CN116712857B - Air purifying agent and preparation method thereof - Google Patents

Air purifying agent and preparation method thereof Download PDF

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CN116712857B
CN116712857B CN202310725653.5A CN202310725653A CN116712857B CN 116712857 B CN116712857 B CN 116712857B CN 202310725653 A CN202310725653 A CN 202310725653A CN 116712857 B CN116712857 B CN 116712857B
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suspension
titanium oxide
preparation
water
temperature
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CN116712857A (en
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华卫东
路伏增
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Zhejiang Academy of Agricultural Sciences
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Zhejiang Academy of Agricultural Sciences
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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Abstract

The invention provides an air purifying agent and a preparation method thereof, wherein the preparation method comprises the following steps: s100, preparing a first suspension by adopting raw materials including palladium chloride, terbium chloride, manganese chloride, titanium oxide, sodium alginate, sodium bicarbonate, polyvinyl alcohol and water; s200, preparing a second suspension by adopting raw materials including tween, active carbon and vegetable oil; s300, dropwise adding the first suspension of the S100 into the second suspension of the S200, and performing ultrasonic emulsification to obtain a mixed solution; and S400, delivering the mixed solution of the step S300 into a reaction kettle, heating and pressurizing, separating solid matters, and drying to obtain the air purifying agent. The preparation method disclosed by the invention can promote the titanium oxide catalyst to be uniformly dispersed in the porous active carbon, so that the air purifying agent with excellent purifying effect is obtained, and the preparation method is especially suitable for air purifying treatment in environments such as animal farms.

Description

Air purifying agent and preparation method thereof
Technical Field
The invention relates to the technical field of separation and purification of harmful substances in waste gas by utilizing a catalytic method, in particular to an air purifying agent and a preparation method thereof.
Background
The air purifying agent adsorbs and decomposes harmful substances in the air by physical, chemical and other modes, and can effectively control the air pollution condition in certain closed spaces (such as indoor, in-vehicle, in-factory buildings and the like). For example, in the environment of animal farms, where livestock emit gases mainly including amines (especially ammonia), sulfides, aromatics, fatty acids, and the like. The air pollutants can reduce the feed intake and the disease resistance of livestock and can also cause harm to the health of breeding personnel. The modes of deodorizing and purifying air in farms include: physical methods such as activated carbon, water curtain, deodorization tower, etc. further include: fungi, bacillus, and the like, and chemical means utilizing redox reactions.
In the prior art, porous materials are adopted for adsorption purification, and the method is an effective purification mode. In order to further improve the purification effect, the prior art generally adopts substances such as titanium dioxide, potassium permanganate and the like to promote the decomposition of harmful substances in the waste gas.
For example, chinese patent publication No. CN106268299B discloses a method for preparing an air purifying material by catalytic oxidation of a microporous medium, which comprises mixing an oxidant solution with a microporous medium matrix to obtain a mixed solution, placing the mixed solution in an autoclave, filtering and autoclaved loading, and finally drying and developing the autoclaved loaded microporous medium matrix.
For another example, chinese patent publication No. CN112973437B discloses a formaldehyde removal master batch for an air purification device, which includes a noble metal supported titanium dioxide nano array tube catalyst, opal shale, a silane coupling agent, an accelerator, a dispersant, and absolute ethanol.
As is clear from the analysis of the prior art, the porous material has a relatively limited effect of purifying exhaust gas by adsorption, and is preferably used together with a highly oxidizing agent or a highly photocatalytic catalyst capable of promoting decomposition of harmful substances in exhaust gas, such as titanium dioxide and potassium permanganate.
However, the above-mentioned oxidizing agent or catalyst is not easily uniformly dispersed and supported in the porous material, resulting in an improvement in air purification efficiency thereof, which is a pain spot to be solved by those skilled in the art.
Disclosure of Invention
The problem addressed by the present invention is how to allow titanium oxide catalysts to be uniformly dispersed and supported in porous activated carbon materials.
In order to solve the above problems, the present invention provides a method for preparing an air purifying agent, comprising:
s100, preparing a first suspension by adopting raw materials including palladium chloride, terbium chloride, manganese chloride, titanium oxide, sodium alginate, sodium bicarbonate, polyvinyl alcohol and water;
s200, preparing a second suspension by adopting raw materials including tween, active carbon and vegetable oil;
s300, dropwise adding the first suspension of the S100 into the second suspension of the S200, and performing ultrasonic emulsification to obtain a mixed solution;
and S400, delivering the mixed solution of the step S300 into a reaction kettle, heating and pressurizing, separating solid matters, and drying to obtain the air purifying agent.
In any of the above technical solutions, S100 specifically includes:
s110, uniformly mixing palladium chloride, terbium chloride and manganese chloride in water to obtain a metal salt solution;
s120, uniformly mixing sodium hexametaphosphate and titanium oxide in water to obtain titanium oxide suspension;
s130, dropwise adding the metal salt solution of S110 into the titanium oxide suspension of S120, stirring, adjusting the pH value to 11-12 after dropwise adding, stirring, aging, filtering, washing, drying and calcining to obtain modified titanium oxide;
and S140, uniformly mixing the sodium alginate, the sodium bicarbonate and the modified titanium oxide and the polyvinyl alcohol obtained in the step 130 in water to obtain a first suspension.
In any of the above embodiments, in S110, palladium chloride: terbium chloride: manganese chloride: water= (0.02-0.04): (0.1-0.2): (2-4): 20, a step of; and/or in S120, sodium hexametaphosphate: titanium oxide: water= (0.2-0.4): (10-20): 100; and/or in S130, a metal salt solution: titanium oxide suspension= (6-8): 100; and/or in S140, sodium alginate: sodium bicarbonate: modified titanium oxide: polyvinyl alcohol: water= (2-4): (6-8): (10-20): (20-30): 100.
in any of the above technical solutions, in S130, the stirring time is 20min to 40min; and/or in S130, the aging time is 4 to 6 hours; and/or in S130, washing with ethanol or acetone for 2 to 3 times; and/or in S130, the temperature of drying is 80-120 ℃ and the time of drying is 2-4 h; and/or in S130, the temperature of calcination is 450 ℃ to 650 ℃ and the time of calcination is 1h to 3h.
In any of the above technical solutions, S200 specifically includes:
s210, according to Tween: activated carbon: vegetable oil= (6-8): (15-25): 100 mass ratio, adding tween and active carbon into vegetable oil, heating and stirring to obtain a second suspension.
In any of the above embodiments, in S210, the temperature condition of the temperature increase is 50 ℃ to 60 ℃; and/or in S210, stirring for a period of 20min to 40min; and/or in S210, tween comprises tween 60 and/or tween 80.
In any of the above technical solutions, S300 specifically includes:
s310, according to the first suspension liquid drops: second suspension= (5-15): 100 mass ratio, dripping the first suspension of S100 into the second suspension of S200, and performing ultrasonic emulsification at the temperature of 40-60 ℃ to obtain a mixed solution.
In any of the above technical solutions, S400 specifically includes:
s410, sending the mixed solution of the step S300 into a reaction kettle, controlling the reaction kettle to be heated to a temperature of 50-55 ℃ under a closed condition, and preserving heat for 40-60 min;
s420, preserving heat and controlling the pressure of the reaction kettle to be 7.5MPa to 8.5MPa, and preserving heat and pressure for 2h to 4h;
s430, decompressing and cooling, separating solid matters from the reaction kettle, and drying to obtain the air purifying agent.
In any of the above technical solutions, the preparation method further includes:
s510, according to polydopamine: trimethylmethanol= (80-90): 100 mass ratio, uniformly mixing polydopamine and trimethyl methanol to obtain a first material;
s520, vinyl trimethoxy silane: chitosan: water= (1-2): (2-4): 100 mass ratio, uniformly mixing vinyl trimethoxy silane and chitosan in water to obtain a second material;
s530, according to the first material: second material = 1:1, dropwise adding a first material into a second material, and mixing for 2-3 hours to obtain a spray;
s540, spraying: air cleaner= (5-15): 100 mass ratio, spraying the spray material on the surface of the air purifying agent, freeze-drying, heating at the temperature of 85-90 ℃ for 1-2 h, and cooling.
In any of the above embodiments, the air purifier obtained in S400 can be used in combination with a deodorizing component of a natural plant functional extract.
The natural plant functional extract comprises caryophyllene, humulone, cedrol, n-hexadecanoic acid, phytol, linoleic acid, 7-tetradecenal, pregnane-3, 17, 20-triol, 1-phenanthrenealdehyde, cis-tulobuterol, iron yellow, 1-naphthoic acid, (-) -Globulol, and Argadine diol. The natural plant functional extract is combined with peptidoglycan to precipitate peptidoglycan, thereby preventing bacterial cell wall formation and achieving antibacterial effect. Meanwhile, the catalyst can react with active oxide to generate hydrogen peroxide so as to play a role in bacteriostasis. In addition, the natural plant functional extract can realize the strong activity of separating unpaired electrons, can play an antioxidant role by scavenging free radicals, chelating metal ions and inhibiting oxidase activity, and can play an indirect antioxidant role by protecting endogenous antioxidant enzymes of organisms. Its molecules quench free radicals through hydrogen atom transfer and single electron transfer mechanisms.
The invention also provides an air purifying agent which is obtained by adopting the preparation method according to any one of the technical schemes.
Advantageous effects
The invention provides a preparation method of an air purifying agent, which comprises the steps of firstly preparing a first suspension by adopting raw materials including palladium chloride, terbium chloride, manganese chloride, titanium oxide, sodium alginate, sodium bicarbonate, polyvinyl alcohol and water. The invention further adopts the raw materials comprising tween, active carbon and vegetable oil to prepare the second suspension. Finally, the first suspension is added into the second suspension in a dropwise manner to obtain a mixed solution, the mixed solution is sent into a reaction kettle, and the mixed solution is heated and pressurized, separated into solid matters and dried to obtain the air purifying agent. Through the technical scheme, the invention utilizes the photocatalysis effect of titanium oxide and the adsorption effect of activated carbon to purify air. In addition, the invention can promote the uniform dispersion of the titanium oxide catalyst in the porous active carbon by preparing the titanium oxide catalyst and the active carbon into emulsion and heating and pressurizing the emulsion, thereby improving the air purifying effect.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
The embodiment of the invention provides a preparation method of an air purifying agent, which comprises the following steps:
s100, preparing a first suspension by adopting raw materials including palladium chloride, terbium chloride, manganese chloride, titanium oxide, sodium alginate, sodium bicarbonate, polyvinyl alcohol and water;
s200, preparing a second suspension by adopting raw materials including tween, active carbon and vegetable oil;
s300, dropwise adding the first suspension of the S100 into the second suspension of the S200, and performing ultrasonic emulsification to obtain a mixed solution;
and S400, delivering the mixed solution of the step S300 into a reaction kettle, heating and pressurizing, separating solid matters, and drying to obtain the air purifying agent.
Titanium oxide acts as a photoactive catalyst that is capable of decomposing organic contaminants in air upon photon excitation. The metal ions palladium and terbium have sensitization effect on titanium oxide, and especially terbium can promote titanium oxide with narrow forbidden band width to absorb and utilize photons of more wavebands. Therefore, the titanium oxide can generate corresponding holes on the valence band by exciting electrons on the valence band to transfer to the conduction band under the action of ultraviolet light or sunlight, the photo-generated holes promote the generation of hydroxyl free radicals, the photo-generated electrons promote the generation of superoxide anions, and the hydroxyl free radicals and the superoxide anions have stronger oxidation-reduction potentials, so that organic pollutants such as formaldehyde are oxidized and decomposed into carbon dioxide and water, and the aim of decomposing the organic pollutants is fulfilled. Based on the principle, the air purifying agent prepared by the method can purify air by utilizing the photocatalysis effect of titanium oxide and the adsorption effect of activated carbon. In addition, the titanium oxide catalyst and the activated carbon are prepared into an emulsion mixture and are subjected to heating and pressurizing treatment, so that the titanium oxide catalyst can be uniformly dispersed in the porous activated carbon, and the air purifying effect is improved.
In some embodiments of the present invention, S100 specifically includes:
s110, palladium chloride: terbium chloride: manganese chloride: water= (0.02-0.04): (0.1-0.2): (2-4): 20, uniformly mixing palladium chloride, terbium chloride and manganese chloride in water to obtain a metal salt solution;
s120, according to sodium hexametaphosphate: titanium oxide: water= (0.2-0.4): (10-20): 100 mass ratio, uniformly mixing sodium hexametaphosphate and titanium oxide in water to obtain titanium oxide suspension;
s130, according to a metal salt solution: titanium oxide suspension= (6-8): 100 mass ratio, dropwise adding the metal salt solution of S110 into the titanium oxide suspension of S120, stirring, adjusting the pH value to 11-12 after dropwise adding, stirring for 20-40 min, aging for 4-6 h, filtering, washing with ethanol or acetone for 2-3 times, drying at 80-120 ℃ for 2-4 h, and calcining at 450-650 ℃ for 1-3 h to obtain modified titanium oxide;
s140, according to sodium alginate: sodium bicarbonate: modified titanium oxide: polyvinyl alcohol: water= (2-4): (6-8): (10-20): (20-30): 100 mass ratio, uniformly mixing sodium alginate, sodium bicarbonate, modified titanium oxide obtained in S130 and polyvinyl alcohol in water to obtain a first suspension.
Preferably, in S110, palladium chloride: terbium chloride: manganese chloride: water = 0.02:0.2:4:20.
preferably, in S120, sodium hexametaphosphate: titanium oxide: water = 0.2:15:100.
preferably, in S130, the metal salt solution: titanium oxide suspension = 6:100.
preferably, in S140, sodium alginate: sodium bicarbonate: modified titanium oxide: polyvinyl alcohol: water = 4:6:20:25:100.
preferably, in S130, the pH is adjusted by a 6wt% aqueous sodium hydroxide solution.
It is understood that the metal salt solution obtained in S110 is a mixed chloride salt of metal palladium, terbium and manganese. Sodium hexametaphosphate is used as a dispersing agent to promote the titanium oxide to be dispersed into suspension in water. The mixed chloride salt of palladium, terbium and manganese metal can be mixed with the titanium oxide suspension by dropping the metal salt solution of S110 into the titanium oxide suspension of S120 and stirring. At a pH of 11-12, the metal ions bind to hydroxyl groups to form hydroxide precipitates on the surface of the titanium oxide particles. By calcination, the unstable hydroxide is converted into an oxide, thereby obtaining a modified titanium oxide. Palladium oxide and terbium oxide can improve the photocatalytic performance of the modified titanium oxide. Manganese oxide imparts excellent oxidation properties to the air cleaner.
In some embodiments of the present invention, S200 specifically includes:
s210, according to Tween: activated carbon: vegetable oil= (6-8): (15-25): 100 mass ratio, adding tween and active carbon into vegetable oil, heating to 50-60 ℃ and stirring for 20-40 min to obtain a second suspension.
Preferably, in S210, tween comprises tween 60 and/or tween 80.
Preferably, in S210, tween: activated carbon: vegetable oil = 6:25:100.
it is understood that the second suspension is an oily suspension of activated carbon. Tween was used as an emulsifier. The operation of warming and stirring promotes a relatively uniform dispersion of the activated carbon in the vegetable oil.
In some embodiments of the present invention, S300 specifically includes:
s310, according to the first suspension liquid drops: second suspension= (5-15): 100 mass ratio, dripping the first suspension of S100 into the second suspension of S200, and performing ultrasonic emulsification at the temperature of 40-60 ℃ to obtain a mixed solution.
Preferably, in S310, the first suspension droplet: second suspension = 10:100.
preferably, the power of the phacoemulsification is 3.0k, the frequency is 20kHz, and the time is 20min to 40min.
It is understood that the first suspension of droplets is an aqueous phase containing modified titanium oxide and the second suspension is an oil phase containing activated carbon. In view of the problems that the activated carbon is a porous material and titanium oxide is difficult to uniformly disperse in the gaps of the activated carbon, the embodiment of the invention drops the water phase containing the modified titanium oxide into the oil phase containing the activated carbon and ultrasonically emulsifies the water phase, thereby forming an oil-in-water emulsion mixture to achieve the aim of promoting the uniform dispersion of the titanium oxide in the gaps of the activated carbon.
In some embodiments of the present invention, S400 specifically includes:
s410, sending the mixed solution of the step S300 into a reaction kettle, controlling the reaction kettle to be heated to a temperature of 50-55 ℃ under a closed condition, and preserving heat for 40-60 min;
s420, preserving heat and controlling the pressure of the reaction kettle to be 7.5MPa to 8.5MPa, and preserving heat and pressure for 2h to 4h;
s430, decompressing and cooling, separating solid matters from the reaction kettle, and drying to obtain the air purifying agent.
It is understood that the reaction kettle has a sealed environment, and is connected with a nitrogen delivery pipe, and a valve is arranged between the nitrogen delivery pipe and the reaction kettle. The nitrogen delivery pipe is used for delivering nitrogen to the reaction kettle so as to regulate and control the air pressure. The reaction kettle is also provided with an exhaust valve, and the exhaust valve is used for exhausting gas so as to regulate and control the air pressure under the condition of overhigh air pressure.
The mixed solution prepared in the step S300 contains sodium bicarbonate, and the sodium bicarbonate is heated to decompose at the temperature of 50-55 ℃ so that the reaction kettle is filled with carbon dioxide. Subsequently, the pressure of the reaction kettle is kept between 7.5MPa and 8.5MPa by heat preservation and control, so that the carbon dioxide reaches a supercritical state. The super-strong dissolving capacity and interface characteristic of the supercritical carbon dioxide can further promote the mutual uniform mixing of the modified titanium oxide and the activated carbon in the mixed solution, thereby achieving the purpose of further promoting the uniform dispersion of the titanium oxide in the gaps of the activated carbon. In summary, the invention can promote the uniform dispersion of the titanium oxide catalyst in the porous activated carbon by supercritical carbon dioxide by preparing the titanium oxide catalyst and the activated carbon into an emulsion mixture and heating and pressurizing the emulsion mixture, thereby improving the air purifying effect.
In some embodiments of the present invention, after S400, the preparation method further includes:
s510, according to polydopamine: trimethylmethanol= (80-90): 100 mass ratio, uniformly mixing polydopamine and trimethyl methanol to obtain a first material;
s520, vinyl trimethoxy silane: chitosan: water= (1-2): (2-4): 100 mass ratio, uniformly mixing vinyl trimethoxy silane and chitosan in water to obtain a second material;
s530, according to the first material: second material = 1:1, dropwise adding a first material into a second material, and mixing for 2-3 hours to obtain a spray;
s540, spraying: air cleaner= (5-15): 100 mass ratio, spraying the spray material on the surface of the air purifying agent, freeze-drying, heating at the temperature of 85-90 ℃ for 1-2 h, and cooling.
Preferably, in S510, polydopamine: trimethylmethanol=80: 100.
preferably, in S520, vinyltrimethoxysilane: chitosan: water = 1:3:100.
preferably, in S540, the spray: air purifier = 5:100.
preferably, in S540, the temperature of freeze-drying is-50 ℃ to-40 ℃ and the time of freeze-drying is 3 hours to 6 hours.
Preferably, in S540, the air cleaner is placed in the drum, and the spray is sprayed into the drum during the rotation or rolling.
The aim of the embodiment of the invention is to form a protective film layer on the activated carbon loaded with titanium oxide so as to achieve the purposes of dewatering, ventilation and prolonging the service cycle of the air purifying agent. In order to achieve the above object, it is necessary to spray a protective material on the surface of the air cleaner obtained in S400 so that the air cleaner forms a hydrophobic breathable film layer after being freeze-dried and heat-treated.
It is understood that the first material is a mixture of polydopamine and trimethylmethanol, and the second material is an aqueous chitosan solution added with a silane coupling agent, and the mixture spray coating can be obtained after the polydopamine and trimethylmethanol are mixed. The spray contains chitosan, and sodium alginate is added in the preparation process of the air purifying agent. Positive and negative charge attraction occurs in the spraying operation of the positively charged chitosan and the negatively charged sodium alginate, so that sprayed matters are uniformly distributed on the surface of the air purifying agent obtained in the step S400. Finally, after freeze-drying, the heat treatment temperature of 85 ℃ to 90 ℃ enables trimethyl methanol to be decomposed, and the polydopamine forms a breathable porous membrane layer with hydrophobic performance on the surface of the air purifying agent obtained in the step S400. The polydopamine has excellent adhesion capability due to strong covalent/non-covalent interaction between catechol moieties and substrates, can be deposited on the surface of active carbon, and endows the active carbon with excellent hydrophobic performance.
Example 1
The preparation method of the air purifying agent comprises the following steps:
s1, palladium chloride: terbium chloride: manganese chloride: water = 0.02:0.2:4:20, uniformly mixing palladium chloride, terbium chloride and manganese chloride in water to obtain a metal salt solution;
s2, according to sodium hexametaphosphate: titanium oxide: water = 0.2:15:100 mass ratio, uniformly mixing sodium hexametaphosphate and titanium oxide in water to obtain titanium oxide suspension;
s3, according to a metal salt solution: titanium oxide suspension = 6:100 mass ratio, dropwise adding a metal salt solution into a titanium oxide suspension, stirring, adjusting the pH value to 12 after the dropwise adding, stirring for 40min, aging for 4h, filtering, washing with acetone for 2 times, drying at 100 ℃ for 2h, and calcining at 500 ℃ for 2h to obtain modified titanium oxide;
s4, according to sodium alginate: sodium bicarbonate: modified titanium oxide: polyvinyl alcohol: water = 4:6:20:25:100 mass ratio, uniformly mixing sodium alginate, sodium bicarbonate, modified titanium oxide and polyvinyl alcohol in water to obtain a first suspension;
s5, according to Tween 80: activated carbon: vegetable oil = 6:25:100 mass ratio, adding Tween 80 and active carbon into vegetable oil, heating to 50 ℃, and stirring for 30min to obtain a second suspension;
s6, according to the first suspension liquid drops: second suspension = 10:100 mass ratio, dripping the first suspension into the second suspension of S200, and performing ultrasonic emulsification at the temperature of 40 ℃ to obtain a mixed solution;
s7, sending the mixed solution into a reaction kettle, controlling the reaction kettle to be heated to a temperature of 52 ℃ under a closed condition, and preserving heat for 40min;
s8, preserving heat and controlling the pressure of the reaction kettle to be 7.5MPa to 8.0MPa, and preserving heat and pressure for 3 hours;
s9, decompressing and cooling, separating solid matters from the reaction kettle, washing for 2 times, filtering, and drying at 60 ℃ for more than 3 hours to obtain the air purifying agent.
Example 2
The preparation method of the air purifying agent comprises the following steps:
s1, according to polydopamine: trimethylmethanol=80: 100 mass ratio, uniformly mixing polydopamine and trimethyl methanol to obtain a first material;
s2, according to vinyl trimethoxy silane: chitosan: water = 1:4:100 mass ratio, uniformly mixing vinyl trimethoxy silane and chitosan in water to obtain a second material;
s3, according to the first material: second material = 1:1, dropwise adding a first material into a second material, and mixing for 2 hours to obtain a spray;
s4, taking part of the air purifying agent obtained in the example 1, and spraying: air purifier = 10:100 mass ratio, spraying the spray material onto the surface of the air purifying agent obtained in example 1, freeze-drying, heat-treating at a temperature of 85 ℃ to 90 ℃ for 1h to 2h, and cooling.
Comparative example 1
The comparative example prepared an air cleaner, which was prepared by the following steps:
s1, palladium chloride: terbium chloride: manganese chloride: water = 0.02:0.2:4:20, uniformly mixing palladium chloride, terbium chloride and manganese chloride in water to obtain a metal salt solution;
s2, according to sodium hexametaphosphate: titanium oxide: water = 0.2:15:100 mass ratio, uniformly mixing sodium hexametaphosphate and titanium oxide in water to obtain titanium oxide suspension;
s3, according to a metal salt solution: titanium oxide suspension = 6:100 mass ratio, dropwise adding a metal salt solution into a titanium oxide suspension, stirring, adjusting the pH value to 12 after the dropwise adding, stirring for 40min, aging for 4h, filtering, washing with acetone for 2 times, drying at 100 ℃ for 2h, and calcining at 500 ℃ for 2h to obtain modified titanium oxide;
s4, according to sodium alginate: modified titanium oxide: polyvinyl alcohol: water = 4:20:25:100, uniformly mixing sodium alginate, modified titanium oxide and polyvinyl alcohol in water to obtain a first suspension;
s5, according to Tween 80: activated carbon: vegetable oil = 6:25:100 mass ratio, adding Tween 80 and active carbon into vegetable oil, heating to 50 ℃, and stirring for 30min to obtain a second suspension;
s6, according to the first suspension liquid drops: second suspension = 10:100 mass ratio, dripping the first suspension into the second suspension of S200, and performing ultrasonic emulsification at the temperature of 40 ℃ to obtain a mixed solution;
and S7, heating the mixed solution to 45 ℃ under normal pressure, preserving heat for 3 hours, separating solid matters after the heat preservation is finished, washing for 2 times, filtering, and drying at 60 ℃ for more than 3 hours to obtain the air purifying agent.
Comparative example 2
The comparative example prepared an air cleaner, which was prepared by the following steps:
s1, palladium chloride: terbium chloride: manganese chloride: water = 0.02:0.2:4:20, uniformly mixing palladium chloride, terbium chloride and manganese chloride in water to obtain a metal salt solution;
s2, according to sodium hexametaphosphate: titanium oxide: water = 0.2:15:100 mass ratio, uniformly mixing sodium hexametaphosphate and titanium oxide in water to obtain titanium oxide suspension;
s3, according to a metal salt solution: titanium oxide suspension = 6:100 mass ratio, dropwise adding a metal salt solution into a titanium oxide suspension, stirring, adjusting the pH value to 12 after the dropwise adding, stirring for 40min, aging for 4h, filtering, washing with acetone for 2 times, drying at 100 ℃ for 2h, and calcining at 500 ℃ for 2h to obtain modified titanium oxide;
s4, according to sodium alginate: modified titanium oxide: polyvinyl alcohol: water = 4:20:25:100, uniformly mixing sodium alginate, modified titanium oxide and polyvinyl alcohol in water to obtain a first suspension;
s5, according to Tween 80: activated carbon: water = 6:25:100 mass ratio, adding Tween 80 and active carbon into water, heating to 50 ℃, and stirring for 30min to obtain a second suspension;
s6, according to the first suspension liquid drops: second suspension = 10:100 mass ratio, dripping the first suspension into the second suspension of S200, and ultrasonically mixing at 40 ℃ to obtain a mixed solution;
and S7, heating the mixed solution to 45 ℃ under normal pressure, preserving heat for 3 hours, separating solid matters after the heat preservation is finished, washing for 2 times, filtering, and drying at 60 ℃ for more than 3 hours to obtain the air purifying agent.
Performance testing
The formaldehyde purification effect of the air purifier of example 1 of the present invention was tested using an environmental test chamber. The temperature in the environmental test chamber was set to 25.+ -. 1 ℃ and the relative humidity was 40.+ -. 2%. 10mL of 37% formaldehyde solution was injected into the environmental chamber and the air was circulated for 30min so that the whole chamber was filled with formaldehyde. Sampling from the positions of two sampling ports distributed on the upper and lower sides of the cabin body, determining the average concentration of formaldehyde in the cabin according to a second method gas chromatography in national standard GB/T18204.26-2016, and recording as the initial formaldehyde equilibrium concentration C 0 . Putting 20g of the air purifying agent prepared in the embodiment 1 into an air purifier, placing the air purifying agent into an environment test cabin for test, sampling from the positions of two sampling ports distributed on the upper and lower sides of the cabin body 1h and 2h after the air purifier is started, and measuring the average concentration of formaldehyde in the cabinThe degree is recorded as the equilibrium concentration C of formaldehyde after 1h 1 And formaldehyde equilibrium concentration C after 2h 2 And calculates the removal rate R of formaldehyde 1 And R is 2 . Wherein R is 1 ＝1-C 1 /C 0 ，R 2 ＝1-C 2 /C 0 . The test methods of inventive example 2 and comparative examples 1-2 were the same as in example 1. The comparative results of formaldehyde purifying effects of the air cleaners of examples 1-2 and comparative examples 1-2 of the present invention are shown in Table 1.
TABLE 1
Sequence number R 1 R 2
Example 1 73.3％ 97.6％
Example 2 72.7％ 95.5％
Comparative example 1 69.8％ 91.2％
Comparative example 2 66.2％ 86.8％
The air-purifying agents of examples 1 to 2 of the present invention were placed under an environment of 60.+ -. 1 ℃ and a relative humidity of 80.+ -. 2% for 45 days, respectively, and an acceleration experiment was conducted. The formaldehyde purification effect test was then performed in the same manner as above. The comparative results of formaldehyde purifying effects of the air cleaners of examples 1 to 2 of the present invention after the acceleration test are shown in Table 2.
TABLE 2
Sequence number R 1 R 2
Example 1 70.6％ 93.5％
Example 2 71.8％ 94.3％
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention, and the scope of the invention should be assessed accordingly to that of the appended claims.

Claims (8)

1.一种空气净化剂的制备方法，其特征在于，所述制备方法包括：1. A preparation method of air purifier, characterized in that the preparation method includes: S100、采用包括氯化钯、氯化铽、氯化锰、氧化钛、海藻酸钠、碳酸氢钠、聚乙烯醇和水的原料，制备第一悬浊液；S100. Prepare a first suspension using raw materials including palladium chloride, terbium chloride, manganese chloride, titanium oxide, sodium alginate, sodium bicarbonate, polyvinyl alcohol and water; S200、采用包括吐温、活性炭、植物油的原料，制备第二悬浊液；S200. Prepare a second suspension using raw materials including Tween, activated carbon, and vegetable oil; S300、将S100的所述第一悬浊液滴加进入S200的所述第二悬浊液并超声乳化，获得混合液；S300. Add the first suspension of S100 dropwise into the second suspension of S200 and perform ultrasonic emulsification to obtain a mixed solution; S400、将S300的所述混合液送入反应釜，加热加压处理，分离固形物并烘干，获得所述空气净化剂；S400. Send the mixed liquid of S300 into the reaction kettle, heat and pressurize it, separate the solids and dry them to obtain the air purifier; 其中，S400具体包括：Among them, S400 specifically includes: S410、将S300的所述混合液送入反应釜，在密闭条件下控制所述反应釜升温到50℃至55℃的温度条件，保温40 min至60min；S410. Send the mixed solution of S300 into the reaction kettle, control the temperature of the reaction kettle to a temperature condition of 50°C to 55°C under closed conditions, and keep it warm for 40 minutes to 60 minutes; S420、保温并控制所述反应釜的压力保持在7.5MPa至8.5MPa，保温保压2h至4h；S420. Keep the temperature and control the pressure of the reaction kettle at 7.5MPa to 8.5MPa, and keep the temperature and pressure for 2h to 4h; S430、泄压降温，从所述反应釜中分离所述固形物并烘干，获得所述空气净化剂；S430. Release the pressure and lower the temperature, separate the solid matter from the reaction kettle and dry it to obtain the air purifier; 在S400之后，所述制备方法还包括：After S400, the preparation method also includes: S510、按聚多巴胺：三甲基甲醇=（80-90）：100的质量比，将所述聚多巴胺和所述三甲基甲醇混合均匀，获得第一物料；S510. According to the mass ratio of polydopamine:trimethylcarbinol = (80-90):100, mix the polydopamine and the trimethylcarbinol evenly to obtain the first material; S520、按乙烯基三甲氧基硅烷：壳聚糖：水=（1-2）：（2-4）：100的质量比，将所述乙烯基三甲氧基硅烷和所述壳聚糖在所述水中混合均匀，获得第二物料；S520. According to the mass ratio of vinyltrimethoxysilane: chitosan: water = (1-2): (2-4): 100, the vinyltrimethoxysilane and the chitosan are placed there Mix evenly in the water to obtain the second material; S530、按第一物料：第二物料=1：1的质量比，将所述第一物料滴加进入所述第二物料，混合2h至3h，获得喷涂物；S530. According to the mass ratio of first material: second material = 1:1, add the first material dropwise into the second material, mix for 2h to 3h, and obtain the sprayed material; S540、按喷涂物：空气净化剂=（5-15）：100的质量比，将所述喷涂物喷涂至所述空气净化剂的表面，冷冻干燥、在85℃至90℃的温度条件下加热处理1h至2h后冷却。S540. According to the mass ratio of spray material: air purifier = (5-15): 100, spray the spray material onto the surface of the air purifier, freeze-dry, and heat at a temperature of 85°C to 90°C. Cool after 1h to 2h treatment. 2.根据权利要求1所述的制备方法，其特征在于，S100具体包括：2. The preparation method according to claim 1, characterized in that S100 specifically includes: S110、将所述氯化钯、所述氯化铽和所述氯化锰在所述水中混合均匀，获得金属盐溶液；S110. Mix the palladium chloride, the terbium chloride and the manganese chloride in the water evenly to obtain a metal salt solution; S120、将六偏磷酸钠和所述氧化钛在所述水中混合均匀，获得氧化钛悬浊液；S120. Mix sodium hexametaphosphate and the titanium oxide evenly in the water to obtain a titanium oxide suspension; S130、将S110的所述金属盐溶液滴加进入S120的所述氧化钛悬浊液并搅拌，滴加完毕后调节pH值至11-12并搅拌、陈化，过滤、洗涤、烘干、煅烧，获得改性氧化钛；S130. Add the metal salt solution in S110 dropwise into the titanium oxide suspension in S120 and stir. After the dropwise addition, adjust the pH value to 11-12 and stir, age, filter, wash, dry, and calcine. , obtain modified titanium oxide; S140、将所述海藻酸钠、所述碳酸氢钠、S130获得的所述改性氧化钛、所述聚乙烯醇在所述水中混合均匀，获得所述第一悬浊液。S140. Mix the sodium alginate, the sodium bicarbonate, the modified titanium oxide obtained in S130, and the polyvinyl alcohol evenly in the water to obtain the first suspension. 3.根据权利要求2所述的制备方法，其特征在于，3. The preparation method according to claim 2, characterized in that, 在S110中，氯化钯：氯化铽：氯化锰：水=（0.02-0.04）：（0.1-0.2）：（2-4）：20；和/或In S110, palladium chloride: terbium chloride: manganese chloride: water = (0.02-0.04): (0.1-0.2): (2-4): 20; and/or 在S120中，六偏磷酸钠：氧化钛：水=（0.2-0.4）：（10-20）：100；和/或In S120, sodium hexametaphosphate: titanium oxide: water = (0.2-0.4): (10-20): 100; and/or 在S130中，金属盐溶液：氧化钛悬浊液=（6-8）：100；和/或In S130, metal salt solution: titanium oxide suspension = (6-8): 100; and/or 在S140中，海藻酸钠：碳酸氢钠：改性氧化钛：聚乙烯醇：水=（2-4）：（6-8）：（10-20）：（20-30）：100。In S140, sodium alginate: sodium bicarbonate: modified titanium oxide: polyvinyl alcohol: water = (2-4): (6-8): (10-20): (20-30): 100. 4.根据权利要求2所述的制备方法，其特征在于，4. The preparation method according to claim 2, characterized in that, 在S130中，所述搅拌的时间为20min至40min；和/或In S130, the stirring time is 20min to 40min; and/or 在S130中，所述陈化的时间为4h至6h；和/或In S130, the aging time is 4h to 6h; and/or 在S130中，采用乙醇或丙酮进行所述洗涤，所述洗涤的次数为2次至3次；和/或In S130, ethanol or acetone is used to perform the washing, and the number of washings is 2 to 3 times; and/or 在S130中，所述烘干的温度为80℃至120℃，所述烘干的时间为2h至4h；和/或In S130, the drying temperature is 80°C to 120°C, and the drying time is 2h to 4h; and/or 在S130中，所述煅烧的温度为450℃至650℃，所述煅烧的时间为1h至3h。In S130, the calcination temperature is 450°C to 650°C, and the calcination time is 1h to 3h. 5.根据权利要求1所述的制备方法，其特征在于，S200具体包括：5. The preparation method according to claim 1, characterized in that S200 specifically includes: S210、按吐温：活性炭：植物油=（6-8）：（15-25）：100的质量比，将所述吐温和所述活性炭加入所述植物油中，升温并搅拌，获得所述第二悬浊液。S210. According to the mass ratio of Tween: activated carbon: vegetable oil = (6-8): (15-25): 100, add the Tween and the activated carbon to the vegetable oil, raise the temperature and stir to obtain the second Suspension. 6.根据权利要求5所述的制备方法，其特征在于，6. The preparation method according to claim 5, characterized in that, 在S210中，所述升温的温度条件为50℃至60℃；和/或In S210, the temperature condition of the heating is 50°C to 60°C; and/or 在S210中，所述搅拌的时间为20min至40min；和/或In S210, the stirring time is 20min to 40min; and/or 在S210中，所述吐温包括吐温60和/或吐温80。In S210, the Tween includes Tween 60 and/or Tween 80. 7.根据权利要求1所述的制备方法，其特征在于，S300具体包括：7. The preparation method according to claim 1, characterized in that S300 specifically includes: S310、按第一悬浊液滴：第二悬浊液=（5-15）：100的质量比，将S100的所述第一悬浊液滴加进入S200的所述第二悬浊液，在40℃至60℃的温度条件下超声乳化，获得所述混合液。S310. According to the mass ratio of first suspension droplet: second suspension liquid = (5-15): 100, add the first suspension liquid droplet in S100 into the second suspension liquid in S200, Ultrasonic emulsification is performed at a temperature of 40°C to 60°C to obtain the mixed liquid. 8.一种空气净化剂，其特征在于，所述空气净化剂采用如权利要求1至7中任一项所述的制备方法获得。8. An air purifier, characterized in that the air purifier is obtained by the preparation method according to any one of claims 1 to 7.
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