CN110326625A - A kind of use in toilet nano-disinfection scavenging material and preparation method thereof - Google Patents
A kind of use in toilet nano-disinfection scavenging material and preparation method thereof Download PDFInfo
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- CN110326625A CN110326625A CN201910725661.3A CN201910725661A CN110326625A CN 110326625 A CN110326625 A CN 110326625A CN 201910725661 A CN201910725661 A CN 201910725661A CN 110326625 A CN110326625 A CN 110326625A
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Abstract
The present invention relates to a kind of use in toilet nano-disinfection scavenging materials and preparation method thereof, the preparation method comprises the following steps: during the entire process of using potassium permanganate and manganese salt as Material synthesis manganese dioxide, processing reaction system is set using ultrasonic nano makeup, and silver ammino solution and hydrogen peroxide solution are added into reaction system when reacting 5~8min, while with the rate fast cooling of 9 DEG C/min or more to -10 DEG C or less obtained use in toilet nano-disinfection scavenging materials after reacting 10~15min；Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous particle of Argent grain；The material of porous particle is manganese dioxide, average grain diameter≤30nm, specific surface area >=300g/m2, porosity of=40%, porous aperture≤5nm.Preparation method is simple for a kind of use in toilet nano-disinfection scavenging material of the invention, excellent and harmless using use in toilet nano-disinfection scavenging material bactericidal effect made from this method.
Description
Technical field
The invention belongs to scavenging material technical field, it is related to a kind of use in toilet nano-disinfection scavenging material and its preparation side
Method.
Background technique
Toilet is be unable to do without during everyone lives, the status that performer holds the balance in life.However it is hygienic
Between bacteria breed be a unavoidable problem, affect each toilet user.There are three types of modes for usual toilet sterilization: disappearing
Malicious lamp sterilization, liquid fungicide sterilization and ozone sterilization.Wherein, it can not be sterilized at sterilamp there are operating distances limited, dead angle
The disadvantages of；Liquid fungicide is mainly made of some chemical components, these ingredients may be harmful to the human body, when liquid component volatilizees
Into air, it is easy sucking human body, causes potential hazard；Ozone has harm due to being a kind of strong oxidizer, to human body, not
Approval is used to final.
Therefore, study it is a kind of for toilet sterilization new material have a very important significance.
Summary of the invention
Present invention aim to address the bactericidal effect of toilet sterilization material in the prior art difference or human body is caused to endanger
Harmful problem provides a kind of use in toilet nano-disinfection scavenging material and preparation method thereof.The present invention develops a kind of solid and kills
Bacterium material can uniformly spray the place that bacterium is easily bred in toilet, can be sterilized, while can avoid because of easily sucking
It may be injured caused by human body.
In order to achieve the above objectives, the scheme that the present invention uses is as follows:
A kind of preparation method of use in toilet nano-disinfection scavenging material, using potassium permanganate and manganese salt as Material synthesis two
During the entire process of manganese oxide, processing reaction system is set using ultrasonic nano makeup, and when reacting 5~8min to reaction system
Middle addition silver ammino solution and hydrogen peroxide solution, while with the rate fast cooling of 9 DEG C/min or more after reacting 10~15min
Use in toilet nano-disinfection scavenging material is made to -10 DEG C or less, silver ammino solution and hydrogen peroxide solution selection are on specific opportunity
It is added to there is a certain amount of manganese dioxide to generate in guarantee system, guarantees that silver can be supported on manganese dioxide.
The present invention added silver ammino solution and hydrogen peroxide solution in the synthesis process of manganese dioxide, the two can occur
Reaction generates Argent grain, since the two is to be added (when 5~8min of reaction, to have part manganese dioxide at this time in moment
Generate), therefore Argent grain can equably be supported on generated manganese dioxide surface；Manganese dioxide has bactericidal effect, kills
Bacterium mechanism are as follows: manganese dioxide has strong oxidizing property, and the sulfydryl in oxidable bacterial metabolism enzyme inactivates enzyme, makes bacterium because cannot
Metabolism and it is dead；Argent grain equally has bactericidal effect, and the sulfydryl in Argent grain and bacterial metabolism enzyme combines, and inactivates enzyme, makes
Bacterium not energy metabolism and it is dead, Argent grain can be acted on bacteria cell wall, interfere the growth of cell wall so that cell wall lose
Integrality is gone, and then kills bacterium；After the area load Argent grain of manganese dioxide, Argent grain enhances the sterilization effect of manganese dioxide
Fruit, the two have certain synergic remove, further enhance the bactericidal effect of material；
During the entire process of using potassium permanganate and manganese salt as Material synthesis manganese dioxide, place is set using ultrasonic nano makeup
Reaction system is managed, so that the partial size of nano-manganese dioxide particle, which is lower than, is not added the dioxy that reaction system preparation is set in ultrasonic nano makeup
Change the partial size of manganese nano particle, this is conducive to the specific surface area for promoting manganese dioxide nano particle, and being promoted can after specific surface area
The contact surface for enhancing manganese dioxide and bacterium, further enhances sulfydryl in manganese dioxide bacterial metabolism enzyme, inactivates enzyme, disease
Substance not energy metabolism and accelerate death；
To -10 DEG C hereinafter, fast cooling is conducive to terminate reaction rapidly, prevention generates fast cooling after reacting a period of time
Manganese dioxide particle be further enlarged, this is because manganese dioxide powder is known from experience and is gradually grown with the progress of reaction in reaction process
Greatly, and temperature is the necessary condition for promoting it to react, moment, which reduces temperature, can inhibit the progress of reaction, prevent the further of powder
It grows up, after fast cooling, has a large number of water molecules in established manganese dioxide powder internal residual, the manganese dioxide of preparation is put
It will form porous structure after liquid water evaporation under to normal temperature environment, improve the specific surface area of manganese dioxide；If temperature does not have
Reach -10 DEG C hereinafter, reaction still slowly progress, it is bigger than normal to will lead to final partial size.
As a preferred option:
A kind of preparation method of use in toilet nano-disinfection scavenging material as described above, before reaction starts, reaction system
It is made of potassium permanganate, manganese salt and water.
A kind of preparation method of use in toilet nano-disinfection scavenging material as described above, before reaction starts, reaction system
The molar ratio of middle potassium permanganate, manganese salt and water is 1:2~4:6~7, this range is optimum molar ratio, and ratio is excessive too small
It will cause to react insufficient；The concentration of silver ammino solution and hydrogen peroxide solution is respectively 15~40wt% and 10~30wt%, silver
The quality additional amount of ammonia solution and hydrogen peroxide solution is respectively 2~8 times and 0.2~0.3 times of potassium permanganate quality additional amount, this
The concentration and quality additional amount for locating silver ammino solution and hydrogen peroxide solution are also optimum valuing range, be will affect finally beyond the range
Bactericidal effect.
A kind of preparation method of use in toilet nano-disinfection scavenging material as described above, manganese salt be manganese sulfate, manganese chloride,
One or more of manganese oxalate, manganese carbonate and manganese acetate.
A kind of preparation method of use in toilet nano-disinfection scavenging material as described above, detailed process are as follows: first will be by
The reaction system of potassium permanganate, manganese salt and water composition is heated to 80~100 DEG C of reaction A min, and accompanies by ultrasonic nano makeup and set
Processing, the B min that then adds after silver ammino solution and hydrogen peroxide solution that the reaction was continued into reaction system, and accompany by ultrasonic nano
Device processing finally with the rate fast cooling of 9~20 DEG C/min to -10~-30 DEG C, and accompanies by ultrasonic nano makeup and sets place
Reason；The adduction that A is 5~8, A and B is 10~15.
A kind of preparation method of use in toilet nano-disinfection scavenging material as described above, ultrasonic nano disguise the work set
Frequency range is 20~25KHz, this range is ultrasonic wave, and ultrasonic wave has significant impact to the synthesis of material, may make particle
Be evenly distributed, size reaches nanoscale, and Ultrasonic Pulverization effect is best under this frequency, be higher or lower than this frequency crushing effect can under
Drop.
The present invention also provides using described in any item a kind of preparations of use in toilet nano-disinfection scavenging material as above
Use in toilet nano-disinfection scavenging material made from method, is negative and is loaded with the porous particle of Argent grain；The material of porous particle is
Manganese dioxide, average grain diameter≤30nm, specific surface area >=300g/m2, porosity of=40%, porous aperture≤5nm.
As a preferred option:
Use in toilet nano-disinfection scavenging material as described above, the average grain diameter of Argent grain are 0.01~0.08nm；It is more
The average grain diameter of hole particle is 10~30nm, and specific surface area is 300~600g/m2, porosity is 40~70%, porous aperture
For 3~5nm.
Use in toilet nano-disinfection scavenging material as described above, the antibiotic rate of use in toilet nano-disinfection scavenging material and
The value range of sterilizing rate is all 99~99.999%, and the antibiotic rate of toilet scavenging material and sterilizing rate be all in the prior art
90% or so, far below data of the invention.
The utility model has the advantages that
(1) preparation method of a kind of use in toilet nano-disinfection scavenging material of the invention, simple and easy, cost is not high,
Great popularization；
(2) a kind of use in toilet nano-disinfection scavenging material of the invention is a kind of novel solid fungicide, bactericidal effect
It is excellent, and be easily applied in real life.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese sulfate and water that molar ratio is 1:2:7 is heated to 80 DEG C of reaction 5min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 20KHz；
(2) 2 times and 0.2 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 15wt%) and hydrogen peroxide solution (concentration 10wt%) the reaction was continued afterwards 5min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 20KHz；
(3) it with the rate fast cooling of 9 DEG C/min to -10 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
The working frequency of device is 20KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.04nm, and the average grain diameter of porous manganese dioxide particle is 22nm, specific surface area 456g/m2, hole
Gap rate is 58%, and porous aperture is 3~5nm, and the antibiotic rate and sterilizing rate of use in toilet nano-disinfection scavenging material are respectively
99.9% and 99.5%.
Comparative example 1
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step is same as Example 1, difference
It is that processing reaction system is not set using ultrasonic nano makeup in step (1) and (2) and (3), final use in toilet nanometer obtained
Bactericidal purifying material, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, and the average grain diameter of Argent grain is 0.04nm, and porous two
The average grain diameter of manganese oxide particle is 80nm, specific surface area 12g/m2, porosity 10%, porous aperture is 5~6nm,
The antibiotic rate and sterilizing rate of use in toilet nano-disinfection scavenging material are respectively 90% and 88.9%.
Embodiment 1 and comparative example 1, which are compared, can be seen that nano-manganese dioxide grain diameter made from embodiment 1 more
It is small, specific surface area is higher, bactericidal effect is more preferable, this is because embodiment 1 during the entire process of reaction use ultrasonic nano
Device handles reaction system, so that the partial size of nano-manganese dioxide particle sets reaction system preparation lower than ultrasonic nano makeup is not added
Manganese dioxide nano particle partial size, this be conducive to promoted manganese dioxide nano particle specific surface area, thus bactericidal effect
It is promoted.
Comparative example 2
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step is same as Example 1, difference
It is in step (3) that rate of temperature fall is 5 DEG C/min, final use in toilet nano-disinfection scavenging material obtained is negative Ag-bearing
The average grain diameter of the porous manganese dioxide particle of grain, Argent grain is 0.04nm, and the average grain diameter of porous manganese dioxide particle is
40nm, specific surface area 30g/m2, porosity 24%, porous aperture is 5~6nm, and use in toilet nano-disinfection purifies material
The antibiotic rate and sterilizing rate of material are respectively 92.3% and 91.5%.
Embodiment 1 and comparative example 2 are compared to the manganese dioxide grain diameter that can be seen that and generate in embodiment 1 more
It is small, porosity is higher, bactericidal effect is more preferable, this is because fast cooling be conducive to rapidly terminate reaction, prevent generate dioxy
Change manganese particle to be further enlarged.
Comparative example 3
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step is same as Example 1, difference
It is in step (3) that for fast cooling to room temperature, final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with Argent grain
Porous manganese dioxide particle, the average grain diameter of Argent grain is 0.04nm, and the average grain diameter of porous manganese dioxide particle is 78nm,
Specific surface area is 14g/m2, porosity 13%, porous aperture is 5~6nm, and use in toilet nano-disinfection scavenging material resists
Bacterium rate and sterilizing rate are respectively 94.5% and 95.7%.
Embodiment 1 and comparative example 3 are compared to the manganese dioxide grain diameter that can be seen that and generate in embodiment 1 more
It is small, porosity is higher, bactericidal effect is more preferable, this is because being reduced to room temperature still and can not preventing continuing for reaction.
Comparative example 4
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step is same as Example 1, difference
Step (2) reaction 8min, final use in toilet nano-disinfection scavenging material obtained are carried out after being step (1) reaction 2min
It is negative and is loaded with the porous manganese dioxide particle of Argent grain, the average grain diameter of Argent grain is 0.04nm, porous manganese dioxide particle
Average grain diameter is 23nm, specific surface area 30g/m2, porosity 40%, porous aperture is 3-5nm, and use in toilet nanometer is killed
The antibiotic rate and sterilizing rate of bacterium scavenging material are respectively 94.3% and 96.1%.
Embodiment 1 and comparative example 4 are compared as can be seen that the use in toilet nano-disinfection in embodiment 1 purifies material
The bactericidal effect of material is more preferable, this is because silver ammino solution and hydrogen peroxide solution, which is added, in step (2) too early can be unfavorable for manganese dioxide
The formation of surface porosity, reduces specific surface area, to influence bactericidal effect.
Comparative example 5
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step is same as Example 1, difference
Step (2) reaction 2min, final use in toilet nano-disinfection scavenging material obtained are just carried out after being step (1) reaction 8min
It is negative and is loaded with the porous manganese dioxide particle of Argent grain, the average grain diameter of Argent grain is 0.04nm, porous manganese dioxide particle
Average grain diameter is 80nm, specific surface area 10g/m2, porosity 20%, porous aperture is 3-5nm, and use in toilet nanometer is killed
The antibiotic rate and sterilizing rate of bacterium scavenging material are respectively 90.8% and 93.7%.
Embodiment 1 and comparative example 5, which are compared, can be seen that use in toilet nano-disinfection scavenging material in embodiment 1
Bactericidal effect it is more preferable, this is because silver ammino solution is added too late in 5 step of comparative example (2) and hydrogen peroxide solution will lead to dioxy
It is more to change the increase of manganese particle, to influence bactericidal effect.
Embodiment 2
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese chloride and water that molar ratio is 1:4:6 is heated to 86 DEG C of reaction 7min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 25KHz；
(2) 5 times and 0.3 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 26wt%) and hydrogen peroxide solution (concentration 18wt%) the reaction was continued afterwards 6min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 25KHz；
(3) it with the rate fast cooling of 15 DEG C/min to -12 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 25KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.05nm, and the average grain diameter of porous manganese dioxide particle is 20nm, specific surface area 529g/m2, hole
Gap rate is 62%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.99% and 99.999%.
Embodiment 3
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese oxalate and water that molar ratio is 1:2:6 is heated to 88 DEG C of reaction 7min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 22KHz；
(2) 5 times and 0.2 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 32wt%) and hydrogen peroxide solution (concentration 24wt%) the reaction was continued afterwards 6min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 22KHz；
(3) it with the rate fast cooling of 11 DEG C/min to -16 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 22KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.03nm, and the average grain diameter of porous manganese dioxide particle is 14nm, specific surface area 548g/m2, hole
Gap rate is 65%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.91% and 99%.
Embodiment 4
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese carbonate and water that molar ratio is 1:3:6 is heated to 90 DEG C of reaction 8min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 25KHz；
(2) 8 times and 0.2 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 40wt%) and hydrogen peroxide solution (concentration 30wt%) the reaction was continued afterwards 7min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 25KHz；
(3) it with the rate fast cooling of 18 DEG C/min to -18 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 25KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.02nm, and the average grain diameter of porous manganese dioxide particle is 12nm, specific surface area 565g/m2, hole
Gap rate is 67%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99% and 99.8%.
Embodiment 5
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese acetate and water that molar ratio is 1:3:7 is heated to 100 DEG C of reaction 6min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 25KHz；
(2) 6 times and 2.6 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 35wt%) and hydrogen peroxide solution (concentration 25wt%) the reaction was continued afterwards 8min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 25KHz；
(3) it with the rate fast cooling of 20 DEG C/min to -20 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 25KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.01nm, and the average grain diameter of porous manganese dioxide particle is 10nm, specific surface area 600g/m2, hole
Gap rate is 70%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.92% and 99.98%.
Embodiment 6
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) by the mixture (mass ratio 1:1) and water of potassium permanganate, manganese sulfate and manganese chloride that molar ratio is 1:4:6
Reaction system be heated to 80 DEG C of reaction 5min, and accompany by ultrasonic nano makeup and set processing, the work that ultrasonic nano makeup is set is frequently
Rate is 20KHz；
(2) 6 times and 0.3 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 30wt%) and hydrogen peroxide solution (concentration 28wt%) the reaction was continued afterwards 7min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 20KHz；
(3) it with the rate fast cooling of 9 DEG C/min to -10 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
The working frequency of device is 20KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.08nm, and the average grain diameter of porous manganese dioxide particle is 30nm, specific surface area 300g/m2, hole
Gap rate is 40%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.5% and 99.91%.
Embodiment 7
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) by potassium permanganate that molar ratio is 1:2:7, mixture, (mass ratio is the manganese sulfate of 1:2:1, manganese carbonate and grass
Sour manganese) and the reaction system of water be heated to 95 DEG C of reaction 8min, and accompany by ultrasonic nano makeup and set processing, ultrasonic nano, which is disguised, to be set
Working frequency be 20KHz；
(2) 5 times and 0.24 times of the silver-colored ammonia that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Solution (concentration 28wt%) and hydrogen peroxide solution (concentration 22wt%) the reaction was continued afterwards 6min, and accompany by ultrasonic nano makeup
Processing is set, the working frequency that ultrasonic nano makeup is set is 20KHz；
(3) it with the rate fast cooling of 12 DEG C/min to -26 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 20KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.04nm, and the average grain diameter of porous manganese dioxide particle is 18nm, specific surface area 511g/m2, hole
Gap rate is 53%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.92% and 99.97%.
Embodiment 8
A kind of preparation method of use in toilet nano-disinfection scavenging material, basic step are as follows:
(1) reaction system of potassium permanganate, manganese sulfate and water that molar ratio is 1:2:7 is heated to 90 DEG C of reaction 5min,
And accompany by ultrasonic nano makeup and set processing, the working frequency that ultrasonic nano makeup is set is 25KHz；
(2) 5.6 times and 0.26 times of the silver that quality is respectively potassium permanganate quality in step (1) is added into reaction system
Ammonia solution (concentration 33wt%) and hydrogen peroxide solution (concentration 25wt%) the reaction was continued afterwards 10min, and accompany by ultrasonic nano
Processing is set in makeup, and the working frequency that ultrasonic nano makeup is set is 25KHz；
(3) it with the rate fast cooling of 20 DEG C/min to -30 DEG C, and accompanies by ultrasonic nano makeup and sets processing, ultrasonic nano
Disguising the working frequency set is 25KHz；
(4) by above-mentioned product filtering and washing, dry be put into Muffle furnace afterwards for 24 hours is calcined in baking oven, and calcination temperature is from room temperature
500 DEG C are raised to the rate of 5 DEG C/min, and keeps 6h, obtains use in toilet nano-disinfection scavenging material.
Final use in toilet nano-disinfection scavenging material obtained, which is negative, is loaded with the porous manganese dioxide particle of Argent grain, silver
The average grain diameter of particle is 0.02nm, and the average grain diameter of porous manganese dioxide particle is 12nm, specific surface area 575g/m2, hole
Gap rate is 68%, and porous aperture is 3~5nm, using the antibiotic rate and sterilizing rate point of use in toilet nano-disinfection scavenging material
It Wei 99.999% and 99.989%.
Claims (9)
1. a kind of preparation method of use in toilet nano-disinfection scavenging material, it is characterized in that: being original with potassium permanganate and manganese salt
Material synthesis manganese dioxide during the entire process of, using ultrasonic nano makeup set processing reaction system, and when reacting 5~8min to
Silver ammino solution and hydrogen peroxide solution are added in reaction system, while fast with the rate of 9 DEG C/min or more after reacting 10~15min
Speed is cooled to -10 DEG C or less and use in toilet nano-disinfection scavenging material is made.
2. a kind of preparation method of use in toilet nano-disinfection scavenging material according to claim 1, which is characterized in that anti-
Before should starting, reaction system is made of potassium permanganate, manganese salt and water.
3. a kind of preparation method of use in toilet nano-disinfection scavenging material according to claim 2, which is characterized in that anti-
Before should starting, the molar ratio of potassium permanganate, manganese salt and water is 1:2~4:6~7 in reaction system；Silver ammino solution and dioxygen are water-soluble
The concentration of liquid is respectively 15~40wt% and 10~30wt%, the quality additional amount respectively height of silver ammino solution and hydrogen peroxide solution
2~8 times and 0.2~0.3 times of potassium manganate quality additional amount.
4. a kind of preparation method of use in toilet nano-disinfection scavenging material according to claim 2, which is characterized in that manganese
Salt is one or more of manganese sulfate, manganese chloride, manganese oxalate, manganese carbonate and manganese acetate.
5. a kind of preparation method of use in toilet nano-disinfection scavenging material according to claim 2, which is characterized in that tool
Body process are as follows: the reaction system being made of potassium permanganate, manganese salt and water is heated to 80~100 DEG C of reaction A min, and companion first
Processing is set with ultrasonic nano makeup, then the reaction was continued the B min after addition silver ammino solution and hydrogen peroxide solution into reaction system,
And accompany by ultrasonic nano makeup and set processing, finally with the rate fast cooling of 9~20 DEG C/min to -10~-30 DEG C, and accompany by super
The processing of sound nanocrystallization device；The adduction that A is 5~8, A and B is 10~15.
6. a kind of preparation method of use in toilet nano-disinfection scavenging material according to claim 5, which is characterized in that super
The operating frequency range of sound nanocrystallization device is 20~25KHz.
7. using a kind of preparation method system of use in toilet nano-disinfection scavenging material as described in any one of claims 1 to 6
The use in toilet nano-disinfection scavenging material obtained, is loaded with the porous particle of Argent grain it is characterized in that: being negative；The material of porous particle
For manganese dioxide, average grain diameter≤30nm, specific surface area >=300g/m2, porosity of=40%, porous aperture≤5nm.
8. use in toilet nano-disinfection scavenging material according to claim 7, which is characterized in that the average grain diameter of Argent grain
For 0.01~0.08nm；The average grain diameter of porous particle is 10~30nm, and specific surface area is 300~600g/m2, porosity 40
~70%, porous aperture is 3~5nm.
9. use in toilet nano-disinfection scavenging material according to claim 7 or 8, which is characterized in that use in toilet nanometer
The antibiotic rate of bactericidal purifying material and the value range of sterilizing rate are all 99~99.999%.
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