1:1.5 mass ratio is compounded, and target product is obtained.
Further, in the step 1, the mass concentration of hydrogen peroxide is 10-12%, and the addition of hydrogen peroxide is formed sediment for corn
The 0.05-0.1 of silty amount.
Further, in the step 2, emulsifier uses OP-10, and the addition of emulsifier is cornstarch quality
0.01-0.015。
Further, in the step 2, graft copolymerization monomer is styrene or acrylamide.
Further, in the step 2, when graft copolymerization monomer is styrene, initiator uses potassium peroxydisulfate or over cure
Sour ammonium.
Further, in the step 2, when graft copolymerization monomer is acrylamide, initiator uses ammonium ceric nitrate.
Further, in the step 2, the amount that initiator is added for the first time is graft copolymerization monomer molar amount
0.0025-0.003 times；The amount of second of addition initiator is 0.0025-0.002 times of graft copolymerization monomer molar amount.
Beneficial effects of the present invention are：Using cheap molysite as polyferric flocculant made from raw material and grafting rate in the present invention
It is appropriate that maize oxidized starch-phenylethene grafted copolymer, the maize oxidized starch-acrylamide grafted copolymer of 100-200 is pressed
The composite flocculant that ratio compounds has preferable treatment effect to raw water and sanitary sewage, has amount ranges big,
Sedimentation is fast, has the characteristics that preferable processing capacity to the sewage within the scope of pH4-7, is a kind of flocculant of broad-spectrum high efficacy, has
There is preferable application prospect.
Description of the drawings
Fig. 1 is that Polyferric Sulfate-maize oxidized starch graft composite flocculant graft copolymerization monomer is styrene infared spectrum；
Fig. 2 is that Polyferric Sulfate-maize oxidized starch graft composite flocculant graft copolymerization monomer is the infrared figure of acrylamide
Spectrum；
Fig. 3 is influence of the grafting rate to treatment effect；
Fig. 4 is influence of the dosage to treatment effect；
Fig. 5 is influence of the raw water pH value to treatment effect；
Fig. 6 is influence of the sedimentation time to treatment effect.
Specific implementation mode
Below by specific embodiment to composite flocculant of the present invention and preparation method thereof and for raw water and sewage
Treatment effect is described in further detail.
Embodiment 1
Graft copolymerization monomer is styrene
A kind of preparation method of Polyferric Sulfate-cornstarch graft composite flocculant, includes the following steps：
The oxidation of step 1, cornstarch：In four-hole boiling flask, 40ml deionized waters and 30g cornstarch, mashing is added
The hydrogen peroxide 2.7ml that 10% is added afterwards aoxidizes 30min, obtains maize oxidized starch；
The preparation of step 2, maize oxidized starch graft copolymer styrenic graft：It aoxidizes and forms sediment in step 1 gained corn
2mlOP-10 emulsifiers are added in powder, 0.2g initiator potassium persulfates are added after stirring evenly for the first time, are reacted under counterflow condition
60ml styrene is added dropwise after 1.5h, 0.1g initiator potassium persulfates are added for the second time, reacts 1h under counterflow condition, is warming up to 88
DEG C, react 0.5h, cooling, filtering, dry finished product.
The synthesis of step 3, polyferric flocculant：100ml ferrous sulfate solutions are added into three-necked flask, are heated to 50 DEG C,
It is slowly added to the concentrated sulfuric acid of 8ml 98%, a small amount of catalyst mistake is added in the hydrogen peroxide of 70 DEG C of addition 8ml 30% after being sufficiently stirred
Ammonium sulfate is warming up to 85-90 DEG C and oxidation, polymerisation occurs, until pH=2.0-3.0, iron concentration is more than 165gL-1When
Cool down, settle thick liquid is product.
The preparation of step 4, Polyferric Sulfate-cornstarch graft composite flocculant：Step 3 gained polyferric flocculant 15g is taken,
Step 2 gained maize oxidized starch graft copolymer styrenic graft 10g, is sufficiently mixed compounding, obtains product.It is denoted as compound
Flocculant I.
Embodiment 2
Graft copolymerization monomer is acrylamide
A kind of preparation method of Polyferric Sulfate-cornstarch graft composite flocculant, includes the following steps：
The oxidation of step 1, cornstarch：In four-hole boiling flask, 40ml deionized waters and 30g cornstarch, mashing is added
The hydrogen peroxide 2.7ml that 10% is added afterwards aoxidizes 30min, obtains maize oxidized starch；
The preparation of step 2, maize oxidized starch graft copolymer acrylamide graft object：It is aoxidized in step 1 gained corn
2mlOP-10 emulsifiers are added in starch, 0.2g initiator ammonium ceric nitrates are added after stirring evenly for the first time, it is anti-under counterflow condition
60ml acrylamides are added dropwise after answering 2h, 0.1g ammonium ceric nitrates are added for the second time, are warming up to 90 DEG C, react 1h, cooling, filtering is done
It is dry to obtain finished product；
The synthesis of step 3, polyferric flocculant：With embodiment 1；
The preparation of step 4, Polyferric Sulfate-cornstarch graft composite flocculant：Step 3 gained polyferric flocculant 15g is taken,
Step 2 gained maize oxidized starch graft copolymer acrylamide graft object 10g, is sufficiently mixed compounding, obtains product.It is denoted as compound
Type flocculant II.
Embodiment 3, Polyferric Sulfate-processing of the cornstarch graft composite flocculant to raw water and sewage
Test sewage：It is derived from activated sludge in Yanerwan sewage plant sewage treatment plant, pH value 5.62, light transmittance 21.5%, COD816mg
L-1。
Flocculating experiment：In 1L beakers, flocculating agent formulation is added at solution in sewage, 150rmin-12min is stirred,
After mixing completely, it is reduced to 50rmin-15min is stirred, is stood, takes supernatant at 3cm under liquid level, is sampled 3 times, test waves
Light transmittance when long 500nm and COD, are averaged.
It is 40mgL in flocculant concentration-1, comparative study difference flocculant is measured under the conditions of pH=6 to sanitary sewage
Treatment effect the results are shown in Table 1.
Comparison of the different flocculants of table 1 to processing sanitary sewage
Composite flocculant has obvious effects on the removal rate of COD, the raising of light transmittance as shown in Table 1.Polyferric Sulfate flocculates
Agent is a kind of alkali high price iron macromolecule polyalcohol, can be miscible rapidly with arbitrary proportion with water, forms a large amount of complexing in water
Ion, these complex ions can quickly neutralize the charge on suspended matter surface, reduce its current potential, at the same Polyferric Sulfate build bridge to be formed it is more
Core complex ion and high polymer coagulant play crosslinking, package and bridging action jointly, form solid sedimented particle, and it is heavy to reduce
The time is dropped, the capacity of outlet water of water purification is improved.
Two, the structural characterization of Polyferric Sulfate-cornstarch graft composite flocculant
1, infared spectrum is analyzed
Fig. 1 is that Polyferric Sulfate-maize oxidized starch graft composite flocculant graft copolymerization monomer is styrene infared spectrum；
By Fig. 1 it can be found that：3400cm-1Nearby there are the characteristic absorption peak-OH stretching vibration characteristic peaks of starch；3030cm-1Nearby go out
The C-H stretching vibration absworption peaks of the existing intensity phenyl ring slightly weaker than the C-H of saturation；2000-1660cm-1There is quantity 2-6 in range
One group of absorption band, be the distinctive wavy absorption of phenyl ring；1600-1500cm-1There is phenyl ring C=C skeletal vibration absorption peaks, table in place
Graft copolymerization has occurred with oxidized starch in bright styrene.
Fig. 2 is that Polyferric Sulfate-maize oxidized starch graft composite flocculant graft copolymerization monomer is the infrared figure of acrylamide
Spectrum；1667cm-1Nearby there is the stretching vibration absworption peak of C=O in amide groups；3421cm-1The stretching vibration of nearby-OH absorbs
The area at peak obviously becomes smaller, 1030-1050cm-1Absorption intensity weaken, and 1022cm-1The absorption intensity at place enhances, and illustrates third
Hydrogen bond, which destroys, after acrylamide grafting increases, and crystallization degree reduces, and amorphous structure increases.Infrared spectrum analysis table more than
Graft reaction, modification of corn starch success has occurred in bright cornstarch and acrylamide.
2, the calculating of grafting rate
The solubility of Starch graft copolymer coal-water and grafting rate are the principal elements for influencing water treatment efficiency in flocculant.It is starch-grafted
The solubility of object is related with cornstarch degree of oxidation, and degree of oxidation is controlled with carboxyl-content.When carboxyl-content be 0.50%,
Under the conditions of pH=6, flocculant concentration 40.0mgL-1When, Fig. 3 is shown in influence of the grafting rate to the treatment effect of raw water.It can see
Go out, when grafting rate is relatively low, treatment effect enhancing is increased with grafting rate, reaching certain value post-processing effect reduces.This is because wadding
It is solidifying to rely primarily on absorption, bridge formation and crosslinked action and have the function that remove pollutant, graft activity when grafting rate is relatively low
Greatly, Swelling Capacity is strong, and solubility, activity, Swelling Capacity substantially reduce when grafting rate is high, and treatment effect declines, therefore grafting rate
It is advisable for 100-200, and the Polyferric Sulfate that graft copolymerization monomer is acrylamide-maize oxidized starch graft composite flocculant wadding
Solidifying effect is slightly above Polyferric Sulfate-maize oxidized starch graft composite flocculant that graft copolymerization monomer is styrene.
The thick grafted products for being dried under vacuum to constant weight are placed in soxhlet's extractor, using acetone as extractant reflux 48h, extraction
It takes to constant weight, removes homopolymer, insoluble matter is dried in vacuo, pure graft is obtained.By infrared spectrum, grafting rate is calculated as follows
(G%)：
Grafting rate=[(pure graft quality-starch quality)/starch quality] × 100%.As a result：The jade of above-mentioned preparation
The grafting rate of rice oxidized starch-acrylamide grafted copolymer or maize oxidized starch-phenylethene grafted copolymer is reachable
100-200。
Three, application of the Polyferric Sulfate-cornstarch graft composite flocculant in handling raw water
Maize oxidized starch graft copolymer styrenic graft, the maize oxidized starch that will be synthesized under optimum process condition
Graft copolymer acrylamide graft object, polyferric flocculant, Polyferric Sulfate-cornstarch graft composite flocculant, are most preferably matching
Than under the conditions of, various flocculants are further compared under the conditions of different dosages, different pH values to raw water or sanitary sewage
Treatment effect and at optimum conditions sedimentation, separating effect.
Fig. 4 is influence of the dosage to treatment effect.As shown in Figure 4, using maize oxidized starch graft copolymer styrenic
Graft, maize oxidized starch graft copolymer acrylamide graft object increase light transmittance with dosage and increase, but increase to certain
Light transmittance gradually becomes smaller after value；Ferric trichloride flocculant process effect is weaker than other, and effect reduces instead when dosage increases,
Light transmittance can also be reduced by being primarily due to iron ion；Polyferric flocculant optimization process effect not as good as organic polymer coargulator, but
It is slightly improved with dosage increase, illustrates that its amount ranges is larger；Composite flocculant taken into account organic polymer coargulator and
The characteristics of inorganic polymer flocculant, treatment effect is apparent, and amount ranges are big.
Fig. 5 is influence of the raw water pH value to treatment effect.As shown in Figure 5, maize oxidized starch graft copolymer styrenic
Graft, maize oxidized starch graft copolymer acrylamide graft object, ferric trichloride flocculant are affected by raw water pH；
Polyferric flocculant, composite flocculant are influenced smaller by pH, all have preferable processing energy to the sewage within the scope of pH=4-7
Power.
Fig. 6 is influence of the sedimentation time to treatment effect.It will be appreciated from fig. 6 that maize oxidized starch graft is with the sedimentation time
Growth, effect of settling improves, that is, settles relatively slow；Polyferric flocculant is than great, and cohesion is fast, and the sedimentation time is short, and processing capacity is strong；
And composite flocculant effect is more preferably.
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its shape or structure, it is every that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (9)
1. a kind of Polyferric Sulfate-cornstarch graft composite flocculant, it is characterised in that：It is oxidized using cornstarch as raw material
After processing and graft copolymerization monomer graft copolymerization, by graft copolymer obtained and using ferrous sulfate heptahydrate as the poly- of Material synthesis
Ferric flocculant compounds to obtain.
2. a kind of preparation method of Polyferric Sulfate prepared in claim 1-cornstarch graft composite flocculant, feature exist
In：Include the following steps：
The oxidation of step 1, cornstarch：Cornstarch and deionized water are pressed 1：1.5-1：It is beaten after 2 solid-liquid mass ratio mixing
Slurry, adds hydrogen peroxide oxidation 30-40min, obtains maize oxidized starch；
The preparation of step 2, maize oxidized starch graft copolymer：Emulsifier is added in step 1 gained maize oxidized starch, stirs
Uniformly rear addition initiator for the first time is mixed, reacts 1.5-2h under reflux conditions, graft copolymerization monomer is then added, adds for second
Enter initiator, be warming up to 88-90 DEG C, react 0.5-1h, cooling, filtering, drying obtain maize oxidized starch graft copolymer；
The preparation of step 3, Polyferric Sulfate-cornstarch graft composite flocculant：Altogether by the grafting of step 2 gained maize oxidized starch
Polymers is with polyferric flocculant with 1:1-1:1.5 mass ratio is compounded, and target product is obtained.
3. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 2
Method：In the step 1, the mass concentration of hydrogen peroxide is 10-12%, and the addition of hydrogen peroxide is cornstarch quality
0.05-0.1。
4. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 2
Method, it is characterised in that：In the step 2, emulsifier uses OP-10, and the addition of emulsifier is cornstarch quality
0.01-0.015。
5. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 2
Method, it is characterised in that：In the step 2, graft copolymerization monomer is styrene or acrylamide.
6. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 5
Method, it is characterised in that：In the step 2, when graft copolymerization monomer is styrene, initiator uses potassium peroxydisulfate or persulfuric acid
Ammonium.
7. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 5
Method, it is characterised in that：In the step 2, when graft copolymerization monomer is acrylamide, initiator uses ammonium ceric nitrate.
8. preparing the preparation of Polyferric Sulfate-cornstarch graft composite flocculant in claim 1 as claimed in claim 2
Method, it is characterised in that：In the step 2, the amount that initiator is added for the first time is the 0.0025- of graft copolymerization monomer molar amount
0.003 times；The amount of second of addition initiator is 0.0025-0.002 times of graft copolymerization monomer molar amount.
9. Polyferric Sulfate as described in claim 1-application of the cornstarch graft composite flocculant in raw water and sewage disposal.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143658A (en) * | 2019-05-15 | 2019-08-20 | 上海理工大学 | A kind of nano-magnetic cationic flocculant and preparation method thereof |
| CN111995029A (en) * | 2020-07-07 | 2020-11-27 | 广西夏阳环保科技有限公司 | Inorganic-natural polymer composite sewage treatment flocculant and preparation method thereof |
| CN115160581A (en) * | 2022-07-05 | 2022-10-11 | 山东鲁抗中和环保科技有限公司 | Preparation method of iron-grafted starch flocculant |
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| JPH06322367A (en) * | 1993-05-11 | 1994-11-22 | Nippon Synthetic Chem Ind Co Ltd:The | Soil property hardener |
| CN101638261A (en) * | 2009-06-13 | 2010-02-03 | 山东国信水处理有限公司 | Starch-based quaternary ammonium salt green flocculant and preparation method |
| CN106335988A (en) * | 2015-07-06 | 2017-01-18 | 迪建东 | Composite high polymer flocculant for coking wastewater and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06322367A (en) * | 1993-05-11 | 1994-11-22 | Nippon Synthetic Chem Ind Co Ltd:The | Soil property hardener |
| CN101638261A (en) * | 2009-06-13 | 2010-02-03 | 山东国信水处理有限公司 | Starch-based quaternary ammonium salt green flocculant and preparation method |
| CN106335988A (en) * | 2015-07-06 | 2017-01-18 | 迪建东 | Composite high polymer flocculant for coking wastewater and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143658A (en) * | 2019-05-15 | 2019-08-20 | 上海理工大学 | A kind of nano-magnetic cationic flocculant and preparation method thereof |
| CN111995029A (en) * | 2020-07-07 | 2020-11-27 | 广西夏阳环保科技有限公司 | Inorganic-natural polymer composite sewage treatment flocculant and preparation method thereof |
| CN115160581A (en) * | 2022-07-05 | 2022-10-11 | 山东鲁抗中和环保科技有限公司 | Preparation method of iron-grafted starch flocculant |
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