CN102250293A - Preparation method and application of acrylamide modified grafted corn cob - Google Patents
Preparation method and application of acrylamide modified grafted corn cob Download PDFInfo
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- CN102250293A CN102250293A CN 201110136514 CN201110136514A CN102250293A CN 102250293 A CN102250293 A CN 102250293A CN 201110136514 CN201110136514 CN 201110136514 CN 201110136514 A CN201110136514 A CN 201110136514A CN 102250293 A CN102250293 A CN 102250293A
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Abstract
The invention relates to the chemical field and discloses a preparation method of acrylamide modified grafted corn cob. The preparation method comprises the following steps: the agricultural waste corn cob is used as a raw material, maleic anhydride is used to modify the corn cob, then ammonium persulfate is used as an initiator, N,N-methylene diacrylamide is used as a crosslinking agent to perform graft copolymerization with acrylamide to prepare the modified corn cob. The product has good stability and flocculation performance, the flocculating rate is up to 89.66%, and the product can be used as a flocculant; and the product has better development and application prospects in the water treatment field. By adopting the method, agricultural resources can be utilized reasonably, the added value of the agricultural product can be increased, environment protection can be favored and the sustainable development strategy is beneficial to realization.
Description
Technical field
The invention belongs to chemical field, relate to a kind of preparation method of multipolymer, the preparation method of particularly a kind of corn cob-maleic anhydride-polyacrylamide copolymer (being acrylamide graft modified corn core) also relates to the application of this multipolymer.
Background technology
Because China and even worldwide water resources crisis and water pollution problems are on the rise, it is more and more important that water treatment problems becomes, and water technology also obtains to develop rapidly.Wherein, flocculence is easy with it, the economic dispatch characteristics, all is used widely in feedwater and sewage disposal.One of gordian technique of flocculence is a flocculation agent; it can make fine suspension and the colloidal particle unstability that is difficult to natural subsidence in the water; form bigger particle or floss by mutual collision, agglomeration or polymerization, bridging, finally to sink naturally or mode such as power come-up and separating with water body.Flocculation agent can be divided into inorganic flocculating agent, organic floculant, natural macromolecule flocculating agent and composite flocculation agent four classes.Wherein, natural macromolecule flocculating agent has advantages such as environmental protection, efficient, nontoxic, non-secondary pollution, applied widely, readily biodegradable because of it, and becomes the emphasis of present flocculation agent research.
Corn is one of main food crop in the world, accounts for about 25% of world food ultimate production.China is a large agricultural country, and corn yield accounts for 1/5th of grain yield, occupies the second place of the world.Corn cob is the agricultural wastes of producing behind the corn, in China's uses that act as a fuel more, not only causes the serious environmental pollution, and causes the significant wastage of resource.How to utilize the corn cob that can be used as renewable resources to cause countries in the world scientist's concern.The main component of corn cob has Mierocrystalline cellulose, xylogen and hemicellulose etc., be rich in functional groups such as hydroxyl, carboxyl, has the basis that is used to prepare flocculation agent, but form strong intramolecularly and intermolecular hydrogen bonding between these functional groups easily, therefore, corn cob generally can not directly utilize, and need carry out modification to it.Bibliographical information, with the natural organic high-molecular corn cob meal is parent, copolymerization product with triethylamine, Trimethylamine 99 and epoxy chloropropane is a cation modifier respectively, can make cationic modified natural macromolecule flocculating agent, be applied to the processing of natural groundwater, city domestic sewage, trade effluent, flocculating effect is good.
Polyacrylamide is the good synthetic flocculant of a kind of flocculating property, but its difficult degradation.Bibliographical information is a raw material with the corn cob, and methacrylic acid, acrylamide are mix monomer, and ferrous ammonium sulphate-hydrogen peroxide is the reduction system initiator, and institute's synthetic corn cob graft copolymer has the good adsorption ability to Cu (II).But do not see up to now, the research report of relevant acrylamide graft modified corn core and flocculating property thereof both at home and abroad as yet.
Summary of the invention
In view of this, one of purpose of the present invention is to provide a kind of preparation method of acrylamide graft modified corn core, and is easy, economical, the products obtained therefrom good stability, and have good flocculating property; Two of purpose is to provide a kind of acrylamide graft modified corn core product that makes according to above-mentioned preparation method; Three of purpose is to provide the application of described acrylamide graft modified corn core product as flocculation agent.
For achieving the above object, the invention provides following technical scheme:
1, the preparation method of acrylamide graft modified corn core may further comprise the steps:
A. the alkalize preparation of corn cob: with corn cob meal and massfraction is that 10 ~ 30% sodium hydroxide solution is that 1g: 6 ~ 130mL mixes according to mass volume ratio, boiling is 1 ~ 6 hour under 100 ~ 120 ℃ of temperature, pressure 0.11MPa condition, suction filtration, filter cake to constant weight, obtains the alkalization corn cob in 60 ~ 80 ℃ of vacuum-dryings of temperature;
B. the preparation of maleic anhydride modified corn cob: is that 1g: 0 ~ 36mL mixes with the alkalization corn cob and the toluene of step a gained according to mass volume ratio, put in 30 ~ 75 ℃ of water-baths of temperature and soaked 0 ~ 9 hour, adding concentration again is the maleic anhydride acetone soln of 0.02 ~ 0.2g/mL, the consumption of maleic anhydride is 10 ~ 100% of alkalization corn cob quality, in 35 ~ 80 ℃ of reactions of temperature 20 ~ 200 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob;
C. the preparation of acrylamide graft modified corn core: is that 1g: 80 ~ 160mL mixes with the maleic anhydride modified corn cob and the water of step b gained according to mass volume ratio, under protection of inert gas, be warming up to 60 ~ 80 ℃, add the acrylamide that is equivalent to maleic anhydride modified corn cob quality 300 ~ 700% successively, the ammonium persulphate and the N that is equivalent to maleic anhydride modified corn cob quality 0.5 ~ 2.5% that are equivalent to maleic anhydride modified corn cob quality 1.5 ~ 3.5%, the N-methylene-bisacrylamide, stirring reaction removed inert protective gas after 2 ~ 5 hours, put and cool off termination reaction in the ice-water bath, the product drying obtains acrylamide graft modified corn core crude product; The heating of acrylamide graft modified corn core crude product water is extracted 2 ~ 4 times, discard the water extract, extract 1 ~ 2 time with the ethanol heating, discard alcohol extract, the residuum drying promptly makes acrylamide graft modified corn core.
Preferably, described step a is to be that 20% sodium hydroxide solution is that 1g: 125mL mixes according to mass volume ratio with corn cob meal and massfraction, and boiling is 4 hours under 120 ℃ of temperature, pressure 0.11MPa condition, suction filtration, filter cake to constant weight, obtains the alkalization corn cob in 60 ℃ of vacuum-dryings of temperature.
Preferably, described step b is to be that 1g: 4mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 55 ℃ of water-baths of temperature and soaked 3 hours, adding concentration again is the maleic anhydride acetone soln of 0.18g/mL, and the consumption of maleic anhydride was 90% of alkalization corn cob quality, in 45 ℃ of reactions of temperature 200 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
Preferably, described step b is to be that 1g: 24mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 75 ℃ of water-baths of temperature and soaked 2 hours, adding concentration again is the maleic anhydride acetone soln of 0.08g/mL, and the consumption of maleic anhydride was 40% of alkalization corn cob quality, in 55 ℃ of reactions of temperature 40 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
Preferably, described step b is to be that 1g: 36mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 65 ℃ of water-baths of temperature and soaked 8 hours, adding concentration again is the maleic anhydride acetone soln of 0.02g/mL, and the consumption of maleic anhydride was 10% of alkalization corn cob quality, in 50 ℃ of reactions of temperature 120 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
Preferred, described step b is to be that 1g: 32mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 50 ℃ of water-baths of temperature and soaked 6 hours, adding concentration again is the maleic anhydride acetone soln of 0.04g/mL, and the consumption of maleic anhydride was 20% of alkalization corn cob quality, in 70 ℃ of reactions of temperature 20 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
Preferably; described step c mixes maleic anhydride modified corn cob and water according to mass volume ratio 1g: 120 ~ 160mL; under nitrogen protection, be warming up to 70 ~ 75 ℃; add the acrylamide that is equivalent to maleic anhydride modified corn cob quality 400 ~ 600% successively; the ammonium persulphate and the N that is equivalent to maleic anhydride modified corn cob quality 0.5 ~ 1.5% that are equivalent to maleic anhydride modified corn cob quality 2 ~ 3%; the N-methylene-bisacrylamide; stirring reaction recession in 3 hours denitrification gas; put and cool off termination reaction in the ice-water bath; the product drying obtains acrylamide graft modified corn core crude product.
Preferred; described step c is to be that 1g: 140mL mixes with maleic anhydride modified corn cob and water according to mass volume ratio; under nitrogen protection, be warming up to 70 ℃; add 500% the acrylamide be equivalent to maleic anhydride modified corn cob quality successively, be equivalent to the ammonium persulphate of maleic anhydride modified corn cob quality 2% and be equivalent to the N of maleic anhydride modified corn cob quality 1%; the N-methylene-bisacrylamide; stirring reaction recession in 3 hours denitrification gas; put and cool off termination reaction in the ice-water bath; the product drying obtains acrylamide graft modified corn core crude product.
2, the acrylamide graft modified corn core that makes according to the method described above.
3, since the acrylamide graft modified corn core good stability that makes according to the method described above and have good flocculating property therefore, it can be used as flocculation agent.
Beneficial effect of the present invention is: the present invention is a raw material with the agricultural wastes corn cob, by maleic anhydride modified corn cob, having made a kind of corn cob-maleic anhydride-acrylamide copolymer with acrylic amide graft copolymerization again is acrylamide graft modified corn core, product stability is good and have a good flocculating property, can be used as flocculation agent and use, have development prospect preferably in water treatment field.The present invention not only helps the reasonable utilization of agricultural resource, improves additional value of farm products, and helps environment protection, is beneficial to the realization strategy of sustainable development.
Description of drawings
Fig. 1 is the infrared spectrogram of unmodified (curve 1) and maleic anhydride modified (curve 2) corn cob.
Embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, the preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
The main agents and the instrument that use in the preferred embodiment are as follows: corn cob is provided by suburbs peasant household, pulverizes with preceding oven dry, and 80 orders sieve; Maleic anhydride, acrylamide, ammonium persulphate and N,N methylene bis acrylamide are commercially available analytical pure; Ethanol, kaolin, calcium chloride and sodium hydroxide are commercially available chemical pure.UV-2450 ultraviolet spectrophotometer and IRP restige-21 infrared spectrometer are day island proper Tianjin company product.
Preparation of embodiment 1 ~ 10, acrylamide graft modified corn core (toxilic acid modified corn core condition optimizing) and flocculating property are investigated
The logical method of preparation:Adding corn cob meal 4.0g and massfraction are 20% sodium hydroxide solution 500mL in pressure kettle, and boiling is 4 hours under 120 ℃ of temperature, pressure 0.11MPa condition, and suction filtration, filter cake to constant weight, obtain the alkalization corn cob in 60 ℃ of vacuum-dryings of temperature; In the 250mL three-necked flask, add alkalization corn cob 1.0g and toluene
X 1 ML puts temperature
X 2 Soak in ℃ water-bath
X 3 Hour, add maleic anhydride again
X 4 The acetone soln 5mL of g is in temperature
X 5 ℃ reaction
X 6 Minute, be cooled to room temperature, use washing with acetone 3 times, oven dry obtains maleic anhydride modified corn cob; In 250mL four neck flasks, add maleic anhydride modified corn cob 0.5g and water 70mL, logical nitrogen is warming up to 70 ℃ after 10 minutes, add acrylamide 2.5g, ammonium persulphate 0.0125g and N successively, N-methylene-bisacrylamide 0.005g, react and stop logical nitrogen after 3 hours, put and cool off termination reaction in the ice-water bath, product obtains acrylamide graft modified corn core crude product in 100 ℃ of oven dry of temperature; With boiling water extraction 3 times of acrylamide graft modified corn core crude product, each 10 minutes, discard the water extract, transfer in the apparatus,Soxhlet's, with extraction using alcohol 1 hour, discard alcohol extract (removing methacrylamide homopolymer), residuum is dried to constant weight, promptly makes acrylamide graft modified corn core.
Flocculating property investigation method:Adding concentration in the 100mL beaker is the kaolin suspension liquid 50mL of 4g/L, and concentration is that the acrylamide graft modified corn core 1mL of 10g/L and massfraction are 1% CaCl
2Solution 1mL, control group (not adding acrylamide graft modified corn core) is set simultaneously, regulator solution pH to 7.0, put on the magnetic stirrer and stir, mixing parametric is as follows: being earlier that 200r/min stirred 1 minute with speed, is that 80r/min stirred 4 minutes again with speed, left standstill at last 2 minutes, draw supernatant liquor, measure absorbancy in wavelength 550nm place with spectrophotometer, the calculating flocculating rate (
E):
E=(
A 0-
A)/
A 0* 100%, in the formula
A 0The absorbancy of expression control group supernatant liquor,
AThe absorbancy of expression experimental group supernatant liquor is represented the flocculating property of acrylamide graft modified corn core with flocculating rate.
The result:The preparation of acrylamide graft modified corn core and flocculating property are investigated and be the results are shown in Table 1.As shown in Table 1, the flocculating property of embodiment 2,7,9,10 gained acrylamide graft modified corn cores is better, and flocculating rate is more than 75%; Wherein, the flocculating property of embodiment 9 gained acrylamide graft modified corn cores is best, flocculating rate is up to 88.83%, the maleic anhydride modified top condition that is corn cob is: 1.0g alkalization corn cob adds in the 32mL toluene, temperature was soaked 6 hours for 50 ℃, mix 70 ℃ of reactions of temperature 20 minutes again with the acetone that 5mL is dissolved with the 0.2g maleic anhydride.
The preparation of table 1 acrylamide graft modified corn core and flocculating property are investigated
The infrared spectrogram of maleic anhydride modified corn cob is seen Fig. 1.As seen from Figure 1, the more unmodified corn cob of modified corn core (curve 2) (curve 1) is 1716cm at wavelength
-1Place's appearance-C=C-charateristic avsorption band illustrates that corn cob has connected maleic anhydride.
Preparation of embodiment 11 ~ 30, acrylamide graft modified corn core (acrylamide and maleic anhydride modified corn cob conditions of graft copolymerization are optimized) and flocculating property are investigated
The logical method of preparation:Adding corn cob meal 4.0g and massfraction are 20% sodium hydroxide solution 500mL in pressure kettle, and boiling is 4 hours under 120 ℃ of temperature, pressure 0.11MPa condition, and suction filtration, filter cake to constant weight, obtain the alkalization corn cob in 60 ℃ of vacuum-dryings of temperature; In the 250mL three-necked flask, add alkalization corn cob 1g and toluene 20mL, put in 40 ℃ of water-baths of temperature and soaked 5 hours, add the acetone soln 10mL of maleic anhydride 0.4g again, in 80 ℃ of reactions of temperature 90 minutes, be cooled to room temperature, use washing with acetone 3 times, oven dry obtains maleic anhydride modified corn cob; Add maleic anhydride modified corn cob 0.5g and water 70mL in 250mL four neck flasks, logical nitrogen was warming up to after 10 minutes
Y 1 ℃, add acrylamide successively
Y 2 G, ammonium persulphate
Y 3 G and N,N methylene bis acrylamide
Y 4 G, stirring reaction stop logical nitrogen after 3 hours, put and cool off termination reaction in the ice-water bath, and product obtains acrylamide graft modified corn core crude product in 100 ℃ of oven dry of temperature; With boiling water extraction 3 times of acrylamide graft modified corn core crude product, each 10 minutes, discard the water extract, transfer in the apparatus,Soxhlet's, with extraction using alcohol 1 hour, discard alcohol extract (removing methacrylamide homopolymer), residuum is dried to constant weight, promptly makes acrylamide graft modified corn core.
Flocculating property investigation method:With embodiment 1 ~ 10.
The result:The preparation of acrylamide graft modified corn core and flocculating property are investigated and be the results are shown in Table 2.
The preparation of table 2 acrylamide graft modified corn core and flocculating property are investigated
By table 2 embodiment 11 ~ 15 as can be known, the temperature of graft copolymerization has considerable influence to the flocculating property of acrylamide graft modified corn core, preferable temperature of reaction is 70 ~ 75 ℃, and the flocculating property of gained acrylamide graft modified corn core is better, and flocculating rate reaches more than 60%; Better temperature of reaction is 70 ℃, and the flocculating rate of gained acrylamide graft modified corn core reaches maximum value 67.18%.
By table 2 embodiment 16 ~ 20 as can be known, the consumption of acrylamide monomer has considerable influence to the flocculating property of acrylamide graft modified corn core in the graft copolymerization, when the consumption of acrylamide monomer be maleic anhydride modified corn cob quality 400 ~ 600% the time, the flocculating property of gained acrylamide graft modified corn core is better, and flocculating rate reaches more than 50%; When the consumption of acrylamide monomer be maleic anhydride modified corn cob quality 500% the time, the flocculating rate of gained acrylamide graft modified corn core reaches maximum value 67.23%.
By table 2 embodiment 21 ~ 25 as can be known, the consumption of initiator ammonium persulfate has a significant impact the flocculating property of acrylamide graft modified corn core in the graft copolymerization, when the consumption of initiator be maleic anhydride modified corn cob quality 2.0 ~ 3.0% the time, the flocculating property of gained acrylamide graft modified corn core is better, and flocculating rate reaches more than 50%; When the consumption of initiator be maleic anhydride modified corn cob quality 2.0% the time, the flocculating rate of gained acrylamide graft modified corn core reaches maximum value 89.66%.
By table 2 embodiment 26 ~ 30 as can be known, linking agent N in the graft copolymerization, the consumption of N-methylene-bisacrylamide is less relatively to the influence of acrylamide graft modified corn core flocculating property, when dosage of crosslinking agent be maleic anhydride modified corn cob quality 0.5 ~ 2.5% the time, the flocculating rate of gained acrylamide graft modified corn core is all more than 50%; When the consumption of linking agent be maleic anhydride modified corn cob quality 1.0% the time, the flocculating rate of gained acrylamide graft modified corn core reaches maximum value 67.23%.
To sum up, the acrylic amide graft copolymerization top condition of modified corn core is: 70 ℃ of temperature of reaction, the consumption of acrylamide monomer is 500% of a maleic anhydride modified corn cob quality, the consumption of initiator ammonium persulfate is 2% of a maleic anhydride modified corn cob quality, the consumption of linking agent N,N methylene bis acrylamide is 1% of a maleic anhydride modified corn cob quality.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (10)
1. the preparation method of acrylamide graft modified corn core is characterized in that: may further comprise the steps:
A. the alkalize preparation of corn cob: with corn cob meal and massfraction is that 10 ~ 30% sodium hydroxide solution is that 1g: 6 ~ 130mL mixes according to mass volume ratio, boiling is 1 ~ 6 hour under 100 ~ 120 ℃ of temperature, pressure 0.11MPa condition, suction filtration, filter cake to constant weight, obtains the alkalization corn cob in 60 ~ 80 ℃ of vacuum-dryings of temperature;
B. the preparation of maleic anhydride modified corn cob: is that 1g: 0 ~ 36mL mixes with the alkalization corn cob and the toluene of step a gained according to mass volume ratio, put in 30 ~ 75 ℃ of water-baths of temperature and soaked 0 ~ 9 hour, adding concentration again is the maleic anhydride acetone soln of 0.02 ~ 0.2g/mL, the consumption of maleic anhydride is 10 ~ 100% of alkalization corn cob quality, in 35 ~ 80 ℃ of reactions of temperature 20 ~ 200 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob;
C. the preparation of acrylamide graft modified corn core: is that 1g: 80 ~ 160mL mixes with the maleic anhydride modified corn cob and the water of step b gained according to mass volume ratio, under protection of inert gas, be warming up to 60 ~ 80 ℃, add the acrylamide that is equivalent to maleic anhydride modified corn cob quality 300 ~ 700% successively, the ammonium persulphate and the N that is equivalent to maleic anhydride modified corn cob quality 0.5 ~ 2.5% that are equivalent to maleic anhydride modified corn cob quality 1.5 ~ 3.5%, the N-methylene-bisacrylamide, stirring reaction removed inert protective gas after 2 ~ 5 hours, put and cool off termination reaction in the ice-water bath, the product drying obtains acrylamide graft modified corn core crude product; The heating of acrylamide graft modified corn core crude product water is extracted 2 ~ 4 times, discard the water extract, extract 1 ~ 2 time with the ethanol heating, discard alcohol extract, the residuum drying promptly makes acrylamide graft modified corn core.
2. the preparation method of acrylamide graft modified corn core according to claim 1, it is characterized in that: described step a is to be that 20% sodium hydroxide solution is that 1g: 125mL mixes according to mass volume ratio with corn cob meal and massfraction, boiling is 4 hours under 120 ℃ of temperature, pressure 0.11MPa condition, suction filtration, filter cake to constant weight, obtains the alkalization corn cob in 60 ℃ of vacuum-dryings of temperature.
3. the preparation method of acrylamide graft modified corn core according to claim 1, it is characterized in that: described step b is to be that 1g: 4mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 55 ℃ of water-baths of temperature and soaked 3 hours, adding concentration again is the maleic anhydride acetone soln of 0.18g/mL, and the consumption of maleic anhydride was 90% of alkalization corn cob quality, in 45 ℃ of reactions of temperature 200 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
4. the preparation method of acrylamide graft modified corn core according to claim 1, it is characterized in that: described step b is to be that 1g: 24mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 75 ℃ of water-baths of temperature and soaked 2 hours, adding concentration again is the maleic anhydride acetone soln of 0.08g/mL, and the consumption of maleic anhydride was 40% of alkalization corn cob quality, in 55 ℃ of reactions of temperature 40 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
5. the preparation method of acrylamide graft modified corn core according to claim 1, it is characterized in that: described step b is to be that 1g: 36mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 65 ℃ of water-baths of temperature and soaked 8 hours, adding concentration again is the maleic anhydride acetone soln of 0.02g/mL, the consumption of maleic anhydride is 10% of alkalization corn cob quality, in 50 ℃ of reactions of temperature 120 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
6. the preparation method of acrylamide graft modified corn core according to claim 1, it is characterized in that: described step b is to be that 1g: 32mL mixes with alkalization corn cob and toluene according to mass volume ratio, put in 50 ℃ of water-baths of temperature and soaked 6 hours, adding concentration again is the maleic anhydride acetone soln of 0.04g/mL, and the consumption of maleic anhydride was 20% of alkalization corn cob quality, in 70 ℃ of reactions of temperature 20 minutes, cooling, product acetone thorough washing, drying obtains maleic anhydride modified corn cob.
7. the preparation method of acrylamide graft modified corn core according to claim 1; it is characterized in that: described step c mixes maleic anhydride modified corn cob and water according to mass volume ratio 1g: 120 ~ 160mL; under nitrogen protection, be warming up to 70 ~ 75 ℃; add the acrylamide that is equivalent to maleic anhydride modified corn cob quality 400 ~ 600% successively; the ammonium persulphate and the N that is equivalent to maleic anhydride modified corn cob quality 0.5 ~ 1.5% that are equivalent to maleic anhydride modified corn cob quality 2 ~ 3%; the N-methylene-bisacrylamide; stirring reaction recession in 3 hours denitrification gas; put and cool off termination reaction in the ice-water bath; the product drying obtains acrylamide graft modified corn core crude product.
8. the preparation method of acrylamide graft modified corn core according to claim 7; it is characterized in that: described step c is to be that 1g: 140mL mixes with maleic anhydride modified corn cob and water according to mass volume ratio; under nitrogen protection, be warming up to 70 ℃; add 500% the acrylamide be equivalent to maleic anhydride modified corn cob quality successively; the ammonium persulphate and the N that is equivalent to maleic anhydride modified corn cob quality 1% that are equivalent to maleic anhydride modified corn cob quality 2%; the N-methylene-bisacrylamide; stirring reaction recession in 3 hours denitrification gas; put and cool off termination reaction in the ice-water bath; the product drying obtains acrylamide graft modified corn core crude product.
9. the acrylamide graft modified corn core that makes according to the described method of the arbitrary claim of claim 1 to 8.
10. the described acrylamide graft modified corn of claim 9 core is as the application of flocculation agent.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719272A (en) * | 1984-06-27 | 1988-01-12 | National Starch And Chemical Corporation | Monomeric cationic glycoside derivatives |
| WO2003095525A1 (en) * | 2002-05-07 | 2003-11-20 | Aquero Company Llc | Copolymers of amino acids and methods of their production |
| CN101007668A (en) * | 2007-01-19 | 2007-08-01 | 盛力 | Natural organic high-molecular flocculant and its preparation method |
| CN101186370A (en) * | 2007-12-11 | 2008-05-28 | 南京师范大学 | Method for purifying chromium-containing industrial waste water by using composite flocculant |
| CN102010108A (en) * | 2010-10-08 | 2011-04-13 | 聊城金太阳生物化工有限公司 | Industrial sludge treatment method and method for preparing various fertilizers by using treated industrial sludge |
-
2011
- 2011-05-25 CN CN2011101365146A patent/CN102250293B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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