CN114684877A - Preparation method of alum water purifying agent - Google Patents

Preparation method of alum water purifying agent Download PDF

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Publication number
CN114684877A
CN114684877A CN202210359788.XA CN202210359788A CN114684877A CN 114684877 A CN114684877 A CN 114684877A CN 202210359788 A CN202210359788 A CN 202210359788A CN 114684877 A CN114684877 A CN 114684877A
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alum
parts
water purifying
purifying agent
water
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Inventor
何朝晖
何青峰
王开宝
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Hengyang Jianheng Industry Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/50Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds

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  • Chemical & Material Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a preparation method of an alum water purifying agent, which relates to the technical field of water purifying agents and comprises the following steps of stirring and mixing 100 parts by mass of alum, 15-25 parts by mass of a nano additive, 2-10 parts by mass of chitosan, 1-4 parts by mass of an antibacterial agent and 30-50 parts by mass of a complexing agent to obtain the alum water purifying agent, wherein aluminum ions in the alum are easy to hydrolyze to generate colloidal aluminum hydroxide with strong adsorption capacity to adsorb suspended matters in water and have a good sterilization effect, the nano additive has a large specific surface area and a pore structure and can further adsorb impurities in water, the added chitosan contains a plurality of active sites and can rapidly adsorb the impurity ions in the water and act together with the antibacterial agent, the sterilization effect of the alum water purifying agent is further improved, the water is purified, the added complexing agent can further accelerate the aggregation and impurity settling, the alum water purifying agent is green and environment-friendly, and has the characteristics of quick adsorption, good effect and strong antibacterial property.

Description

Preparation method of alum water purifying agent
Technical Field
The invention relates to the technical field of water purifying agents, and particularly relates to a preparation method of an alum water purifying agent.
Background
Alum, also called alum, potassium alumen, is a double salt of potassium sulfate and aluminum sulfate containing crystal water, and has the chemical formula of KAl (SO)4)2·12H2The O is directly extracted from alunite, is abundant in reserves in China, is soluble in water, can be hydrolyzed into colloidal aluminum hydroxide with strong adsorption capacity when the alunite is dissolved in the water, adsorbs impurities suspended in water, forms a precipitate to achieve the effect of purifying water, and is a water purifying agent with low price, convenient use and excellent effect.
The water purifying agent is the most commonly used water quality modifying agent in the aquaculture industry, and mainly aggregates and enlarges fragments of feed in a water body, microorganisms, silt and the like in the water body to form floccules through adding the water purifying agent, so that the floccules are precipitated, a large amount of bacteria can be bred due to pollution of the water body, the aim of purifying the water body can be better achieved by adding antibacterial ingredients in the water purifying agent, and further wastewater can be recycled, and the phenomenon of water resource deterioration is reduced.
The invention patent CN108889281A discloses a preparation method of aquaculture water purifying agent, which is prepared by crushing walnut shells, coconut shells, corn straws and the like into water purifying agent with strong adsorption effect, but the adsorption effect is general and the water body is not subjected to antibacterial purification treatment.
Disclosure of Invention
The invention aims to provide a preparation method of an alum water purifying agent, which solves the following technical problems:
the existing water purifying agent is mainly only a precipitable substance in purified water, and has poor antibacterial purification effect on water.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of an alum water purifying agent comprises the following steps: weighing the following raw materials in parts by weight: 100 parts of alum, 15-25 parts of nano additive, 2-10 parts of chitosan, 1-4 parts of antibacterial agent and 30-50 parts of complexing agent; and respectively adding the alum, the nano additive, the chitosan, the antibacterial agent and the complexing agent into a high-speed stirrer, stirring and mixing uniformly to obtain the alum water purifying agent.
As a further scheme of the invention: the nano additive comprises one or more of nano iron oxide, nano carbon nano tubes, nano graphene oxide and nano montmorillonite.
As a further scheme of the invention: the antibacterial agent comprises one or more of antibacterial peptide, baicalin, copper chloride and copper nitrate.
As a further scheme of the invention: the complexing agent comprises one or more of disodium ethylene tetraacetate, trisodium citrate, tripotassium citrate and triammonium citrate.
As a further scheme of the invention: the rotating speed of the stirring is 1200-1600r/min, and the stirring time is 60-120 min.
As a further scheme of the invention: the preparation method of the alum comprises the following steps: crushing the aluminum material into powder for later use, adding a potassium hydroxide solution, heating to 85-95 ℃ in a water bath, continuously stirring in the heating process until no bubbles are generated, performing suction filtration, and collecting filtrate; adding a sulfuric acid solution into the filtrate to generate a precipitate, and performing suction filtration to obtain the precipitate when the precipitate is not generated any more; adding sulfuric acid solution into the precipitate until the precipitate is completely dissolved, adding potassium sulfate, stirring and mixing, cooling, performing suction filtration, and washing with ethanol to obtain alum.
As a further scheme of the invention: and in the process of generating the precipitate, the pH value of the solution is adjusted to be 8-9, and the reaction temperature is controlled to be 60-75 ℃.
As a further scheme of the invention: the concentration of the potassium hydroxide solution is 2 mol/L; the concentration of the sulfuric acid solution is 3-9 mol/L.
As a further scheme of the invention: 100 parts of aluminum material, 350-650 parts of potassium hydroxide solution and 80-150 parts of potassium sulfate.
The invention has the beneficial effects that:
1. the aluminum material is used as an aluminum source, the aluminum material is dissolved under the action of strong alkali potassium hydroxide, the sulfuric acid solution is added to provide hydrogen ions to generate aluminum hydroxide precipitate, the sulfuric acid solution is continuously added to dissolve the precipitate to generate aluminum ions, alum is generated under the action of potassium sulfate, the method has the advantages of simple operation, good crystal form of the obtained alum, high yield, quick dissolution of the alum in water after being added into water, potassium ions and aluminum ions are ionized in water, the aluminum ions are easy to hydrolyze to generate colloidal aluminum hydroxide with strong adsorption capacity, suspended matters in water are effectively adsorbed, the characteristics of fast adsorption and good effect are achieved, precipitates are quickly formed to achieve the effect of purifying water, meanwhile, the alum has a good sterilization effect, can effectively kill bacteria in water, and has a good water quality purification effect.
2. The nano additive and the chitosan added in the invention both have large specific surface area and pore structure, can firstly adsorb impurities in water, simultaneously expose more active sites and contain hydroxyl, amino, carboxyl and other groups which can quickly adsorb impurity ions in the water, reduce the impurity concentration in the water, at the moment, colloidal aluminum hydroxide generated by aluminum ions ionized by alum can adsorb the residual impurities in the water, the added complexing agent can further accelerate the action of gathering and settling the impurities, remove organic pollutants in the water, quickly remove the impurities in the water through synergistic effect, achieve the aim of water purification, and after the alum water purifying agent adsorbs and treats the impurities in the water, the obtained adsorbate can be well removed, is green and environment-friendly, does not produce secondary pollution to the water, and simultaneously the added chitosan has certain bactericidal effect, the alum water purifying agent has the characteristics of strong antibacterial property.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below with reference to embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum material into powder, adding the powder into 350 parts of 2mol/L potassium hydroxide solution, heating the solution to 85 ℃ in a water bath, continuously stirring the solution in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 3mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to 8, controlling the reaction temperature to be 60 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and no precipitate is generated; and adding a 3mol/L sulfuric acid solution into the precipitate, stirring, adding 80 parts of potassium sulfate when the precipitate is completely dissolved in the process of adding the sulfuric acid solution, stirring and mixing, cooling, performing suction filtration, and washing by using ethanol to obtain the alum.
(2) Adding 100 parts of alum, 15 parts of nano carbon nano tube, 2 parts of chitosan, 1 part of antibacterial peptide and 30 parts of disodium edetate into a high-speed stirrer, stirring and mixing at the rotating speed of 1200r/min for 60min, and uniformly mixing to obtain the alum water purifying agent.
Example 2:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum material into powder, adding the powder into 420 parts of 2mol/L potassium hydroxide solution, heating the mixture to 90 ℃ in a water bath, continuously stirring the mixture in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 3mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to 8, controlling the reaction temperature to 65 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and no precipitate is generated; and adding a 4mol/L sulfuric acid solution into the precipitate, stirring, adding 100 parts of potassium sulfate when the precipitate is completely dissolved in the process of adding the sulfuric acid solution, stirring and mixing, cooling, performing suction filtration, and washing with ethanol to obtain the alum.
(2) Adding 100 parts of alum, 10 parts of nano iron oxide, 8 parts of nano carbon nano tube, 4 parts of chitosan, 2 parts of baicalin and 35 parts of trisodium citrate into a high-speed stirrer, stirring and mixing at the rotating speed of 1300r/min for 80min, and uniformly mixing to obtain the alum water purifying agent.
Example 3:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum material into powder, adding the powder into 500 parts of 2mol/L potassium hydroxide solution, heating the mixture to 90 ℃ in a water bath, continuously stirring the mixture in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 6mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to 8.5, controlling the reaction temperature to 65 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and no precipitate is generated; and adding a 6mol/L sulfuric acid solution into the precipitate, stirring, adding 120 parts of potassium sulfate when the precipitate is completely dissolved in the process of adding the sulfuric acid solution, stirring and mixing, cooling after uniform mixing, performing suction filtration, and washing with ethanol to obtain the alum.
(2) Adding 100 parts of alum, 20 parts of nano graphene oxide, 6 parts of chitosan, 2 parts of copper chloride and 40 parts of tripotassium citrate into a high-speed stirrer, stirring and mixing at the rotating speed of 1400r/min for 90min, and uniformly mixing to obtain the alum water purifying agent.
Example 4:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum into powder, adding the powder into 600 parts of 2mol/L potassium hydroxide solution, heating the solution to 90 ℃ in a water bath, continuously stirring the solution in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 8mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to be 9, controlling the reaction temperature to be 70 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and the precipitate is not generated any more; adding 8mol/L sulfuric acid solution into the precipitate, stirring, adding 140 parts of potassium sulfate when the precipitate is completely dissolved in the sulfuric acid solution, stirring and mixing, uniformly mixing, cooling, performing suction filtration, and washing with ethanol to obtain alum.
(2) Adding 100 parts of alum, 22 parts of nano-montmorillonite, 8 parts of chitosan, 3 parts of copper chloride and 45 parts of tripotassium citrate into a high-speed stirrer, stirring and mixing at the rotating speed of 1500r/min for 100min, and uniformly mixing to obtain the alum water purifying agent.
Example 5:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum material into powder, adding the powder into 650 parts of 2mol/L potassium hydroxide solution, heating the solution in a water bath to 95 ℃, continuously stirring the solution in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 9mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to 9, controlling the reaction temperature to be 75 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and no precipitate is generated; adding 9mol/L sulfuric acid solution into the precipitate, stirring, adding 150 parts of potassium sulfate when the precipitate is completely dissolved in the sulfuric acid solution, stirring and mixing, cooling, performing suction filtration, and washing with ethanol to obtain alum.
(2) Adding 100 parts of alum, 25 parts of nano carbon nanotube, 10 parts of chitosan, 4 parts of antibacterial peptide and 50 parts of disodium edetate into a high-speed stirrer, stirring and mixing at 1600r/min for 120min, and uniformly mixing to obtain the alum water purifying agent.
Comparative example 1:
a preparation method of an alum water purifying agent comprises the following steps:
(1) crushing 100 parts of aluminum material into powder, adding the powder into 600 parts of 2mol/L potassium hydroxide solution, heating the solution to 90 ℃ in a water bath, continuously stirring the solution in the heating process until no bubbles are generated, stopping stirring, carrying out suction filtration on the mixed solution, and collecting filtrate; adding 8mol/L sulfuric acid solution into the filtrate, generating precipitate in the adding process, adjusting the pH of the solution to 9, controlling the reaction temperature to be 70 ℃, and performing suction filtration to obtain precipitate when the sulfuric acid solution is added and no precipitate is generated; and adding 8mol/L sulfuric acid solution into the precipitate, stirring, adding 140 parts of potassium sulfate when the precipitate is completely dissolved in the process of adding the sulfuric acid solution, stirring and mixing, cooling after uniform mixing, performing suction filtration, and washing with ethanol to obtain the alum water purifying agent.
Comparative example 2:
a preparation method of an alum water purifying agent comprises the following steps:
(1) adding 100 parts of alum, 22 parts of nano-montmorillonite, 8 parts of chitosan, 3 parts of copper chloride and 45 parts of tripotassium citrate into a high-speed stirrer, stirring and mixing at the rotating speed of 1500r/min for 100min, and uniformly mixing to obtain the alum water purifying agent.
Experimental detection
1. And (3) pH test:
and (3) measuring the test water sample according to a GB/T9620 glass electrode method.
2. And (3) COD test:
the test water samples were tested according to the GB/T11914 potassium dichromate method.
3. And (3) testing suspended matters:
and (3) determining the test water sample according to a GB/T11901 weight method.
4. Testing ammonia nitrogen:
and (3) determining the test water sample according to a GB/T7481 salicylic acid spectrophotometric method.
5. Nitrite nitrogen test:
and (3) determining the test water sample according to a GB/T7493 molecular absorption spectrophotometer.
Water sample treatment:
(1) before adding the alum water purifying agent, detecting various indexes of a water sample, recording the indexes before treatment, taking a water body sample as a pond for culturing fishes and shrimps, and selecting the water sample at a position 0.5m away from the bank;
(2) respectively taking 500mL of the water samples, respectively adding 0.2g, 0.5g and 1.0g of the alum water purifying agents prepared in the examples and the comparative examples into each water sample, keeping the stirring state, and directly performing suction filtration treatment by using a Buchner funnel after 30min to obtain a treated clear water sample;
(3) and (3) determining each index of the clarified water sample obtained in the step (2) again, wherein the detection result is shown in a table 1.
Table 1: results of testing Water quality after treatment in examples 1 to 5 and comparative examples 1 to 2
Figure BDA0003583369150000071
Figure BDA0003583369150000081
Figure BDA0003583369150000091
As can be seen from the detection results in Table 1, the alum water purifying agent prepared by the invention is used for purifying aquaculture water samples, can quickly enable the polluted water samples to be clarified, stabilize the pH value of the water body, remove organic pollutants in the water body, and can also perform sterilization treatment on the water body, and has the characteristics of high settling speed of suspended matters and environmental protection.
Five embodiments of the present invention have been described in detail, but the description is only for the preferred embodiment of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (9)

1. The preparation method of the alum water purifying agent is characterized by comprising the following steps: weighing the following raw materials in parts by weight: 100 parts of alum, 15-25 parts of nano additive, 2-10 parts of chitosan, 1-4 parts of antibacterial agent and 30-50 parts of complexing agent; and respectively adding the alum, the nano additive, the chitosan, the antibacterial agent and the complexing agent into a high-speed stirrer, stirring and mixing uniformly to obtain the alum water purifying agent.
2. The method for preparing an alum water purifying agent according to claim 1, wherein the nano additive comprises one or more of nano iron oxide, nano carbon nanotube, nano graphene oxide and nano montmorillonite.
3. The method for preparing an alum water purifying agent according to claim 1, wherein the antibacterial agent comprises one or more of antibacterial peptide, baicalin, copper chloride and copper nitrate.
4. The method for preparing the alum water purifying agent according to claim 1, wherein the complexing agent comprises one or more of disodium edetate, trisodium citrate, tripotassium citrate and triammonium citrate.
5. The method for preparing an alum water purifying agent as claimed in claim 1, wherein the stirring speed is 1200-1600r/min, and the stirring time is 60-120 min.
6. The method for preparing alum water purifying agent according to claim 1, wherein the method for preparing alum comprises the following steps: crushing aluminum into powder for later use, adding a potassium hydroxide solution, heating to 85-95 ℃ in a water bath, continuously stirring in the heating process until no bubbles are generated, performing suction filtration, and collecting filtrate; adding a sulfuric acid solution into the filtrate to generate a precipitate, and performing suction filtration to obtain the precipitate when the precipitate is not generated any more; adding sulfuric acid solution into the precipitate until the precipitate is completely dissolved, adding potassium sulfate, stirring and mixing, cooling, performing suction filtration, and washing with ethanol to obtain alum.
7. The method for preparing an alum water purifying agent according to claim 6, wherein the pH of the solution is adjusted to 8-9 during the precipitation process, and the reaction temperature is controlled to 60-75 ℃.
8. The method of claim 6, wherein the concentration of the potassium hydroxide solution is 2 mol/L; the concentration of the sulfuric acid solution is 3-9 mol/L.
9. The method for preparing an alum water purifying agent as claimed in claim 6, wherein the aluminum material is 100 parts, the potassium hydroxide solution is 350-650 parts, and the potassium sulfate is 80-150 parts.
CN202210359788.XA 2022-04-06 2022-04-06 Preparation method of alum water purifying agent Pending CN114684877A (en)

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Citations (3)

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CN108341457A (en) * 2018-03-02 2018-07-31 合肥浦邦农业科技有限公司 A kind of freshwater aquiculture fishpond disinfection oxygenation agent
CN108383196A (en) * 2018-04-02 2018-08-10 合肥卓畅农业科技有限公司 Antibacterial decontamination environment-friendly high-efficiency water purification agent of one kind and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN108341457A (en) * 2018-03-02 2018-07-31 合肥浦邦农业科技有限公司 A kind of freshwater aquiculture fishpond disinfection oxygenation agent
CN108217782A (en) * 2018-03-21 2018-06-29 合肥浦邦农业科技有限公司 It is a kind of for environment-friendly type water purification agent of aquaculture and preparation method thereof
CN108383196A (en) * 2018-04-02 2018-08-10 合肥卓畅农业科技有限公司 Antibacterial decontamination environment-friendly high-efficiency water purification agent of one kind and preparation method thereof

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