CN112551669A - Water treatment flocculant with high settling velocity and preparation method thereof - Google Patents
Water treatment flocculant with high settling velocity and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 25
- 239000003999 initiator Substances 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229920002472 Starch Polymers 0.000 claims description 49
- 239000008107 starch Substances 0.000 claims description 43
- 235000019698 starch Nutrition 0.000 claims description 43
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 20
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 20
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 20
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 20
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 20
- 229920000926 Galactomannan Polymers 0.000 claims description 18
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 claims description 17
- XFHJDMUEHUHAJW-UHFFFAOYSA-N n-tert-butylprop-2-enamide Chemical compound CC(C)(C)NC(=O)C=C XFHJDMUEHUHAJW-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 229920005615 natural polymer Polymers 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 229920001592 potato starch Polymers 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 244000017020 Ipomoea batatas Species 0.000 claims description 6
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 6
- 240000003183 Manihot esculenta Species 0.000 claims description 6
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 6
- 235000003283 Pachira macrocarpa Nutrition 0.000 claims description 6
- 235000014364 Trapa natans Nutrition 0.000 claims description 6
- 240000004922 Vigna radiata Species 0.000 claims description 6
- 235000010721 Vigna radiata var radiata Nutrition 0.000 claims description 6
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 claims description 6
- 235000009165 saligot Nutrition 0.000 claims description 6
- 229940100445 wheat starch Drugs 0.000 claims description 6
- 229920002521 macromolecule Polymers 0.000 claims description 5
- 229920002261 Corn starch Polymers 0.000 claims description 4
- 239000008120 corn starch Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000012716 precipitator Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- YQIGLEFUZMIVHU-UHFFFAOYSA-N 2-methyl-n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C(C)=C YQIGLEFUZMIVHU-UHFFFAOYSA-N 0.000 claims description 3
- 244000151018 Maranta arundinacea Species 0.000 claims description 3
- 235000010804 Maranta arundinacea Nutrition 0.000 claims description 3
- 240000002853 Nelumbo nucifera Species 0.000 claims description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 3
- 235000012419 Thalia geniculata Nutrition 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 229920005610 lignin Polymers 0.000 claims description 3
- VQGWOOIHSXNRPW-UHFFFAOYSA-N n-butyl-2-methylprop-2-enamide Chemical compound CCCCNC(=O)C(C)=C VQGWOOIHSXNRPW-UHFFFAOYSA-N 0.000 claims description 3
- CNPHCSFIDKZQAK-UHFFFAOYSA-N n-prop-2-enylprop-2-enamide Chemical compound C=CCNC(=O)C=C CNPHCSFIDKZQAK-UHFFFAOYSA-N 0.000 claims description 3
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- 240000001085 Trapa natans Species 0.000 claims 2
- 239000006185 dispersion Substances 0.000 abstract description 5
- 238000005345 coagulation Methods 0.000 abstract description 3
- 230000015271 coagulation Effects 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 8
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 241001083492 Trapa Species 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000008394 flocculating agent Substances 0.000 description 4
- 229920002401 polyacrylamide Polymers 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- 239000010865 sewage Substances 0.000 description 1
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- 239000007858 starting material Substances 0.000 description 1
- 229920005613 synthetic organic polymer Polymers 0.000 description 1
- -1 thallus cells Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/02—Odour removal or prevention of malodour
Abstract
The invention relates to the technical field of water treatment, in particular to a water treatment flocculant with a high settling velocity and a preparation method thereof. The raw materials comprise: according to the weight portion, the polymerization monomer is 15-72 portions, the natural high molecular compound is 1-10 portions, and the initiator is 0.1-2 portions. The water treatment flocculant prepared by the invention has excellent performance, and the existence of the optimized high-efficiency adsorption component can adsorb organic matters and heavy metal ions which are difficult to flocculate and precipitate, and has the functions of coagulation aiding, color and odor removing. The flocculant has excellent dispersion performance, is not easy to agglomerate, has the characteristics of high settling speed, good effluent quality, small dosage and the like when being applied to water quality treatment, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a water treatment flocculant with a high settling velocity and a preparation method thereof.
Background
Water treatment refers to physical and chemical measures taken to make water quality meet certain use standards, and aims to improve water quality. According to the different treatment methods, the method can be divided into physical water treatment, chemical water treatment, biological water treatment and the like. Sewage treatment and drinking water treatment can be classified according to different treatment objects. The core of the realization of the water treatment target lies in the selection of water treatment technology and water treatment medicament, and the water treatment medicament not only has good water purification effect, but also can not cause 2 times of pollution. In the course of water treatment, flocculants play an essential role as water treatment agents for enhancing solid-liquid separation.
Flocculants are various in variety and can be classified into inorganic flocculants and organic flocculants according to the total chemical components. Wherein the inorganic flocculant also comprises an inorganic coagulant and an inorganic polymeric flocculant; the organic flocculant also comprises a synthetic organic polymer flocculant, a natural organic polymer flocculant and a microbial flocculant. The inorganic flocculant is low in price, but has adverse effects on human health and ecological environment; although the organic polymeric flocculant has less consumption, less scum yield and strong flocculation capability, the residual monomer of the organic polymeric flocculant has the hidden troubles of teratogenesis, carcinogenesis and mutagenesis, thereby limiting the application range of the organic polymeric flocculant; the microbial flocculant is a special macromolecular metabolite which is generated by microorganisms and can cause the coagulation and precipitation of solid suspended particles, thallus cells, colloid particles and the like which are not easy to settle in liquid, has wide flocculation objects and unique decoloration effect, but is not popularized in the field of actual production of water treatment.
Based on the above, the preparation of a cheap, practical, nontoxic and efficient water treatment flocculant becomes a problem to be solved in the field.
Disclosure of Invention
The invention provides the water treatment flocculant with high settling velocity and the preparation method thereof, which solve the defects of low floc strength of the organic flocculant and large potential safety hazard of residual monomers; the prepared flocculant can efficiently adsorb pollutants in water, has excellent dispersion performance and is not easy to agglomerate.
The invention provides a water treatment flocculant with high settling velocity, which comprises the following raw materials: according to the weight portion, the polymerization monomer is 15-72 portions, the natural high molecular compound is 1-10 portions, and the initiator is 0.1-2 portions.
In a preferred embodiment, the feed of the fast settling water treatment flocculant comprises: 26-54 parts of polymerized monomer, 2-7 parts of natural macromolecular compound and 0.2-0.8 part of initiator according to parts by weight.
In a preferred embodiment, the polymerizable monomer is at least one of acrylamide, N-isopropyl methacrylamide, N-tert-butyl acrylamide, N-isopropyl acrylamide, N-allyl acrylamide, and N-N-butyl methacrylamide.
In a preferred embodiment, the polymerized monomers are acrylamide and N-t-butylacrylamide.
In a preferred embodiment, the weight ratio of acrylamide to N-t-butylacrylamide is (3-6): 1.
in a preferred embodiment, the natural polymer compound comprises at least one of starch, protein, lignin, cellulose, carboxymethyl cellulose, and galactomannan.
In a preferred embodiment, the natural polymer compound includes starch, carboxymethyl cellulose and galactomannan.
In a preferred embodiment, the weight ratio of starch, carboxymethyl cellulose and galactomannan is (1-4): (2-6): 1.
in a preferred embodiment, the starch is selected from at least one of mung bean starch, potato starch, wheat starch, sweet potato starch, water chestnut starch, lotus root starch, water chestnut starch, corn starch, sweet potato starch, arrowroot starch and tapioca starch.
The invention provides a preparation method of a water treatment flocculant with high settling velocity, which comprises the following specific steps:
s1, dissolving a natural high molecular compound;
s2, under nitrogen atmosphere, adding the natural high molecular compound obtained in the step S1 into a four-mouth bottle, adding an initiator, stirring at the speed of 40-60r/min for 3-5min, adding a polymerization monomer, keeping the temperature at 30-50 ℃, and stirring at 50-240r/min for 1-3 h;
s3, adding a precipitator, stirring at the speed of 40-80r/min until no white substance is separated out, carrying out suction filtration and drying to obtain white powder, refluxing the white powder for 6-10h by using acetone, and drying to obtain a finished flocculant product.
Has the advantages that:
the water treatment flocculant prepared by the invention has excellent performance, and the existence of the optimized high-efficiency adsorption component can adsorb organic matters and heavy metal ions which are difficult to flocculate and precipitate, and has the functions of coagulation aiding, color and odor removing. The flocculant has excellent dispersion performance, is not easy to agglomerate, has the characteristics of high settling speed, good effluent quality, small dosage and the like when being applied to water quality treatment, and has wide application prospect.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present application, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. In addition, the starting materials for the present invention are commercially available unless otherwise specified.
In order to solve the above problems, the invention provides, in a first aspect, a water treatment flocculant with a high settling rate, which comprises the following raw materials: according to the weight portion, the polymerization monomer is 15-72 portions, the natural high molecular compound is 1-10 portions, and the initiator is 0.1-2 portions.
In some preferred embodiments, the high settling rate water treatment flocculant comprises: 26-54 parts of polymerized monomer, 2-7 parts of natural macromolecular compound and 0.2-0.8 part of initiator according to parts by weight.
In some preferred embodiments, the polymerized monomer is at least one of acrylamide, N-isopropyl methacrylamide, N-tert-butyl acrylamide, N-isopropyl acrylamide, N-allyl acrylamide, N-N-butyl methacrylamide.
In some preferred embodiments, the polymerized monomers are acrylamide and N-t-butylacrylamide.
In some preferred embodiments, the weight ratio of acrylamide to N-t-butylacrylamide is (3-6): 1.
in some preferred embodiments, the initiator is ammonium persulfate (CAS number 7727-54-0) and/or sodium bisulfite (CAS number 7631-90-5).
In some preferred embodiments, the initiator is ammonium persulfate and sodium bisulfite in a weight ratio of 1: (0.7-1.5).
In some preferred embodiments, the natural polymer compound comprises at least one of starch, protein, lignin, cellulose, carboxymethyl cellulose, and galactomannan.
In some preferred embodiments, the natural polymers include starch, carboxymethyl cellulose and galactomannan.
In some preferred embodiments, the weight ratio of starch, carboxymethyl cellulose and galactomannan is (1-4): (2-6): 1.
in some preferred embodiments, the starch is selected from at least one of mung bean starch, potato starch, wheat starch, sweet potato starch, water chestnut starch, lotus root starch, water chestnut starch, corn starch, sweet potato starch, arrowroot starch, tapioca starch.
According to the invention, acrylamide monomers are selected for polymerization, and a composite space reticular structure is obtained under the synergistic effect of natural high molecular compounds, the product is supported by a natural high molecular skeleton, and a polyacrylamide molecular chain containing an active group is grafted, so that the stability of colloid in water can be rapidly lost when the product is applied to wastewater, the collision and aggregation between colloidal particles are promoted, and the colloidal particles are aggregated and settled.
The applicant further finds that the active crosslinking points of the polymer are increased by adopting acrylamide (CAS No. 79-06-1) and N-tertiary butyl acrylamide (CAS No. 107-58-4) for polymerization, and the grafting rate of the polyacrylamide is effectively improved; when the weight ratio of the acrylamide to the N-tertiary butyl acrylamide is (3-6): 1, the grafting rate can reach more than 60 percent; it is possible that the weight ratio of acrylamide to N-tert-butylacrylamide is (3-6): 1, the monomer moves to the natural high molecular compound rapidly and orderly, the monomer polymerization and the grafting reaction reach dynamic balance, the acrylamide monomer participates in the reaction to the maximum extent, and the grafting rate of the product is improved.
The grafting rate is determined by a method commonly used in the field, and specifically can be determined by a weight method:
K＝(m2-m1)/m1×100％
wherein K is the grafting rate and the unit is%; m2 represents the mass of the natural polymer compound before the reaction, and m1 represents the mass of the product after the reaction.
The applicant also finds that the removal capacity of the flocculant can be further improved by adopting the synergistic effect of the starch, the carboxymethyl cellulose and the galactomannan, and the prepared flocculant can be effectively adsorbed on the surface of fine particles to promote collision, adhesion and coprecipitation of colloidal particles in a water body. And when the weight ratio of the starch, the carboxymethyl cellulose and the galactomannan is (1-4): (2-6): 1, the removal rate of COD in the water body can reach 80%, and the removal rate of COD in the wastewater can reach the highest when the reaction time is 85min, wherein the weight ratio is (1-4): (2-6): 1, the skeleton formed by the starch, the carboxymethyl cellulose and the galactomannan is firmly combined with the polyacrylamide to form a macromolecular reticular structure in a water dispersion phase, so that the polymerization inhibition potential of colloidal particles is effectively reduced, and the effect of efficiently removing colloidal substances in the water can be achieved in a short time.
The applicant also unexpectedly finds that when the initiator is the combined action of ammonium persulfate and sodium bisulfite, the phenomenon of difficult dissolution and agglomeration of polyacrylamide is obviously improved, the polymerization of acrylamide monomers and the grafting with natural high molecular compounds are carried out in a stable reaction process, the obtained macromolecular reticular polymer is uniformly dispersed, the agglomeration phenomenon is inhibited, and the dispersing performance of the flocculant is excellent. The invention provides a preparation method of a water treatment flocculant with high settling velocity, which comprises the following specific preparation steps:
s1, dissolving a natural high molecular compound;
s2, under nitrogen atmosphere, adding the natural high molecular compound obtained in the step S1 into a four-mouth bottle, adding an initiator, stirring at the speed of 40-60r/min for 3-5min, adding a polymerization monomer, keeping the temperature at 30-50 ℃, and stirring at 50-240r/min for 1-3 h;
s3, adding a precipitator, stirring at the speed of 40-80r/min until no white substance is separated out, carrying out suction filtration and drying to obtain white powder, refluxing the white powder for 6-10h by using acetone, and drying to obtain a finished flocculant product.
In some preferred embodiments, the precipitating agent is absolute ethanol.
In some preferred embodiments, the step of dissolving the natural polymer compound comprises: mixing starch and water according to a weight ratio of 1: (10-20) dissolving, setting the temperature at 70-90 ℃, stirring at the speed of 80-150r/min to paste, adding carboxymethyl cellulose and galactomannan, continuously stirring for 0.5-2h, and cooling to 35-45 ℃ to obtain the dissolved natural polymer compound.
Examples
Example 1.
A water treatment flocculant with high settling velocity comprises the following raw materials: 60 parts of polymerized monomer, 8 parts of natural macromolecular compound and 0.7 part of initiator according to parts by weight.
The polymerization monomers are acrylamide (CAS number 79-06-1) and N-tert-butyl acrylamide (CAS number 107-58-4); the weight ratio of the acrylamide to the N-tertiary butyl acrylamide is 5: 1.
the initiator is ammonium persulfate (CAS number 7727-54-0) and sodium bisulfite (CAS number 7631-90-5), and the weight ratio of the ammonium persulfate to the sodium bisulfite is 1: 1.2.
the natural high molecular compound is starch, carboxymethyl cellulose and galactomannan.
The carboxymethyl cellulose was purchased from oku biotechnology limited, jiang.
The galactomannans are purchased from Henan Rinderea bioengineering, Inc.
The weight ratio of the starch to the carboxymethyl cellulose to the galactomannan is 2: 5: 1.
the starch is mung bean starch, cassava flour and wheat starch; the weight ratio of the mung bean starch, the cassava powder and the wheat starch is 1: 2: 1.
the mung bean starch is purchased from cigarette Tai double-tower food products GmbH, the cassava flour is purchased from China Jade Biotechnology GmbH, Dongying, and the wheat starch is purchased from Shandong multiple-harvest chemical GmbH.
The preparation method of the water treatment flocculant with high settling speed comprises the following steps:
s1, dissolving a natural high molecular compound;
s2, under nitrogen atmosphere, adding the natural high molecular compound obtained in the step S1 into a four-mouth bottle, adding an initiator, stirring for 3min at the speed of 45r/min, adding a polymerization monomer, keeping the temperature at 40 ℃, and stirring for 3h at 160 r/min;
s3, adding a precipitator, stirring at the speed of 60r/min until no white substance is separated out, carrying out suction filtration and drying to obtain white powder, refluxing the white powder for 8 hours by using acetone, and drying to obtain a finished flocculant product.
The precipitant is absolute ethyl alcohol.
The step of dissolving the natural polymer compound includes: mixing starch and water according to a weight ratio of 1: 15 dissolving, setting the temperature at 75 ℃, stirring at the speed of 100r/min to be pasty, adding carboxymethyl cellulose and galactomannan, continuously stirring for 1h, and cooling to 40 ℃ to obtain the dissolved natural high molecular compound.
Example 2.
The specific implementation mode of the water treatment flocculant with high settling velocity is the same as that of example 1. The difference is that the weight ratio of the acrylamide to the N-tertiary butyl acrylamide is 1: 1.
example 3.
The specific implementation mode of the water treatment flocculant with high settling velocity is the same as that of example 1. The difference is that the natural high molecular compound is carboxymethyl cellulose;
the step of dissolving the natural polymer compound includes: mixing carboxymethyl cellulose and water according to the weight ratio of 1: 15, setting the temperature at 75 ℃, stirring for 1h at the speed of 100r/min, and cooling to 40 ℃ to obtain the dissolved natural macromolecular compound.
Example 4.
The specific implementation mode of the water treatment flocculant with high settling velocity is the same as that of example 1. The difference is that the weight ratio of the starch, the carboxymethyl cellulose and the galactomannan is 1: 1: 1.
example 5.
The specific implementation mode of the water treatment flocculant with high settling velocity is the same as that of example 1. The difference is that the starch is corn starch, and is purchased from Jinan constant chemical industry Co.
Example 6.
The specific implementation mode of the water treatment flocculant with high settling velocity is the same as that of example 1. Except that the temperature in the step of S2 was 55 ℃.
Performance test method
COD removal rate and optimal reaction time:
the pH of the wastewater (COD-519.792) was adjusted to 7, the flocculant samples prepared in the examples were put into the wastewater at an input of 100mg/L, the samples were taken at regular intervals, the COD concentration of the wastewater after the reaction was measured, the removal rate of COD in the water was calculated, and the optimum reaction time corresponding to the maximum removal rate was recorded.
COD was determined according to national standard GB/T32208-2015.
Evaluation of dispersibility:
a 5-person sensory panel was established and scored for the degree of dispersion of the flocculant into water. The evaluation scale was from 0 (poor dispersibility, easy caking) to 5 (good dispersibility, difficult caking).
Performance test data
TABLE 1 results of the Performance test of the samples of examples 1-6
| Removal rate% | Optimum reaction time min | Dispersibility | |
| Example 1 | 81.3 | 85 | 5 |
| Example 2 | 63.4 | 117 | 3 |
| Example 3 | 56.7 | 103 | 3 |
| Example 4 | 62.9 | 98 | 4 |
| Example 5 | 48.2 | 106 | 2 |
| Example 6 | 52.8 | 94 | 2 |
Finally, it is pointed out that the foregoing examples are illustrative only, serving to explain some of the characteristics of the process according to the invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. A water treatment flocculant with high settling velocity is characterized by comprising the following raw materials: according to the weight portion, the polymerization monomer is 15-72 portions, the natural high molecular compound is 1-10 portions, and the initiator is 0.1-2 portions.
2. The flocculant for water treatment according to claim 1, which is prepared from the following raw materials: 26-54 parts of polymerized monomer, 2-7 parts of natural macromolecular compound and 0.2-0.8 part of initiator according to parts by weight.
3. The water treatment flocculant with high settling velocity according to claim 1, wherein the polymeric monomer is at least one of acrylamide, N-isopropyl methacrylamide, N-tert-butyl acrylamide, N-isopropyl acrylamide, N-allyl acrylamide and N-N-butyl methacrylamide.
4. The water treatment flocculant with high settling velocity according to claim 3, wherein the polymerized monomers are acrylamide and N-tert-butylacrylamide.
5. The water treatment flocculant with high settling speed according to claim 4, wherein the weight ratio of acrylamide to N-tert-butyl acrylamide is (3-6): 1.
6. the flocculant according to claim 1, wherein the natural polymer compound is at least one of starch, protein, lignin, cellulose, carboxymethyl cellulose and galactomannan.
7. The flocculant according to claim 6, wherein the natural polymer compound includes starch, carboxymethyl cellulose and galactomannan.
8. The flocculant for water treatment with high settling rate according to claim 7, wherein the weight ratio of the starch, the carboxymethyl cellulose and the galactomannan is (1-4): (2-6): 1.
9. the water treatment flocculant with a high settling rate as claimed in claim 6, wherein the starch is at least one selected from the group consisting of mung bean starch, potato starch, wheat starch, sweet potato starch, water chestnut starch, lotus root starch, water chestnut starch, corn starch, sweet potato starch, arrowroot starch and tapioca starch.
10. The preparation method of the water treatment flocculant with high settling speed according to any one of claims 1 to 9, characterized by comprising the following specific preparation steps:
s1, dissolving a natural high molecular compound;
s2, under nitrogen atmosphere, adding the natural high molecular compound obtained in the step S1 into a four-mouth bottle, adding an initiator, stirring at the speed of 40-60r/min for 3-5min, adding a polymerization monomer, keeping the temperature at 30-50 ℃, and stirring at 50-240r/min for 1-3 h;
s3, adding a precipitator, stirring at the speed of 40-80r/min until no white substance is separated out, carrying out suction filtration and drying to obtain white powder, refluxing the white powder for 6-10h by using acetone, and drying to obtain a finished flocculant product.
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| US6020422A (en) * | 1996-11-15 | 2000-02-01 | Betzdearborn Inc. | Aqueous dispersion polymers |
| CN101935377A (en) * | 2010-07-26 | 2011-01-05 | 北京化工大学 | Method for preparing flocculating agent used for solid-liquid separation treatment of waste drilling fluid |
| JP2013094720A (en) * | 2011-10-31 | 2013-05-20 | Sanyo Chem Ind Ltd | Organic coagulant |
| WO2016144645A1 (en) * | 2015-03-10 | 2016-09-15 | Baker Hughes Incorporated | Cement spacer system for wellbores, methods of making, and methods of use |
| CN106335988A (en) * | 2015-07-06 | 2017-01-18 | 迪建东 | Composite high polymer flocculant for coking wastewater and preparation method thereof |
| CN109535319A (en) * | 2018-11-07 | 2019-03-29 | 济宁明升新材料有限公司 | A kind of environmentally friendly drying strengthening agent and preparation method thereof |
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2020
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6020422A (en) * | 1996-11-15 | 2000-02-01 | Betzdearborn Inc. | Aqueous dispersion polymers |
| CN101935377A (en) * | 2010-07-26 | 2011-01-05 | 北京化工大学 | Method for preparing flocculating agent used for solid-liquid separation treatment of waste drilling fluid |
| JP2013094720A (en) * | 2011-10-31 | 2013-05-20 | Sanyo Chem Ind Ltd | Organic coagulant |
| WO2016144645A1 (en) * | 2015-03-10 | 2016-09-15 | Baker Hughes Incorporated | Cement spacer system for wellbores, methods of making, and methods of use |
| CN106335988A (en) * | 2015-07-06 | 2017-01-18 | 迪建东 | Composite high polymer flocculant for coking wastewater and preparation method thereof |
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