CN109880009A - A kind of starch-based composite flocculant and its preparation method and application - Google Patents
A kind of starch-based composite flocculant and its preparation method and application Download PDFInfo
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- CN109880009A CN109880009A CN201910239050.8A CN201910239050A CN109880009A CN 109880009 A CN109880009 A CN 109880009A CN 201910239050 A CN201910239050 A CN 201910239050A CN 109880009 A CN109880009 A CN 109880009A
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Abstract
The present invention provides a kind of starch-based composite flocculants and its preparation method and application, are related to technical field of sewage.Starch is carried out radiation treatment with ray by the present invention, obtains irradiated starch；The irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water are mixed, mixture is obtained；The mixture is subjected to twin-screw extrusion, obtains starch-based composite flocculant.The present invention by carrying out radiation treatment to starch, makes starch generate more free radicals, enhances amylase activity, be then grafted to MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and acrylamide sufficiently on starch molecule by twin-screw extrusion first.Preparation method provided by the invention is at low cost, process is simple, easily operated, and starch-grafted rate is high, and manufactured starch-based composite flocculant is good to the flocculating effect of sewage.
Description
Technical field
The present invention relates to technical field of sewage, in particular to a kind of starch-based composite flocculant and preparation method thereof and
Using.
Background technique
Starch is a kind of natural polymer renewable, from a wealth of sources, is made from starch and starch base wadding is made
Solidifying agent can be used for sewage treatment field.Currently, starch-based flocculant is usually by ative starch through quaternised modified or graft copolymerization etc.
The problems such as method preparation, the conventional generally existing complex process of quaternised modified or graft copolymerization method, operating difficulties, and
The starch-based flocculant of the preparation sewage extremely complex for high chroma, high concentrtion, ingredient, is not achieved ideal flocculating effect.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of starch-based composite flocculants and its preparation method and application.
Preparation method provided by the invention is at low cost, process is simple, easily operated, and starch-grafted rate is high, and manufactured starch base is compound
Flocculant has good flocculating effect to the sewage of high chroma, high concentrtion.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of starch-based composite flocculant, comprising the following steps:
(1) starch is subjected to radiation treatment with ray, obtains irradiated starch；
(2) irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water are mixed, is obtained
Mixture；
(3) mixture is subjected to twin-screw extrusion, obtains starch-based composite flocculant.
Preferably, the ray in the step (1) is alpha ray, β ray or cobalt60The irradiation dose of ray, the ray is
4~20kGy.
Preferably, the time of radiation treatment is 1~2h in the step (1).
Preferably, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride in the starch in the step (1) and step (2),
The mass ratio of acrylamide and water is 1:(0.1~0.15): (0.01~0.03): (0.1~0.12).
Preferably, the temperature of twin-screw extrusion is 85~100 DEG C in the step (3).
Preferably, the screw speed of twin-screw extrusion is 1200~1600rpm in the step (3).
The present invention provides the starch-based composite flocculants of the preparation of preparation method described in above technical scheme.
The present invention provides application of the starch-based composite flocculant described in above technical scheme in sewage treatment.
Preferably, the dosage of the starch-based composite flocculant is 0.003~0.007g/mL sewage.
Preferably, pH value >=10 of the sewage, turbidity >=50NTU, coloration >=300.
The present invention provides a kind of preparation methods of starch-based composite flocculant, comprising the following steps: by starch ray
Radiation treatment is carried out, irradiated starch is obtained；By the irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloyl
Amine and water mixing, obtain mixture；The mixture is subjected to twin-screw extrusion, obtains starch-based composite flocculant.The present invention
First by carrying out irradiation pretreatment to starch, so that starch is generated more free radicals, enhance amylase activity, then pass through double spiral shells
Bar extrusion is grafted to MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and acrylamide sufficiently on starch molecule.The present invention provides
Preparation method it is at low cost, process is simple, easily operated, and starch-grafted rate is high, and manufactured starch-based composite flocculant is to dirt
The flocculating effect of water is good.Embodiment the result shows that, preparation method provided by the invention has successfully been grafted methyl-prop on starch
Alkene acyloxyethyl trimethyl ammonium chloride and acrylamide, grafting rate is up to 44.21%, and the starch-based flocculant prepared is to high color
It spends, the sewage of high concentrtion has good flocculating effect.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of starch graft copolymer in embodiment 1.
Specific embodiment
The present invention provides a kind of preparation methods of starch-based composite flocculant, comprising the following steps:
(1) starch is subjected to radiation treatment with ray, obtains irradiated starch；
(2) irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water are mixed, is obtained
Mixture；
(3) mixture is subjected to twin-screw extrusion, obtains starch-based composite flocculant.
Starch is carried out radiation treatment with ray by the present invention, obtains irradiated starch.In the present invention, the ray is preferably
Alpha ray, β ray or cobalt60Ray, the irradiation dose of the ray are preferably 4~20kGy, more preferably 10~15kGy.At this
In invention, the time of the radiation treatment is preferably 1.~2h, more preferably 1.3~1.7h.The present invention is by carrying out starch
Radiation treatment makes starch generate more free radicals, enhances amylase activity.The present invention is not special to the type of the starch
It is required that using starch well known in the art.
After obtaining irradiated starch, the present invention is by the irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, propylene
Amide and water mixing, obtain mixture.In the present invention, the starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, propylene
The mass ratio of amide and water is preferably 1:(0.1~0.15): (0.01~0.03): (0.1~0.12), more preferably 1:0.13:
0.02:0.11.In the present invention, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride can neutralize the anion in sewage；Institute
It states the particle surface that acrylamide is easy to by hydrogen bond in sewage to adsorb, in addition, the polyacrylamide flocculant generated has very
Long strand, the long-chain of a large number of grade have huge adsorption surface area in water, and flocculation is good, also using length
Chain is built bridge between coagulated particles, forms bulky grain floccule body, accelerated sedimentation.
Mixing of the present invention to the irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water
Mode does not require particularly, guarantees that each component is uniformly mixed using hybrid mode well known in the art.The present invention is to institute
The source for stating starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and acrylamide does not require particularly, and use is commercially available
Corresponding product.
After obtaining mixture, the mixture is carried out twin-screw extrusion by the present invention, obtains starch-based composite flocculant.?
In the present invention, the temperature of the twin-screw extrusion is preferably 85~100 DEG C, and more preferably 90~95 DEG C；The twin-screw extrusion
Screw speed be preferably 1200~1600rpm, more preferably 1400~1500rpm；It is squeezed using the twin-screw of this field routine
Machine carries out twin-screw extrusion out.The present invention is extruded at a certain temperature using double screw extruder, makes metering system
Acyloxyethyl trimethyl ammonium chloride and acrylamide are sufficiently grafted on irradiated starch molecule.
The present invention provides the starch-based composite flocculants of the preparation of preparation method described in above technical scheme.The present invention provides
Starch-based composite flocculant be in extruding state, be easy to store transport, and to sewage with good flocculating effect.
The present invention also provides application of the starch-based composite flocculant described in above technical scheme in sewage treatment.At this
In invention, the dosage of the starch-based composite flocculant is preferably 0.003~0.007g/mL sewage, more preferably 0.004~
0.006g/mL sewage.In the present invention, the sewage pH value preferably >=10, turbidity preferably >=50NTU, coloration preferably >=
300.Starch-based composite flocculant provided by the invention has preferable wadding to the sewage of high chroma, high concentrtion, complicated component
Solidifying effect.
Starch-based composite flocculant provided by the invention and its preparation method and application is carried out below with reference to embodiment detailed
Thin explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) by 200g starch cobalt60Ray carries out radiation treatment, cobalt60The irradiation dose of ray is 10kGy, irradiation time
1.5h obtains irradiated starch；
(2) by the irradiated starch of (1) and 20g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (hereinafter referred to as DMC), 4g third
Acrylamide (hereinafter referred to as AM) and 20g water are uniformly mixed；
(3) mixture is squeezed out under the conditions of 95 DEG C using double screw extruder, screw speed 1400rpm is formed sediment
Powder base composite flocculation agent.
Sewage flocculation measure of merit is carried out to obtained starch-based composite flocculant:
Take sewage 100mL, pH value 11.57, turbidity 210.1NTU, coloration 876.4；The starch base that 0.5g is added is multiple
After closing flocculant, just there is obvious layering and precipitating phenomenon at once, the sewage after processing 30min is tested, as a result: treated
PH value of sewage water is 8.522, turbidity 12.5NTU, coloration 162.6.
Starch-grafted rate calculates:
Purification process is carried out to the above starch-based composite flocculant, steps are as follows:
(1) acetone 30mL is added in starch-based composite flocculant, after mixing evenly, stands, is precipitated, remove acetone
Afterwards, it repeats for several times, then dries 12h in vacuum oven at 50 DEG C, the mixture after obtaining removal acrylamide；
(2) mixture that (1) is purified, is wrapped with filter paper, is mixed with glacial acetic acid-ethylene glycol of 60:40 (volume ratio)
Solvent refluxing extracting, carries out 3 siphon circulations, then uses ethanol washing 3 times, the product after washing is in 60 DEG C of vacuum ovens
12h is dried, the mixture after obtaining removal acrylamide and homopolymer；
(3) potassium hydroxide solution (0.5mol/L) of 50ml of mixture obtained by (2) is dissolved, is placed in blender and heats
To 50 DEG C of stirring 10min, filtered on buchner funnel is then used, filtered product is pure graft copolymer；The calculating of grafting rate
Formula are as follows:
Grafting rate=(mixture quality-addition starch gross mass after removal acrylamide and homopolymer)/is added single
Gross mass × 100% of body；Wherein, the gross mass that monomer is added is the DMC being added and the gross mass of AM.
Being computed grafting rate is 44.21%.
The infrared spectrogram of pure graft copolymer is as shown in Figure 1.In Fig. 1,3414.60 be amine groups peak position, shows sample
Product have successfully been grafted amide groups, i.e. acrylamide；2928.54 be the characteristic absorption peak of methyl in quaternary ammonium cation structural unit,
Show that sample has successfully been grafted MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride.
Embodiment 2
(1) by 200g starch cobalt60Ray carries out radiation treatment, cobalt60The irradiation dose of ray is 10kGy, irradiation time
1.5h obtains irradiated starch；
(2) by the irradiated starch of (1) and 20g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (hereinafter referred to as DMC), 4g third
Acrylamide (hereinafter referred to as AM) and 20g water are uniformly mixed；
(3) mixture is squeezed out under the conditions of 95 DEG C using double screw extruder, screw speed 1200rpm is formed sediment
Powder base composite flocculation agent.
Sewage flocculation measure of merit is carried out to obtained starch-based composite flocculant:
Take sewage 100mL, pH value 11.57, turbidity 210.1NTU, coloration 876.4；The starch base that 0.5g is added is multiple
After closing flocculant, just there is obvious layering and precipitating phenomenon at once, the sewage after processing 30min is tested, as a result: treated
PH value of sewage water is 8.665, turbidity 13.0NTU, coloration 201.2.
The above starch-based composite flocculant is purified using method same as Example 1, calculates starch-grafted rate,
As a result: grafting rate 37.9%.
As can be seen from the above embodiments, process of the present invention is simple, easily operated, and starch-grafted rate is high, manufactured shallow lake
Powder base composite flocculation agent is good to the flocculating effect of sewage.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of starch-based composite flocculant, which comprises the following steps:
(1) starch is subjected to radiation treatment with ray, obtains irradiated starch；
(2) irradiated starch, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water are mixed, is mixed
Object；
(3) mixture is subjected to twin-screw extrusion, obtains starch-based composite flocculant.
2. preparation method according to claim 1, which is characterized in that the ray in the step (1) is alpha ray, β ray
Or cobalt60Ray, the irradiation dose of the ray are 4~20kGy.
3. preparation method according to claim 1, which is characterized in that in the step (1) time of radiation treatment be 1~
2h。
4. preparation method according to claim 1, which is characterized in that in the starch and the step (2) in step (1)
The mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylamide and water is 1:(0.1~0.15): (0.01~
0.03): (0.1~0.12).
5. preparation method according to claim 1, which is characterized in that the temperature of twin-screw extrusion is in the step (3)
85~100 DEG C.
6. preparation method according to claim 1, which is characterized in that the screw rod of twin-screw extrusion turns in the step (3)
Speed is 1200~1600rpm.
7. the starch-based composite flocculant of the preparation of preparation method described in claim 1~6 any one.
8. application of the starch-based composite flocculant described in claim 7 in sewage treatment.
9. application according to claim 8, which is characterized in that the dosage of the starch-based composite flocculant be 0.003~
0.007g/mL sewage.
10. application according to claim 8, which is characterized in that pH value >=10 of the sewage, turbidity >=50NTU, coloration
≥300。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3976552A (en) * | 1975-08-13 | 1976-08-24 | The United States Of America As Represented By The Secretary Of Agriculture | Water-soluble graft polymers produced by an outwardly dry radiation polymerization process |
| CN102211804A (en) * | 2011-03-10 | 2011-10-12 | 武汉纺织大学 | Preparation method of starch-based flocculating agent |
| CN104804137A (en) * | 2015-01-31 | 2015-07-29 | 武汉纺织大学 | Preparation method of water-soluble cationic grafted starch |
-
2019
- 2019-03-27 CN CN201910239050.8A patent/CN109880009A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3976552A (en) * | 1975-08-13 | 1976-08-24 | The United States Of America As Represented By The Secretary Of Agriculture | Water-soluble graft polymers produced by an outwardly dry radiation polymerization process |
| CN102211804A (en) * | 2011-03-10 | 2011-10-12 | 武汉纺织大学 | Preparation method of starch-based flocculating agent |
| CN104804137A (en) * | 2015-01-31 | 2015-07-29 | 武汉纺织大学 | Preparation method of water-soluble cationic grafted starch |
Non-Patent Citations (2)
| Title |
|---|
| 王小雄等: "淀粉絮凝剂的研究概况", 《工业水处理》 * |
| 童丹等: "《马铃薯变性淀粉加工技术》", 31 October 2015, 武汉大学出版社 * |
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Application publication date: 20190614 |