CN109455776A - A kind of sewage scavenging material and preparation method thereof - Google Patents
A kind of sewage scavenging material and preparation method thereof Download PDFInfo
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- CN109455776A CN109455776A CN201811355281.7A CN201811355281A CN109455776A CN 109455776 A CN109455776 A CN 109455776A CN 201811355281 A CN201811355281 A CN 201811355281A CN 109455776 A CN109455776 A CN 109455776A
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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
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/14—Esterification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C08G81/024—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
- C08G81/025—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G containing polyether sequences
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
Abstract
The present invention relates to a kind of sewage scavenging materials and preparation method thereof.The sewage scavenging material is by modified polyacrylate, improved ferroferric oxide presoma, second alcohol and water composition, the modified polyacrylate is by polyacrylate, Macrogol 600, isomerous tridecanol, polyethylene glycol 400 and alchlor reaction are made, the polyacrylate is by acrylic acid, acrylamide, water, benzoyl peroxide, own dioxane, sorbester p18, dichloroethanes, polyvinyl alcohol 1788 and N, the reaction of N- methylene-bisacrylamide is made, the improved ferroferric oxide presoma is by ferroso-ferric oxide presoma, aluminium polychloride, ethyl alcohol and Macrogol 600 reaction are made, the ferroso-ferric oxide presoma is by ferric trichloride, formic acid, water, ethyl alcohol and cetomacrogol 1000 reaction are made.Sewage provided by the invention has excellent reduction water body COD performance and recuperability with scavenging material.
Description
Technical field
The present invention relates to water body purification fields, and in particular to a kind of sewage scavenging material and preparation method thereof.
Background technique
With national economy and industrialized fast development, attention of the environmental pollution increasingly by country, especially water
The pollution of body, water pollution will seriously affect people's lives environment and health, the governing problem urgent need to resolve of water pollution.Cause
This, country encourages different field research worker to study the efficient administering method of polluted-water.Since common sewage is with only
It is relatively low to the treatment effeciency for reducing COD performance in polluted-water to change material.Therefore, sewage scavenging material reduces water in high efficiency
COD aspect of performance needs improve in body.
Summary of the invention
The purpose of the present invention is to provide a kind of sewage scavenging material, which uses modified polypropene with scavenging material
Acid esters, improved ferroferric oxide presoma, second alcohol and water are prepared, and with excellent reduction water body COD performance and can be recycled
Property.
Another object of the present invention is to provide the preparation methods of above-mentioned sewage scavenging material.
To achieve the goals above, technical scheme is as follows:
A kind of sewage scavenging material is 81:15~21:75~90:28~41 modified polypropene by mass parts ratio
Acid esters, improved ferroferric oxide presoma, second alcohol and water composition；Wherein, the modified polyacrylate is by mass parts ratio
For 83:6~11:7~12:5~10:0.3~1 polyacrylate, Macrogol 600, isomerous tridecanol, polyethylene glycol 400
It is made with alchlor reaction；The polyacrylate is 36:57~69:82~100:0.2~1:121 by mass parts ratio
~150:1~6:56~71:0.5~3:0.02~0.1 acrylic acid, acrylamide, water, benzoyl peroxide, own dioxane, department
Disk 60, dichloroethanes, polyvinyl alcohol 1788 and N,N methylene bis acrylamide reaction are made；The improved ferroferric oxide
Presoma by mass parts ratio 51:17~23:53~70:0.8~5 ferroso-ferric oxide presoma, aluminium polychloride, ethyl alcohol and
Macrogol 600 reaction is made；The ferroso-ferric oxide presoma by mass parts ratio be 36:8.7~21:2~8:68~
Ferric trichloride, formic acid, water, ethyl alcohol and the cetomacrogol 1000 reaction of 83:0.3~3 are made.
Preferably, the mass parts ratio of the modified polyacrylate, improved ferroferric oxide presoma, second alcohol and water
For 81:19.5:86:34.
The preparation method of above-mentioned sewage scavenging material, includes the following steps:
(1), ferric trichloride, water, ethyl alcohol and cetomacrogol 1000 are added in reaction kettle, mixing speed 125r/
Min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, formic acid is added according to 0.02 mass parts/min adding rate
It adds in reaction kettle, the 1~5h that maintains under above-mentioned reaction condition that the reaction was continued obtains ferroso-ferric oxide presoma；The formic acid
Purpose be for reaction reduction atmosphere is provided；
(2), aluminium polychloride, ethyl alcohol and Macrogol 600 are added in reaction kettle, mixing speed 100r/min,
25min is reacted under the conditions of 50 DEG C of maintenance system reaction temperature, ferroso-ferric oxide presoma is added according to 0.05 mass parts/min
Rate of acceleration is added in reaction kettle, the 0.5~3h that maintains under above-mentioned reaction condition that the reaction was continued, temperature of reaction kettle is warming up to 60~
85 DEG C of 0.2~1h of reaction, obtain improved ferroferric oxide presoma；The purpose of the aluminium polychloride and Macrogol 600
It is to improve ferroso-ferric oxide presoma and reducing water body COD performance；
(3), by benzoyl peroxide, own dioxane, sorbester p18, dichloroethanes, polyvinyl alcohol 1788 and N, N- di-2-ethylhexylphosphine oxide
Acrylamide is added in reaction kettle, mixing speed 140r/min, and reaction temperature is 41~58 DEG C of 28~45min of reaction, will
The mixed liquor of acrylic acid, acrylamide and water is added in reaction kettle according to 0.09 mass parts/min adding rate, in maintenance
The 1.5h that states under reaction condition that the reaction was continued, is warming up to 61~80 DEG C of 1~5h of reaction for temperature of reaction kettle, temperature of reaction kettle is heated up
To 95 DEG C of heat preservation 25min, reaction kettle is reacted into 35min under the conditions of 100 DEG C, -0.06MPa reduced-pressure backflow, reaction kettle is cooled down
To 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving polyacrylate；The purpose of the acrylic acid is
To improve polyacrylate chemical mobility of the surface；
(4), polyacrylate, Macrogol 600, isomerous tridecanol, polyethylene glycol 400 and alchlor are added to instead
Answer in kettle, mixing speed 115r/min, under the conditions of 119~137 DEG C of maintenance system temperature, -0.08MPa reduced-pressure backflow react 1~
5h, product through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times, it is 500mL ethanol washing 3 times, dry to get arriving
Modified polyacrylate；The purpose of the Macrogol 600, isomerous tridecanol and polyethylene glycol 400 is to improve polypropylene
The reduction water body COD performance of acid esters；(5), modified polyacrylate, second alcohol and water are added in reaction kettle, mixing speed is
160r/min reacts 30min under the conditions of maintenance system temperature 45 C, by improved ferroferric oxide presoma according to 0.07 mass
The adding rate of part/min is added in reaction kettle, and it is anti-that product is transferred to hydro-thermal by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
It answers in kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 123~146 DEG C of hydro-thermals
React 1~6h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
The beneficial effects of the present invention are:
1, formic acid has reproducibility, and reduction atmosphere can be provided for reaction system, can be reacted with ferric ion, is catalyzed
While stably dispersing, promote going back for ferric ion in ethyl alcohol and cetomacrogol 1000 with promotion ferroso-ferric oxide presoma
It is former；Ferroso-ferric oxide forerunner's physical efficiency of preparation improves the recuperability of sewage scavenging material；
2, aluminium polychloride and Macrogol 600 are by dispersing ferroso-ferric oxide presoma in the reaction system, through water
After heat treatment, ferroso-ferric oxide can be coated on inside aluminium polychloride and Macrogol 600, it is recyclable to improve aluminium polychloride
While property, improve the reduction water body COD performance of ferroso-ferric oxide；Improved ferroferric oxide forerunner's physical efficiency of preparation improves sewage
With the reduction water body COD performance and recuperability of scavenging material；
3, acrylic acid is introduced into polyacrylic acid ester structure by acrylic acid chemical activity with higher, keeps polypropylene
While acid esters water imbibition and flocculability, polyacrylate chemical mobility of the surface can be improved, increase can reactive chemistry functional group number
Amount；The polyacrylate of preparation can be obviously improved sewage because of chemical mobility of the surface energy, water imbibition and flocculating property with higher
With the reduction water body COD performance and recuperability of scavenging material；
4, polyacrylate is because containing carboxylic group in its structure, in the presence of a catalyst, can be with Macrogol 600, different
Structure tridecanol and polyethylene glycol 400 react, and can improve the flocculability of polyacrylate；The modified polyacrylate of preparation because
The reduction water body COD of polyacrylate can be obviously improved containing Macrogol 600, isomerous tridecanol and polyethylene glycol 400 structure
Performance；
5, while modified polyacrylate has excellent flocculation, also there is water suction volume to swell effect, is conducive to
The recycling of scavenging material；While improved ferroferric oxide presoma has elite clone recycling effect, because of modified four oxidation three
Iron contains aluminium polychloride and has flocculability, thus, both modified polyacrylate and improved ferroferric oxide have collaboration
Effect assigns sewage scavenging material excellent reduction water body COD performance and recuperability.
Specific embodiment
A specific embodiment of the invention is described below with reference to embodiment, to better understand the present invention.This
It is a little that examples are only for illustrating the present invention and not for limiting the scope of the present invention.Actual conditions are not specified in lower example embodiment
Experimental method, usually according to this field normal condition or the condition suggested according to manufacturer；Used raw material, reagent etc.,
It unless otherwise specified, is the raw materials and reagents that can be obtained from commercial sources such as conventional markets.Those skilled in the art is at this
The variation and replacement of any unsubstantiality done on the basis of invention belong to scope of the present invention.
Embodiment 1
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 5.9 parts of water, 75 parts of ethyl alcohol and 1.7 parts of cetomacrogol 1000s are weighed and are added to reaction kettle
In, mixing speed 125r/min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 13 parts of formic acid according to 0.02
The adding rate of part/min is added in reaction kettle, the 3.5h that maintains under above-mentioned reaction condition that the reaction was continued, obtains ferroso-ferric oxide
Presoma；
(2), 19 parts of aluminium polychlorides, 65 parts of ethyl alcohol and 1.6 parts of Macrogol 600s are weighed to be added in reaction kettle, are stirred
Speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas according to
The adding rate of 0.05 part/min is added in reaction kettle, the 2.5h that maintains under above-mentioned reaction condition that the reaction was continued, will react kettle temperature
Degree is warming up to 65 DEG C of reaction 0.5h, obtains improved ferroferric oxide presoma；
(3), 0.3 part of benzoyl peroxide, 135 parts of own dioxanes, 3.2 parts of sorbester p18s, 63 parts of dichloroethanes, 0.9 part are weighed
Polyvinyl alcohol 1788 and 0.03 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 45 DEG C of reaction 35min, by the mixed liquor of 36 parts of acrylic acid, 61 parts of acrylamides and 96 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 68 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 3h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow condition
Reaction kettle is cooled to 45 DEG C by lower reaction 35min, and product is through filtering, 900mL ethanol washing 5 times, dry to get arriving polypropylene
Acid esters；
(4), 83 parts of polyacrylate, 7.6 parts of Macrogol 600s, 9.5 parts of isomerous tridecanols, 7.8 parts of polyethylene glycol are weighed
400 and 0.4 parts of alchlors are added in reaction kettle, mixing speed 115r/min, 135 DEG C of maintenance system temperature, -0.08MPa
React 3.5h under the conditions of reduced-pressure backflow, product washs 3 times, 500mL ethyl alcohol through filtering, 650mL ethanol washing 2 times, 750mL methanol
It washs 3 times, dry to get modified polyacrylate is arrived；
(5), it weighs 81 parts of modified polyacrylates, 86 parts of ethyl alcohol and 34 parts of water to be added in reaction kettle, mixing speed is
160r/min reacts 30min under the conditions of maintenance system temperature 45 C, by 19.5 parts of improved ferroferric oxide presomas according to 0.07
The adding rate of part/min is added in reaction kettle, and it is anti-that product is transferred to hydro-thermal by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
It answers in kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 139 DEG C of hydro-thermal reactions
4h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 2
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 2 parts of water, 68 parts of ethyl alcohol and 0.3 part of cetomacrogol 1000 is weighed to be added in reaction kettle,
Mixing speed is 125r/min, reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 8.7 parts of formic acid according to 0.02 part/
The adding rate of min is added in reaction kettle, the 1h that maintains under above-mentioned reaction condition that the reaction was continued, obtains ferroso-ferric oxide forerunner
Body；
(2), 17 parts of aluminium polychlorides, 53 parts of ethyl alcohol and 0.8 part of Macrogol 600 are weighed to be added in reaction kettle, is stirred
Speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas according to
The adding rate of 0.05 part/min is added in reaction kettle, the 0.5h that maintains under above-mentioned reaction condition that the reaction was continued, will react kettle temperature
Degree is warming up to 60 DEG C of reaction 1h, obtains improved ferroferric oxide presoma；
(3), weigh 0.2 part of benzoyl peroxide, 121 parts of own dioxanes, 1 part of sorbester p18,56 parts of dichloroethanes, 0.5 part it is poly-
Vinyl alcohol 1788 and 0.02 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, reaction
Temperature is 41 DEG C of reaction 45min, by the mixed liquor of 36 parts of acrylic acid, 57 parts of acrylamides and 82 parts of water according to 0.09 part/min's
Adding rate is added in reaction kettle, the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued, and temperature of reaction kettle is warming up to 61 DEG C
5h is reacted, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle under the conditions of 100 DEG C, -0.06MPa reduced-pressure backflow
35min is reacted, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving polyacrylic acid
Ester；
(4), weigh 83 parts of polyacrylate, 6 parts of Macrogol 600s, 7 parts of isomerous tridecanols, 5 parts of polyethylene glycol 400s and
0.3 part of alchlor is added in reaction kettle, mixing speed 115r/min, and 119 DEG C of maintenance system temperature, -0.08MPa are depressurized back
React 5h under the conditions of stream, product through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times, 500mL ethanol washing 3 times,
It dries to get modified polyacrylate is arrived；
(5), it weighs 81 parts of modified polyacrylates, 75 parts of ethyl alcohol and 28 parts of water to be added in reaction kettle, mixing speed is
160r/min reacts 30min under the conditions of maintenance system temperature 45 C, by 15 parts of improved ferroferric oxide presomas according to 0.07
The adding rate of part/min is added in reaction kettle, and it is anti-that product is transferred to hydro-thermal by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
It answers in kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 123 DEG C of hydro-thermal reactions
6h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 3
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 8 parts of water, 83 parts of ethyl alcohol and 3 parts of cetomacrogol 1000s are weighed to be added in reaction kettle, are stirred
Mixing speed is 125r/min, 16min is reacted under the conditions of 65 DEG C of maintenance system reaction temperature, by 21 parts of formic acid according to 0.02 part/min
Adding rate be added in reaction kettle, the 5h that maintains under above-mentioned reaction condition that the reaction was continued obtains ferroso-ferric oxide presoma；
(2), it weighs 23 parts of aluminium polychlorides, 70 parts of ethyl alcohol and 5 parts of Macrogol 600s to be added in reaction kettle, stirring speed
Degree is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas according to
The adding rate of 0.05 part/min is added in reaction kettle, the 3h that maintains under above-mentioned reaction condition that the reaction was continued, by temperature of reaction kettle
85 DEG C of reaction 0.2h are warming up to, improved ferroferric oxide presoma is obtained；
(3), 1 part of benzoyl peroxide, 150 parts of own dioxanes, 6 parts of sorbester p18s, 71 parts of dichloroethanes, 3 parts of polyethylene are weighed
Alcohol 1788 and 0.1 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, and reaction temperature is
58 DEG C of reaction 28min, by the mixed liquor of 36 parts of acrylic acid, 69 parts of acrylamides and 100 parts of water according to the addition of 0.09 part/min
Rate is added in reaction kettle, the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued, and temperature of reaction kettle is warming up to 80 DEG C of reactions
1h, is warming up to 95 DEG C of heat preservation 25min for temperature of reaction kettle, and reaction kettle is reacted under the conditions of 100 DEG C, -0.06MPa reduced-pressure backflow
Reaction kettle is cooled to 45 DEG C by 35min, and product is through filtering, 900mL ethanol washing 5 times, dry to get arriving polyacrylate；
(4), 83 parts of polyacrylate, 11 parts of Macrogol 600s, 12 parts of isomerous tridecanols, 10 parts of polyethylene glycol 400s are weighed
It is added in reaction kettle with 1 part of alchlor, mixing speed 115r/min, 137 DEG C of maintenance system temperature, -0.08MPa are depressurized back
React 1h under the conditions of stream, product through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times, 500mL ethanol washing 3 times,
It dries to get modified polyacrylate is arrived；(5), 81 parts of modified polyacrylates, 90 parts of ethyl alcohol and 41 parts of water are weighed to be added to instead
It answers in kettle, mixing speed 160r/min, reacts 30min under the conditions of maintenance system temperature 45 C, by 21 parts of modified four oxidations three
Iron presoma is added in reaction kettle according to the adding rate of 0.07 part/min, and maintaining under above-mentioned reaction condition that the reaction was continued, 2h will
Product is transferred in hydrothermal reaction kettle, and maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is heated up
To 146 DEG C of hydro-thermal reaction 1h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 4
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 2.3 parts of water, 69 parts of ethyl alcohol and 0.5 part of cetomacrogol 1000 are weighed and is added to reaction kettle
In, mixing speed 125r/min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 8.9 parts of formic acid according to 0.02
The adding rate of part/min is added in reaction kettle, the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued, obtains ferroso-ferric oxide
Presoma；
(2), 17.8 parts of aluminium polychlorides, 55 parts of ethyl alcohol and 1.3 parts of Macrogol 600s are weighed to be added in reaction kettle, are stirred
Mixing speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, 51 parts of ferroso-ferric oxide presomas are pressed
It is added in reaction kettle according to the adding rate of 0.05 part/min, the 0.9h that maintains under above-mentioned reaction condition that the reaction was continued, by reaction kettle
Temperature is warming up to 63 DEG C of reaction 0.4h, obtains improved ferroferric oxide presoma；
(3), 0.3 part of benzoyl peroxide, 122 parts of own dioxanes, 1.3 parts of sorbester p18s, 58 parts of dichloroethanes, 0.8 part are weighed
Polyvinyl alcohol 1788 and 0.03 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 43 DEG C of reaction 29min, by the mixed liquor of 36 parts of acrylic acid, 59 parts of acrylamides and 83 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 63 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 1.5h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow item
35min is reacted under part, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving poly- third
Olefin(e) acid ester；
(4), 83 parts of polyacrylate, 6.8 parts of Macrogol 600s, 7.6 parts of isomerous tridecanols, 5.5 parts of polyethylene glycol are weighed
400 and 0.4 parts of alchlors are added in reaction kettle, mixing speed 115r/min, 120 DEG C of maintenance system temperature, -0.08MPa
React 1.3h under the conditions of reduced-pressure backflow, product washs 3 times, 500mL ethyl alcohol through filtering, 650mL ethanol washing 2 times, 750mL methanol
It washs 3 times, dry to get modified polyacrylate is arrived；
(5), it weighs 81 parts of modified polyacrylates, 78 parts of ethyl alcohol and 28.9 parts of water to be added in reaction kettle, mixing speed
For 160r/min, react 30min under the conditions of maintenance system temperature 45 C, by 15.7 parts of improved ferroferric oxide presomas according to
The adding rate of 0.07 part/min is added in reaction kettle, and product is transferred to water by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
In thermal response kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 125 DEG C of hydro-thermals
React 1.5h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 5
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 2.7 parts of water, 73 parts of ethyl alcohol and 0.9 part of cetomacrogol 1000 are weighed and is added to reaction kettle
In, mixing speed 125r/min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 14.6 parts of formic acid according to
The adding rate of 0.02 part/min is added in reaction kettle, the 1.9h that maintains under above-mentioned reaction condition that the reaction was continued, obtains four oxidations
Three-iron presoma；
(2), 18.9 parts of aluminium polychlorides, 58 parts of ethyl alcohol and 1.8 parts of Macrogol 600s are weighed to be added in reaction kettle, are stirred
Mixing speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, 51 parts of ferroso-ferric oxide presomas are pressed
It is added in reaction kettle according to the adding rate of 0.05 part/min, the 0.9h that maintains under above-mentioned reaction condition that the reaction was continued, by reaction kettle
Temperature is warming up to 67 DEG C of reaction 0.5h, obtains improved ferroferric oxide presoma；
(3), 0.4 part of benzoyl peroxide, 129 parts of own dioxanes, 2.3 parts of sorbester p18s, 59 parts of dichloroethanes, 1.3 parts are weighed
Polyvinyl alcohol 1788 and 0.04 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 44 DEG C of reaction 32min, by the mixed liquor of 36 parts of acrylic acid, 60 parts of acrylamides and 88 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 69 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 2.7h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow item
35min is reacted under part, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving poly- third
Olefin(e) acid ester；
(4), 83 parts of polyacrylate, 8.8 parts of Macrogol 600s, 9.2 parts of isomerous tridecanols, 7.8 parts of polyethylene glycol are weighed
400 and 0.5 parts of alchlors are added in reaction kettle, mixing speed 115r/min, 123 DEG C of maintenance system temperature, -0.08MPa
React 1.9h under the conditions of reduced-pressure backflow, product washs 3 times, 500mL ethyl alcohol through filtering, 650mL ethanol washing 2 times, 750mL methanol
It washs 3 times, dry to get modified polyacrylate is arrived；
(5), it weighs 81 parts of modified polyacrylates, 81 parts of ethyl alcohol and 32 parts of water to be added in reaction kettle, mixing speed is
160r/min reacts 30min under the conditions of maintenance system temperature 45 C, by 16.9 parts of improved ferroferric oxide presomas according to 0.07
The adding rate of part/min is added in reaction kettle, and it is anti-that product is transferred to hydro-thermal by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
It answers in kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 128 DEG C of hydro-thermal reactions
2.6h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 6
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 5 parts of water, 75 parts of ethyl alcohol and 1.9 parts of cetomacrogol 1000s are weighed to be added in reaction kettle,
Mixing speed is 125r/min, reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 14 parts of formic acid according to 0.02 part/
The adding rate of min is added in reaction kettle, the 4.5h that maintains under above-mentioned reaction condition that the reaction was continued, obtains ferroso-ferric oxide forerunner
Body；
(2), it weighs 19 parts of aluminium polychlorides, 60 parts of ethyl alcohol and 3 parts of Macrogol 600s to be added in reaction kettle, stirring speed
Degree is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas according to
The adding rate of 0.05 part/min is added in reaction kettle, the 2h that maintains under above-mentioned reaction condition that the reaction was continued, by temperature of reaction kettle
71 DEG C of reaction 0.6h are warming up to, improved ferroferric oxide presoma is obtained；
(3), 0.5 part of benzoyl peroxide, 138 parts of own dioxanes, 3.5 parts of sorbester p18s, 65 parts of dichloroethanes, 2.1 parts are weighed
Polyvinyl alcohol 1788 and 0.06 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 51 DEG C of reaction 40min, by the mixed liquor of 36 parts of acrylic acid, 61 parts of acrylamides and 90 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 70 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 2.5h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow item
35min is reacted under part, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving poly- third
Olefin(e) acid ester；
(4), 83 parts of polyacrylate, 8.8 parts of Macrogol 600s, 9.5 parts of isomerous tridecanols, 8.6 parts of polyethylene glycol are weighed
400 and 0.6 parts of alchlors are added in reaction kettle, mixing speed 115r/min, 123 DEG C of maintenance system temperature, -0.08MPa
React 3.5h under the conditions of reduced-pressure backflow, product washs 3 times, 500mL ethyl alcohol through filtering, 650mL ethanol washing 2 times, 750mL methanol
It washs 3 times, dry to get modified polyacrylate is arrived；
(5), it weighs 81 parts of modified polyacrylates, 83 parts of ethyl alcohol and 32 parts of water to be added in reaction kettle, mixing speed is
160r/min reacts 30min under the conditions of maintenance system temperature 45 C, by 18.5 parts of improved ferroferric oxide presomas according to 0.07
The adding rate of part/min is added in reaction kettle, and it is anti-that product is transferred to hydro-thermal by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
It answers in kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 141 DEG C of hydro-thermal reactions
3.6h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 7
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 7.8 parts of water, 81.3 parts of ethyl alcohol and 2.9 parts of cetomacrogol 1000s are weighed and are added to reaction
In kettle, mixing speed 125r/min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 20.7 parts of formic acid according to
The adding rate of 0.02 part/min is added in reaction kettle, the 4.6h that maintains under above-mentioned reaction condition that the reaction was continued, obtains four oxidations
Three-iron presoma；
(2), 22.8 parts of aluminium polychlorides, 67.9 parts of ethyl alcohol and 4.6 parts of Macrogol 600s are weighed to be added in reaction kettle,
Mixing speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas
It is added in reaction kettle according to the adding rate of 0.05 part/min, the 2.9h that maintains under above-mentioned reaction condition that the reaction was continued will react
Kettle temperature degree is warming up to 84 DEG C of reaction 0.9h, obtains improved ferroferric oxide presoma；
(3), 0.8 part of benzoyl peroxide, 149 parts of own dioxanes, 5.5 parts of sorbester p18s, 70 parts of dichloroethanes, 2.8 parts are weighed
Polyvinyl alcohol 1788 and 0.08 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 57 DEG C of reaction 43min, by the mixed liquor of 36 parts of acrylic acid, 67 parts of acrylamides and 96 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 78 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 4.5h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow item
35min is reacted under part, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving poly- third
Olefin(e) acid ester；
(4), 83 parts of polyacrylate, 10.8 parts of Macrogol 600s, 11.6 parts of isomerous tridecanols, 9.6 parts of poly- second two are weighed
Alcohol 400 and 0.8 part alchlor is added in reaction kettle, mixing speed 115r/min, 136 DEG C of maintenance system temperature ,-
React 4.5h under the conditions of 0.08MPa reduced-pressure backflow, product through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times,
It is 500mL ethanol washing 3 times, dry to get arriving modified polyacrylate；
(5), it weighs 81 parts of modified polyacrylates, 88 parts of ethyl alcohol and 40.6 parts of water to be added in reaction kettle, mixing speed
For 160r/min, react 30min under the conditions of maintenance system temperature 45 C, by 20.8 parts of improved ferroferric oxide presomas according to
The adding rate of 0.07 part/min is added in reaction kettle, and product is transferred to water by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
In thermal response kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 145 DEG C of hydro-thermals
React 5.5h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Embodiment 8
A kind of sewage scavenging material, preparation method includes the following steps:
(1), 36 parts of ferric trichlorides, 6.5 parts of water, 78 parts of ethyl alcohol and 2.2 parts of cetomacrogol 1000s are weighed and are added to reaction kettle
In, mixing speed 125r/min reacts 16min under the conditions of 65 DEG C of maintenance system reaction temperature, by 18.5 parts of formic acid according to
The adding rate of 0.02 part/min is added in reaction kettle, the 3.5h that maintains under above-mentioned reaction condition that the reaction was continued, obtains four oxidations
Three-iron presoma；
(2), 21 parts of aluminium polychlorides, 66 parts of ethyl alcohol and 3.7 parts of Macrogol 600s are weighed to be added in reaction kettle, are stirred
Speed is 100r/min, reacts 25min under the conditions of 50 DEG C of maintenance system reaction temperature, by 51 parts of ferroso-ferric oxide presomas according to
The adding rate of 0.05 part/min is added in reaction kettle, the 2.2h that maintains under above-mentioned reaction condition that the reaction was continued, will react kettle temperature
Degree is warming up to 81 DEG C of reaction 0.7h, obtains improved ferroferric oxide presoma；
(3), 0.6 part of benzoyl peroxide, 141 parts of own dioxanes, 3.9 parts of sorbester p18s, 64 parts of dichloroethanes, 2.1 parts are weighed
Polyvinyl alcohol 1788 and 0.07 part N, N- methylene-bisacrylamide is added in reaction kettle, mixing speed 140r/min, instead
Answering temperature is 55 DEG C of reaction 41min, by the mixed liquor of 36 parts of acrylic acid, 66 parts of acrylamides and 91 parts of water according to 0.09 part/min
Adding rate be added in reaction kettle, temperature of reaction kettle is warming up to 73 by the 1.5h that maintains under above-mentioned reaction condition that the reaction was continued
DEG C reaction 3.3h, temperature of reaction kettle is warming up to 95 DEG C of heat preservation 25min, by reaction kettle in 100 DEG C, -0.06MPa reduced-pressure backflow item
35min is reacted under part, reaction kettle is cooled to 45 DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving poly- third
Olefin(e) acid ester；
(4), 83 parts of polyacrylate, 9.8 parts of Macrogol 600s, 10.2 parts of isomerous tridecanols, 8.6 parts of poly- second two are weighed
Alcohol 400 and 0.9 part alchlor is added in reaction kettle, mixing speed 115r/min, 135 DEG C of maintenance system temperature ,-
React 3.8h under the conditions of 0.08MPa reduced-pressure backflow, product through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times,
It is 500mL ethanol washing 3 times, dry to get arriving modified polyacrylate；
(5), it weighs 81 parts of modified polyacrylates, 87 parts of ethyl alcohol and 38.6 parts of water to be added in reaction kettle, mixing speed
For 160r/min, react 30min under the conditions of maintenance system temperature 45 C, by 19.6 parts of improved ferroferric oxide presomas according to
The adding rate of 0.07 part/min is added in reaction kettle, and product is transferred to water by the 2h that maintains under above-mentioned reaction condition that the reaction was continued
In thermal response kettle, maintenance hydrothermal temperature is 86 DEG C of hydro-thermal reaction 45min, and hydrothermal temperature is warming up to 141 DEG C of hydro-thermals
React 4.5h, product is through filtering, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
Reference examples 1
In this reference examples, ferroso-ferric oxide presoma is not added, and other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, improved ferroferric oxide presoma, other components and preparation method and 1 phase of embodiment are not added
Together.
Reference examples 3
In this reference examples, polyacrylate is not added, other components and preparation method are same as Example 1.Reference examples 4
In this reference examples, modified polyacrylate is not added, other components and preparation method are same as Example 1.Control
Example 5
The ferroso-ferric oxide presoma in common ferroso-ferric oxide alternate embodiment 1 is selected in this reference examples, in formula,
Its component and preparation method are same as Example 1.
Reference examples 6
The improved ferroferric oxide forerunner in common ferroso-ferric oxide alternate embodiment 1 is selected in this reference examples, in formula
Body, other components and preparation method are same as Example 1.
Reference examples 7
The polyacrylate in plain polypropylene acid esters alternate embodiment 1, other components are selected in this reference examples, in formula
It is same as Example 1 with preparation method.
Reference examples 8
The modified polyacrylate in plain polypropylene acid esters alternate embodiment 1 is selected in this reference examples, in formula, it is other
Component is same as Example 1 with preparation method.
It is 2000mg/ with COD content in sewage to sewage scavenging material made from Examples 1 to 8 and reference examples 1~8
L is staying water sample；COD content is tested according to HJ/T 399-2007, and test result sees below Tables 1 and 2.
The performance parameter of sewage scavenging material made from 1 Examples 1 to 8 of table
The performance parameter of sewage scavenging material made from 2 embodiment 1 of table and reference examples 1~8
By upper Tables 1 and 2 it is found that the reduction water body COD for the sewage scavenging material that various embodiments of the present invention are prepared
Performance and recuperability performance are more excellent, this show the sewage being prepared with raw material provided by the invention with scavenging material have compared with
Good reduction water body COD performance and recuperability performance；In contrast, the sewage purification that the raw material of each reference examples is prepared
The reduction water body COD performance and recuperability performance of material are poor.In addition, the sewage that various embodiments of the present invention are prepared is with only
Changing material has preferable reduction water body COD performance and recuperability.
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art
For, under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as
The protection scope of the invention.
Claims (3)
1. a kind of sewage scavenging material, which is characterized in that changed by mass parts ratio for 81:15~21:75~90:28~41
Property polyacrylate, improved ferroferric oxide presoma, second alcohol and water composition；Wherein, the modified polyacrylate is by matter
Amount portion rate is 83:6~11:7~12:5~10:0.3~1 polyacrylate, Macrogol 600, isomerous tridecanol, poly- second
Glycol 400 and alchlor reaction are made；The polyacrylate is 36:57~69:82~100:0.2 by mass parts ratio
~1:121~150:1~6:56~71:0.5~3:0.02~0.1 acrylic acid, acrylamide, water, benzoyl peroxide, oneself
Dioxane, sorbester p18, dichloroethanes, polyvinyl alcohol 1788 and N,N methylene bis acrylamide reaction are made；The modification four
Fe 3 O presoma is by mass parts ratio 51:17~23:53~70:0.8~5 ferroso-ferric oxide presoma, polyaluminium
Aluminium, ethyl alcohol and Macrogol 600 reaction are made；The ferroso-ferric oxide presoma is 36:8.7~21:2 by mass parts ratio
Ferric trichloride, formic acid, water, ethyl alcohol and the cetomacrogol 1000 reaction of~8:68~83:0.3~3 are made.
2. sewage scavenging material according to claim 1, which is characterized in that the modified polyacrylate, modified four
Fe 3 O presoma, second alcohol and water mass parts ratio be 81:19.5:86:34.
3. the preparation method of any sewage scavenging material of claim 1~2, which comprises the steps of:
(1), ferric trichloride, water, ethyl alcohol and cetomacrogol 1000 are added in reaction kettle, mixing speed 125r/min, are tieed up
16min is reacted under the conditions of holding 65 DEG C of system reaction temperature, formic acid is added to instead according to 0.02 mass parts/min adding rate
It answers in kettle, the 1~5h that maintains under above-mentioned reaction condition that the reaction was continued obtains ferroso-ferric oxide presoma；
(2), aluminium polychloride, ethyl alcohol and Macrogol 600 are added in reaction kettle, mixing speed 100r/min, are maintained
25min is reacted under the conditions of 50 DEG C of system reaction temperature, by ferroso-ferric oxide presoma according to 0.05 mass parts/min addition speed
Rate is added in reaction kettle, the 0.5~3h that maintains under above-mentioned reaction condition that the reaction was continued, and temperature of reaction kettle is warming up to 60~85 DEG C
0.2~1h is reacted, improved ferroferric oxide presoma is obtained；
(3), by benzoyl peroxide, own dioxane, sorbester p18, dichloroethanes, polyvinyl alcohol 1788 and N, N- methylene bisacrylamide
Amide is added in reaction kettle, mixing speed 140r/min, and reaction temperature is 41~58 DEG C of 28~45min of reaction, by propylene
The mixed liquor of acid, acrylamide and water is added in reaction kettle according to 0.09 mass parts/min adding rate, remains above-mentioned anti-
The reaction was continued under the conditions of answering 1.5h, is warming up to 61~80 DEG C of 1~5h of reaction for temperature of reaction kettle, temperature of reaction kettle is warming up to 95
DEG C heat preservation 25min, reaction kettle is reacted into 35min under the conditions of 100 DEG C, -0.06MPa reduced-pressure backflow, reaction kettle is cooled to 45
DEG C, product is through filtering, 900mL ethanol washing 5 times, dry to get arriving polyacrylate；
(4), polyacrylate, Macrogol 600, isomerous tridecanol, polyethylene glycol 400 and alchlor are added to reaction kettle
In, mixing speed 115r/min reacts 1~5h under the conditions of 119~137 DEG C of maintenance system temperature, -0.08MPa reduced-pressure backflow, produces
Object through filtering, 650mL ethanol washing 2 times, 750mL methanol wash 3 times, it is 500mL ethanol washing 3 times, dry to get to modified poly-
Acrylate；
(5), modified polyacrylate, second alcohol and water are added in reaction kettle, mixing speed 160r/min, maintenance system temperature
30min is reacted under the conditions of 45 DEG C of degree, improved ferroferric oxide presoma is added according to 0.07 mass parts/min adding rate
Into reaction kettle, maintaining under above-mentioned reaction condition that the reaction was continued, product is transferred in hydrothermal reaction kettle by 2h, maintains hydro-thermal reaction
Temperature is 86 DEG C of hydro-thermal reaction 45min, hydrothermal temperature is warming up to 123~146 DEG C of 1~6h of hydro-thermal reaction, product passes through
It is filter, 900mL ethanol washing 5 times, dry to get to sewage scavenging material.
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