CN111003774A - Modified water treatment agent and preparation method thereof - Google Patents
Modified water treatment agent and preparation method thereof Download PDFInfo
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- CN111003774A CN111003774A CN201911371942.XA CN201911371942A CN111003774A CN 111003774 A CN111003774 A CN 111003774A CN 201911371942 A CN201911371942 A CN 201911371942A CN 111003774 A CN111003774 A CN 111003774A
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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
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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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
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a modified water treatment agent and a preparation method thereof, wherein the modified water treatment agent is prepared from the following raw materials in parts by weight: 100-140 parts of acrylamide, 3-4 parts of ammonium persulfate, 1-2 parts of isooctyl thioglycolate, 2.5-3 parts of allyl triphenyl phosphonium bromide, 0.01-0.02 part of initiator, 10-20 parts of microcrystalline cellulose, 1-2 parts of polyglycerol fatty acid ester, 30-40 parts of calcium zeolite and 1-3 parts of aluminum dihydrogen phosphate. The adsorbability of the calcium zeolite can play a good synergistic effect with the bacteriostatic and purifying properties of the quaternary phosphonium microcrystalline cellulose and the flocculating property of polyacrylamide, and particularly has a better purifying effect on sewage with suspended particles carrying negative charges, so that a higher purifying effect is achieved.
Description
Technical Field
The invention belongs to the field of water treatment, and particularly relates to a modified water treatment agent and a preparation method thereof.
Background
The water treatment agent means a chemical agent for water treatment. Generally referred to as chemicals used in sewage treatment. The method is widely applied to the industries of chemical industry, petroleum, light industry, daily chemicals, textile, printing and dyeing, construction, metallurgy, machinery, medicine and health, traffic, urban and rural environmental protection and the like, so as to achieve the purposes of saving water and preventing water source pollution. Comprises agents required by technologies such as treatment of cooling water and boiler water, seawater desalination, membrane separation, biological treatment, flocculation, ion exchange and the like. Such as corrosion inhibitor, scale inhibition and dispersion agent, sterilization algicide, flocculant, ion exchange resin, purifying agent, cleaning agent, prefilming agent and the like; the water treating agent is a generic name of chemical agents for water treatment, and is widely used in industrial departments of petroleum, chemical industry, metallurgy, traffic, light industry, textile and the like. The water treatment agent comprises a corrosion inhibitor, a scale inhibitor, a bactericide, a flocculating agent, a purifying agent, a cleaning agent, a prefilming agent and the like. In practical application, a water treatment agent with a compound formula is often used, or various water treatment agents are comprehensively applied. Therefore, attention is paid to the fact that the synergistic effect (synergistic effect generated when several medicaments coexist) is fully utilized to realize the synergy, and the components are not properly compounded to generate the antagonistic effect so as to reduce or lose the effect. In addition, most water treatment systems are open systems, and have a certain discharge amount, and the influence of various water treatment agents on the environment needs to be considered when the system is used. The common water treatment agents comprise flocculating agent, ferrous sulfate heptahydrate, polymeric ferric salt, calcium hydroxide, ferric chloride hexahydrate, bactericidal algicide, chlorine dioxide, scale and corrosion inhibitor, polyacrylamide (cation, anion and nonionic), polyaluminium chloride, polyaluminium ferric chloride, ferrous sulfate and the like.
The water treatment agent is one of the most widely applied and most used special products in the current water industry, pollution treatment and water-saving recycling treatment engineering technology, comprises a flocculating agent, a scale inhibition and dispersion agent, a corrosion inhibitor, a biocide and the like, is mainly used for removing suspended solids and toxic substances in water, controlling the formation of scale and sludge, reducing the corrosion to water contact materials, deodorizing and sterilizing, decoloring, softening and stabilizing water quality and seawater;
however, the existing water treatment agent has the defects of low reuse rate and low treatment efficiency, and some water bodies can be polluted to a certain extent.
Disclosure of Invention
The invention aims to provide a modified water treatment agent and a preparation method thereof aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a modified water treatment agent is composed of the following raw materials in parts by weight:
100-140 parts of acrylamide, 3-4 parts of ammonium persulfate, 6-9 parts of allyl triphenyl phosphonium bromide, 0.01-0.02 part of initiator, 10-20 parts of microcrystalline cellulose, 1-2 parts of polyglycerol fatty acid ester, 30-40 parts of calcium zeolite and 1-3 parts of aluminum dihydrogen phosphate.
The initiator is azobisisobutyronitrile.
The preparation method of the modified water treatment agent comprises the following steps:
(1) adding aluminum dihydrogen phosphate into deionized water with the weight of 10-17 times of that of the aluminum dihydrogen phosphate, raising the temperature to 60-70 ℃, and keeping the temperature and stirring for 30-40 minutes to obtain an aluminum dihydrogen phosphate aqueous solution;
(2) mixing microcrystalline cellulose and isooctyl thioglycolate, adding into chloroform with the weight of 3-5 times of that of the mixture, and stirring uniformly to obtain a fiber dispersion;
(3) adding allyl triphenyl phosphine bromide into the fiber dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen to remove oxygen, adjusting the temperature of the reaction kettle to be 50-60 ℃, adding an initiator, stirring for reaction for 10-20 minutes, cooling to normal temperature, carrying out ultraviolet irradiation for 40-50 minutes, discharging, removing the solvent by rotary evaporation, and drying at normal temperature to obtain phosphorus modified cellulose;
(4) taking the calcium zeolite, sending the calcium zeolite into 1-2mol/l sodium hydroxide aqueous solution, soaking for 1-2 hours, filtering, washing the precipitate with water, adding the precipitate into the aluminum dihydrogen phosphate aqueous solution, sending the solution into a sintering furnace, introducing nitrogen, calcining for 1-2 hours at the temperature of 300-400 ℃, discharging, cooling, and grinding into fine powder to obtain modified zeolite powder;
(5) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(6) mixing the phosphorus modified cellulose with acrylamide, adding the mixture into deionized water which is 5-7 times of the weight of the mixture, uniformly stirring, sending the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate aqueous solution, the polyglycerol fatty acid ester and the modified zeolite powder, keeping the temperature, stirring for 3-5 hours, discharging, sending the discharged material into an oven, drying the material to constant weight at the temperature of 80-86 ℃, discharging and cooling to obtain the modified water treatment agent.
The invention has the advantages that:
the invention firstly takes allyl triphenyl phosphonium bromide as raw material, reacts with sulfydryl under the action of an initiator, carries out quaternary phosphonium modification on microcrystalline cellulose to obtain phosphorus modified cellulose, then carries out alkali treatment on calcium zeolite, then carries out blending calcination with aluminum dihydrogen phosphate to improve the stability of the microporous structure of the phosphorus modified cellulose, finally carries out blending on the phosphorus modified cellulose and acrylamide monomer, carries out polymerization under the action of the initiator, introduces zeolite powder in the polymerization process, realizes the doping of the zeolite powder by polyacrylamide under the action of a dispersing agent, can well disperse the phosphorus modified cellulose introduced in the doping into the microporous structure of the calcium zeolite powder, thereby improving the stability strength of the finished treating agent, and the adsorbability of the calcium zeolite can play a good synergistic effect with the bacteriostatic and purifying performance of the quaternary phosphonium microcrystalline cellulose and the flocculating performance of the polyacrylamide, and especially has a better purifying effect on sewage with suspended particles carrying negative charges, thereby achieving higher clarification effect, and the treating agent has high stability, is not easy to decompose and is convenient to recycle.
Detailed Description
Example 1
A modified water treatment agent is composed of the following raw materials in parts by weight: 100 parts of acrylamide, 3 parts of ammonium persulfate, 1 part of isooctyl thioglycolate, 2.5 parts of allyl triphenyl phosphine bromide, 0.01 part of initiator, 10 parts of microcrystalline cellulose, 1 part of polyglycerol fatty acid ester, 30 parts of calcium zeolite and 1 part of aluminum dihydrogen phosphate.
The initiator is azobisisobutyronitrile.
The preparation method of the modified water treatment agent comprises the following steps:
(1) adding aluminum dihydrogen phosphate into deionized water with the weight 10 times of that of the aluminum dihydrogen phosphate, raising the temperature to 60 ℃, and stirring for 30 minutes under the condition of heat preservation to obtain an aluminum dihydrogen phosphate aqueous solution;
(2) mixing microcrystalline cellulose and isooctyl thioglycolate, adding the mixture into chloroform with the weight being 3 times of that of the mixture, and uniformly stirring to obtain a fiber dispersion liquid;
(3) adding allyl triphenyl phosphine bromide into the fiber dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen to remove oxygen, adjusting the temperature of the reaction kettle to 50 ℃, adding an initiator, stirring for 10 minutes, cooling to normal temperature, carrying out ultraviolet irradiation for 40 minutes, discharging, carrying out rotary evaporation to remove a solvent, and drying at normal temperature to obtain the phosphorus modified cellulose;
(4) taking the calcium zeolite, sending the calcium zeolite into a 1mol/l sodium hydroxide aqueous solution, soaking for 1 hour, filtering, washing the precipitate with water, adding the precipitate into the aluminum dihydrogen phosphate aqueous solution, sending the precipitate into a sintering furnace, introducing nitrogen, calcining for 1 hour at 300 ℃, discharging, cooling, and grinding into fine powder to obtain modified zeolite powder;
(5) adding ammonium persulfate into deionized water with the weight of 20 times of that of the ammonium persulfate, and uniformly stirring;
(6) mixing the phosphorus modified cellulose with acrylamide, adding the mixture into deionized water which is 5 times of the weight of the mixture, uniformly stirring, sending the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the ammonium persulfate aqueous solution, the polyglycerol fatty acid ester and the modified zeolite powder, keeping the temperature, stirring for 3 hours, discharging, sending the discharged material into an oven, drying at 80 ℃ in vacuum until the weight is constant, discharging and cooling to obtain the modified water treatment agent.
Example 2
A modified water treatment agent is composed of the following raw materials in parts by weight:
acrylamide 140, ammonium persulfate 4, isooctyl thioglycolate 2, allyl triphenyl phosphine bromide 3, an initiator 0.02, microcrystalline cellulose 20, polyglycerol fatty acid ester 2, calcium zeolite 40 and aluminum dihydrogen phosphate 3.
The initiator is azobisisobutyronitrile.
The preparation method of the modified water treatment agent comprises the following steps:
(1) adding aluminum dihydrogen phosphate into deionized water 17 times the weight of the aluminum dihydrogen phosphate, raising the temperature to 70 ℃, and stirring for 40 minutes under heat preservation to obtain an aluminum dihydrogen phosphate aqueous solution;
(2) mixing microcrystalline cellulose and isooctyl thioglycolate, adding the mixture into chloroform with the weight 5 times of that of the mixture, and uniformly stirring to obtain a fiber dispersion liquid;
(3) adding allyl triphenyl phosphine bromide into the fiber dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen to remove oxygen, adjusting the temperature of the reaction kettle to 60 ℃, adding an initiator, stirring for 20 minutes, cooling to normal temperature, carrying out ultraviolet irradiation for 50 minutes, discharging, carrying out rotary evaporation to remove a solvent, and drying at normal temperature to obtain the phosphorus modified cellulose;
(4) taking the calcium zeolite, sending the calcium zeolite into a 2mol/l sodium hydroxide aqueous solution, soaking for 2 hours, filtering, washing the precipitate with water, adding the precipitate into the aluminum dihydrogen phosphate aqueous solution, sending the precipitate into a sintering furnace, introducing nitrogen, calcining for 2 hours at 400 ℃, discharging, cooling, and grinding into fine powder to obtain modified zeolite powder;
(5) adding ammonium persulfate into deionized water with the weight 30 times that of the ammonium persulfate, and uniformly stirring;
(6) mixing the phosphorus modified cellulose with acrylamide, adding the mixture into deionized water 7 times of the weight of the mixture, uniformly stirring, sending the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 75 ℃, adding the ammonium persulfate aqueous solution, the polyglycerol fatty acid ester and the modified zeolite powder, keeping the temperature, stirring for 5 hours, discharging, sending the discharged material into an oven, drying at 86 ℃ in vacuum to constant weight, discharging and cooling to obtain the modified water treatment agent.
Example 3
A modified water treatment agent is composed of the following raw materials in parts by weight:
acrylamide 130, ammonium persulfate 3.5, isooctyl thioglycolate 2, allyl triphenyl phosphine bromide 2.8, an initiator 0.01, microcrystalline cellulose 15, polyglycerol fatty acid ester 1.5, calcium zeolite 35 and aluminum dihydrogen phosphate 2.
The initiator is azobisisobutyronitrile.
The preparation method of the modified water treatment agent comprises the following steps:
(1) adding aluminum dihydrogen phosphate into deionized water with the weight 14 times that of the aluminum dihydrogen phosphate, raising the temperature to 60 ℃, and stirring for 35 minutes under the condition of heat preservation to obtain an aluminum dihydrogen phosphate aqueous solution;
(2) mixing microcrystalline cellulose and isooctyl thioglycolate, adding the mixture into chloroform with the weight 4 times that of the mixture, and uniformly stirring to obtain a fiber dispersion liquid;
(3) adding allyl triphenyl phosphine bromide into the fiber dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen to remove oxygen, adjusting the temperature of the reaction kettle to 50 ℃, adding an initiator, stirring for reaction for 15 minutes, cooling to normal temperature, carrying out ultraviolet irradiation for 45 minutes, discharging, carrying out rotary evaporation to remove a solvent, and drying at normal temperature to obtain the phosphorus modified cellulose;
(4) taking the calcium zeolite, sending the calcium zeolite into 1.5mol/l sodium hydroxide aqueous solution, soaking for 1.5 hours, filtering, washing precipitates, adding the precipitates into the aluminum dihydrogen phosphate aqueous solution, sending the aluminum dihydrogen phosphate aqueous solution into a sintering furnace, introducing nitrogen, calcining for 1.5 hours at 300 ℃, discharging, cooling and grinding into fine powder to obtain modified zeolite powder;
(5) adding ammonium persulfate into deionized water with the weight of 20 times of that of the ammonium persulfate, and uniformly stirring;
(6) mixing the phosphorus modified cellulose with acrylamide, adding the mixture into deionized water 6 times the weight of the mixture, uniformly stirring, sending the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the ammonium persulfate aqueous solution, the polyglycerol fatty acid ester and the modified zeolite powder, keeping the temperature, stirring for 4 hours, discharging, sending the discharged material into an oven, drying at 80 ℃ in vacuum until the weight is constant, discharging and cooling to obtain the modified water treatment agent.
And (3) testing the adsorption performance:
respectively adding 0.01g of modified water treatment agent of embodiment 1 of the invention, 0.01g of modified water treatment agent of embodiment 2 of the invention, 0.01g of modified water treatment agent of embodiment 3 of the invention, 0.01g of calcium zeolite powder and 0.01g of activated carbon powder into 500ml of methylene blue solution with the mass concentration of 20 mg/l; oscillating at room temperature until the solution is balanced, measuring the absorbance at 665nm wavelength by using a spectrophotometer, and calculating the saturated adsorption quantity according to the absorbance;
as a result:
the saturated adsorption capacity of the modified water treatment agent in embodiment 1 of the present invention is: 233 mg/g;
the saturated adsorption capacity of the modified water treatment agent in embodiment 2 of the present invention is: 209 mg/g;
the saturated adsorption capacity of the modified water treatment agent in embodiment 3 of the present invention is: 216 mg/g;
the saturated adsorption capacity of the scolecite powder is as follows: 77 mg/g;
the saturated adsorption capacity of the activated carbon powder is as follows: 140 mg/g;
and (3) testing the antibacterial performance:
the water-purified diatom ooze has the bacteriostasis rate of 93.3-97% on escherichia coli and the bacteriostasis rate of 96.4-100% on staphylococcus aureus.
Claims (3)
1. The modified water treatment agent is characterized by comprising the following raw materials in parts by weight:
100-140 parts of acrylamide, 3-4 parts of ammonium persulfate, 1-2 parts of isooctyl thioglycolate, 2.5-3 parts of allyl triphenyl phosphonium bromide, 0.01-0.02 part of initiator, 10-20 parts of microcrystalline cellulose, 1-2 parts of polyglycerol fatty acid ester, 30-40 parts of calcium zeolite and 1-3 parts of aluminum dihydrogen phosphate.
2. The modified water treatment agent according to claim 1, wherein the initiator is azobisisobutyronitrile.
3. A method for preparing the modified water treatment agent according to claim 1, comprising the steps of:
(1) adding aluminum dihydrogen phosphate into deionized water with the weight of 10-17 times of that of the aluminum dihydrogen phosphate, raising the temperature to 60-70 ℃, and keeping the temperature and stirring for 30-40 minutes to obtain an aluminum dihydrogen phosphate aqueous solution;
(2) mixing microcrystalline cellulose and isooctyl thioglycolate, adding into chloroform with the weight of 3-5 times of that of the mixture, and stirring uniformly to obtain a fiber dispersion;
(3) adding allyl triphenyl phosphine bromide into the fiber dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen to remove oxygen, adjusting the temperature of the reaction kettle to be 50-60 ℃, adding an initiator, stirring for reaction for 10-20 minutes, cooling to normal temperature, carrying out ultraviolet irradiation for 40-50 minutes, discharging, removing the solvent by rotary evaporation, and drying at normal temperature to obtain phosphorus modified cellulose;
(4) taking the calcium zeolite, sending the calcium zeolite into 1-2mol/l sodium hydroxide aqueous solution, soaking for 1-2 hours, filtering, washing the precipitate with water, adding the precipitate into the aluminum dihydrogen phosphate aqueous solution, sending the solution into a sintering furnace, introducing nitrogen, calcining for 1-2 hours at the temperature of 300-400 ℃, discharging, cooling, and grinding into fine powder to obtain modified zeolite powder;
(5) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(6) mixing the phosphorus modified cellulose with acrylamide, adding the mixture into deionized water which is 5-7 times of the weight of the mixture, uniformly stirring, sending the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate aqueous solution, the polyglycerol fatty acid ester and the modified zeolite powder, keeping the temperature, stirring for 3-5 hours, discharging, sending the discharged material into an oven, drying the material to constant weight at the temperature of 80-86 ℃, discharging and cooling to obtain the modified water treatment agent.
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| CN201911371942.XA CN111003774A (en) | 2019-12-26 | 2019-12-26 | Modified water treatment agent and preparation method thereof |
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| CN201911371942.XA CN111003774A (en) | 2019-12-26 | 2019-12-26 | Modified water treatment agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461128A (en) * | 2021-06-24 | 2021-10-01 | 南京师范大学 | Preparation method of starch grafted quaternary phosphonium salt flocculant for treating bacteria-containing sewage |
| CN114905806A (en) * | 2022-05-24 | 2022-08-16 | 瑞安市大虎鞋业有限公司 | Deodorizing insole based on antibacterial fibers and preparation method thereof |
-
2019
- 2019-12-26 CN CN201911371942.XA patent/CN111003774A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461128A (en) * | 2021-06-24 | 2021-10-01 | 南京师范大学 | Preparation method of starch grafted quaternary phosphonium salt flocculant for treating bacteria-containing sewage |
| CN114905806A (en) * | 2022-05-24 | 2022-08-16 | 瑞安市大虎鞋业有限公司 | Deodorizing insole based on antibacterial fibers and preparation method thereof |
| CN114905806B (en) * | 2022-05-24 | 2024-03-26 | 瑞安市大虎鞋业有限公司 | Deodorant insole based on antibacterial fibers and preparation method thereof |
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