CN113599988A - Preparation method of chicken farm micro-nano zinc deodorant - Google Patents
Preparation method of chicken farm micro-nano zinc deodorant Download PDFInfo
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- CN113599988A CN113599988A CN202110742003.2A CN202110742003A CN113599988A CN 113599988 A CN113599988 A CN 113599988A CN 202110742003 A CN202110742003 A CN 202110742003A CN 113599988 A CN113599988 A CN 113599988A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/58—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8612—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8634—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20792—Zinc
Abstract
The invention provides a preparation method of a chicken farm micro-nano zinc deodorant, which comprises the following steps: preparing a zinc particle solution by using a micro-emulsion method; transferring the prepared zinc particle solution to the next reaction kettle, and preparing a micro-nano zinc solution A by utilizing the cavitation phenomenon; adding water to obtain a micro-nano zinc solution B; adding citric acid, stirring and dispersing to obtain a micro-nano zinc solution C, adding essence to dissolve to obtain a micro-nano zinc solution D, adding an ethanol solution to obtain a micro-nano zinc solution E, adding a dissolved copper sulfate solution to obtain a micro-nano zinc solution F, and stirring the micro-nano zinc solution F at normal temperature to obtain the final micro-nano zinc deodorant for the chicken farm; the invention can reduce the odor concentration inside and outside the chicken farm and improve the surrounding environment, has no corrosion, quick deodorization effect and lasting effect, meets the requirement of green environmental protection, and has high cost performance.
Description
Technical Field
The invention relates to the technical field of chicken house deodorization, in particular to a preparation method of a chicken house micro-nano zinc deodorant.
Background
However, because a plurality of farms have insufficient mastery of chicken raising technology, a plurality of unscientific cognition and management means still exist, the chicken manure in the chicken farm is not treated in place, the surrounding environment pollution is caused, especially the odor pollution is serious, especially the odor problem of the chicken farm is very urgent when the odor reaches the hot high-temperature season, and not only the odor brings about great harm to the chicken and the health of breeders, but also influences on the surrounding environment and neighbors. When the chicken manure is not properly treated, germs, flies, mosquitoes and other pests are more easily bred, and many diseases are transmitted and diffused to surrounding villages and crowds through the flies and the mosquitoes, so that not only can safety hazards be caused to the body health of workers in the chicken farm and nearby resident crowds, but also pollution to nearby soil, water sources, air and the like can be caused. If the complaint leads to future inspection by the environmental protection department, the influence degree of the complaint causes the consequence far beyond your imagination, if the complaint is slight, rectification is required, and if the complaint is heavy, case penalty is even closed. Losses are then unthinkable for the chicken farm. Many chicken farms do not have large-scale infrastructure investment conditions, generally only have the most basic knowledge of chicken raising, and the deodorization and environmental protection problems are almost solved by the outsiders. On the basis, the micro-nano zinc deodorant technology newly developed by the inventor is adopted to solve the stink of the chicken farm and the environmental protection problem of treating both symptoms and root causes. The feed additive is low in cost, and can better solve the problems of frequent intestinal diseases, odor, flies, liquid dung, sewage and dead chickens in a chicken farm.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel chicken farm micro-nano zinc deodorant which can quickly and effectively deodorize, is harmless to the environment and human health, can make up for the defects in the prior art, and is green, environment-friendly, nontoxic and harmless, and the preparation method is simple.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a chicken farm micro-nano zinc deodorant comprises the following steps:
step 1: preparing a zinc particle solution by using a micro-emulsion method, wherein the particle size of zinc particles is 10nm-600 nm;
step 2: transferring the prepared zinc particle solution to the next reaction kettle, and preparing a micro-nano zinc solution A by utilizing the cavitation phenomenon;
step 3.1: mixing and dispersing 1-5 parts by mass of the micro-nano zinc solution A and 50-200 parts by mass of water to prepare a micro-nano zinc solution B;
step 3.2: adding 50 parts by mass of the micro-nano zinc solution B into 0.1-30 parts by mass of citric acid, and stirring to obtain a micro-nano zinc solution C;
step 3.3: adding 50 parts by mass of the micro-nano zinc solution C into 0.1-30 parts by mass of essence, and stirring to obtain a micro-nano zinc solution D;
step 3.4: adding 50 parts by mass of the micro-nano zinc solution D into 0.1-50 parts by mass of ethanol, and stirring to obtain a micro-nano zinc solution E;
step 3.5: adding 50 parts by mass of the micro-nano zinc solution E into 0.1-20 parts by mass of copper sulfate solution, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
Further, in step 3.2, the mixing steps are as follows: heating to 30-40 deg.C in constant temperature water bath, and reacting for 10-20 min.
Further, in step 3.3, the mixing steps are as follows: heating to 20-30 deg.C in constant temperature water bath, and reacting for 10-20 min.
Further, in step 3.4, the mixing step is as follows: magnetically stirring at room temperature for 30-50 min.
Further, the mass concentration of the citric acid in the step 3.2 is 50 percent;
further, the essence in the step 3.3 is any one of lavender essence, lemon essence, citronella essence and citrus essence;
further, the mass concentration of the ethanol in the step 3.4 is 95 percent;
further, the mass concentration of the copper sulfate solution in step 3.5 is 20%.
Further, step 1 also includes step 1.1, the microemulsion is prepared to form WPO reverse microemulsion system: dissolving a surfactant in an organic solvent, mixing with a cosurfactant and deionized water, and stirring to prepare a uniform, transparent and thermodynamic stable WPO (waterborne polyurethane) reverse microemulsion system; the volume ratio of the total volume of the surfactant, the cosurfactant and the organic solvent to the deionized water is 1-4:1, and the volume ratio of the surfactant, the cosurfactant and the organic solvent is 1-5:1: 2-4;
when the surfactant concentration exceeds the critical micelle concentration CMC, a liquid particle structure with hydrophilic polar heads inward and hydrophobic organic chains outward is formed, and the core thereof can solubilize water molecules or hydrophilic substances.
Further, in the step 1.1, the organic solvent is one or more of alkane and cyclane;
the surfactant is a nonionic surfactant; the nonionic surfactant is one or more of polyoxyethylene nonyl phenyl ether, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether or high-carbon fatty polyoxyethylene ether;
the cosurfactant is fatty alcohol.
Further, in step 1.1, the organic solvent is cyclohexane; the cosurfactant is one or more of isoamyl alcohol, n-heptanol, n-octanol, n-nonanol, n-decanol or cetyl alcohol.
Further, step 1 also includes step 1.2:
preparation of zinc particle solution: respectively adding a zinc salt aqueous solution with the concentration of 400-600 g/L and a hydrazine hydrate solution into a WPO reverse microemulsion system, stirring and mixing, and reacting for 5-8h to prepare a zinc particle solution with the particle size of 10-600 nm; the reaction temperature is 40-80 ℃, and the stirring speed is 2000-5000 rpm;
wherein the volume ratio of the zinc salt aqueous solution to the hydrazine hydrate solution is 1:1, and the volume ratio of the hydrazine hydrate solution to the WPO reversed-phase microemulsion system is 1: 3.5-4; the zinc salt is one or more of zinc sulfate, zinc nitrate, zinc citrate and zinc gluconate.
Further, the step 2 further comprises:
step 2.1: transferring the zinc particle solution prepared in the step 1 to the next reaction kettle, stirring at 60 ℃, wherein the stirring speed is 2000-5000rpm, and simultaneously introducing high-speed air flow to form a cavitation phenomenon; fine liquid-gas interphase interfaces are formed by utilizing the processes of forming, developing, collapsing and rebounding of the liquid vacuoles, and the surfaces of the zinc particles are corroded by utilizing the micro-jet flow and the impact action generated when the vacuoles collapse;
step 2.2: reacting for 5 hours to prepare the micro-nano zinc solution.
When the micro-nano zinc is prepared, the surface of zinc particles is corroded by adopting a cavitation phenomenon to form an acute angle with an irregular shape, and the micro-nano zinc shows a positive charge effect when contacting bacteria or viruses and generates coulomb force with bacterial cell walls or virus cells showing a negative charge effect; the attraction of coulomb force and the edge of the spike can kill bacteria and viruses quickly, and the bacteria and the viruses can not be propagated or transferred continuously and die; the micro-nano zinc is not consumed in the process of killing bacteria or viruses, and can continuously cause the death of the bacteria and the viruses, so the micro-nano zinc can continuously and durably kill the bacteria and the viruses, and the defect of the nano zinc in the aspect of quick bactericidal performance is overcome.
According to the invention, the micro-nano zinc is used as a raw material, the prepared chicken farm micro-nano zinc deodorant has extremely high surface energy and very good activity, and can simultaneously perform chemical reactions such as catalysis, oxidation, complexation, adsorption, decomposition and the like after being contacted with hydrogen sulfide and ammonia gas, and can instantly decompose ammonia (NH3) and hydrogen sulfide to generate nontoxic and harmless gas. The zinc ions can react with hydrogen sulfide and ammonia gas in odor and also react with-NH, -COOH, -SH and the like in bacteria, so that the structure of cells is damaged, and the effect of inhibiting the breeding of the bacteria is achieved; the attraction of coulomb force, in combination with the edges of the spikes, can rapidly kill bacteria and viruses. Meanwhile, the micro-nano zinc deodorant for the chicken farm can effectively adsorb odor molecules in the air and destroy the activity of cell synthetases in the adsorbed odor molecules, so that an energy metabolic system and a breeding system of the deodorizer are destroyed to generate harmless N2，CO2And H2O, and the like. Substances such as lavender essence, lemon essence, citronella essence, citrus essence and the like in the formula also play a good auxiliary effect on deodorization and odor removal to a certain extent.
Compared with the prior art, the invention has the following beneficial effects because the technology is adopted:
1. the micro-nano zinc deodorant for the chicken farm prepared by the invention can inhibit the breeding of bacteria in the chicken farm and deodorize chicken manure; the disinfectant is nontoxic, harmless, tasteless and non-irritant, can replace most disinfectant and odor-removing products, is beneficial to environmental protection, improves the healthy living standard, and achieves the effects of really, durably, effectively, stably, efficiently, environmentally and tasteless in disinfection, disinfection and odor removal.
2. The micro-nano zinc deodorant for chicken farms prepared by the invention has the advantages of short time, quick response and removal rate of hydrogen sulfide and ammonia of over 99 percent;
3. the micro-nano zinc deodorant for chicken farms, which is prepared by the invention, has high economic and practical performance-price ratio and wide market application prospect.
Drawings
FIG. 1 is a microstructure diagram of micro-nano zinc with etching pits obtained by utilizing cavitation effect in example 1;
fig. 2 is a distribution diagram of the particle size of the micro-nano zinc in example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work based on the embodiments of the present invention belong to the scope of the present invention.
Example 1 preparation of micro-nano Zinc solution A and Performance Effect
(1) The preparation method of the micro-nano zinc solution A comprises the following steps:
step 1.1: dissolving 50mL of nonylphenol polyoxyethylene ether and 30mL of n-octanol in 120mL of cyclohexane, and stirring with 20mL of isoamyl alcohol and 200mL of deionized water to prepare a WPO (waterborne polyurethane emulsion) reverse microemulsion system;
step 1.2: adding 1000mL of zinc salt aqueous solution (mixed solution of zinc citrate and zinc nitrate) with the concentration of 450g/L and 1000mL of hydrazine hydrate solution into 3600mL of HPO reverse microemulsion for mixing, and reacting for 6.5h at 65 ℃ and the rotating speed of 4600rpm to prepare zinc particle solution with the particle size of 10nm-600 nm;
step 2.1: transferring the prepared zinc particle solution into the next reaction kettle, stirring at 60 ℃, 4600rpm, and introducing high-speed air flow to form a cavitation phenomenon;
step 2.2: the reaction time is 5 hours, and the micro-nano zinc solution A is prepared.
A TEM image of the prepared micro-nano zinc is shown in fig. 1.
As shown in fig. 2, the microemulsion method is used to prepare zinc with the particle size between micron and nanometer, and the reaction conditions are controlled to prepare zinc particles with the particle size:
preferred results are:
the zinc particles 1 account for 50% of the total number, and the particle diameter of the zinc particles 1
Accounting for 30% of the total.
The invention controls the reaction condition to prepare the product with the grain diameter of
The micro-nano zinc and the cavitation effect are applied to form corrosion pits on the particle surfaces of zinc particles so as to improve the effect of quickly sterilizing and inactivating viruses.
It is recognized at home and abroad that the average diameter of the nano particles is
When used, the particles are referred to as nanoparticles. The diameter of the prepared zinc particles is between nanometer and micrometer, so the micro-nano zinc is called micrometer nano zinc and is called micro-nano zinc for short.
(2) Micro-nano zinc solution A sterilization effect
Preparing the micro-nano zinc solution A prepared in the above step into a micro-nano zinc aqueous solution with the concentration of 1000mg/kg, and then sequentially diluting the micro-nano zinc aqueous solution A into a solution with the concentration of: the method comprises the following steps of sequentially marking micro-nano zinc aqueous solutions with the concentrations of 800mg/kg, 500mg/kg, 400mg/kg and 300mg/kg as a group 5, a group 4, a group 3, a group 2 and a group 1, measuring the sterilization rate of the micro-nano zinc aqueous solution according to a suspension quantitative method of disinfection technical specification, wherein test strains comprise escherichia coli, staphylococcus aureus, candida albicans and pseudomonas aeruginosa for 20s, 30s and 60 s; the test results are shown in table 1.
TABLE 1 Sterilization Effect of micro-nano Zinc solution A under different time
(3) Micro-nano zinc solution A virus inactivation effect
(a) Preparing the micro-nano zinc solution A prepared in the above step into a micro-nano zinc aqueous solution with the concentration of 1000mg/kg, and then sequentially diluting the micro-nano zinc aqueous solution A into a solution with the concentration of: the method comprises the following steps of sequentially marking micro-nano zinc aqueous solutions with the concentrations of 1000mg/kg, 800mg/kg, 500mg/kg, 400mg/kg and 300mg/kg as a group 5, a group 4, a group 3, a group 2 and a group 1, determining the virus inactivation rate of the micro-nano zinc aqueous solution according to disinfection technical specifications, testing the viruses to be poliovirus, influenza A virus H1N1, enterovirus and avian influenza virus H5N1 for 10s, 20s and 30 s; the test results are shown in table 2.
TABLE 2 Virus inactivating effect of micro-nano zinc solution A on different time
(b) Preparing the micro-nano zinc solution A prepared in the above step into an aqueous solution with the concentration of 1000mg/kg, diluting the micro-nano zinc aqueous solution by 10000 times to obtain a micro-nano zinc aqueous solution with the concentration of 100 mug/kg, and taking 5 parallel samples to mark as: group 1, group 2, group 3, group 4 and group 5, groups 1 to 5 respectively with a concentration of 106TCID50Mixing pseudorabies virus and coronavirus (PEDV) in a contact manner for 30min, and measuring the virus inactivation rate; the test results are shown in table 3.
TABLE 3 Virus inactivating effect of micro-nano zinc solution A
Example 2: preparation of micro-nano zinc deodorant for chicken farm
A preparation method of a chicken farm micro-nano zinc deodorant comprises the following specific steps:
step 3.1: adding 1 part by mass of the micro-nano zinc solution A prepared in example 1 into 50 parts by mass of water, heating to 30 ℃ in a constant-temperature water bath for 4 hours, and stirring and dispersing to obtain a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 0.1 part by mass of citric acid into the micro-nano zinc solution B, and stirring the mixture in a constant-temperature water bath at the temperature of 30 ℃ for 10min to dissolve the mixture to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 0.1 part by mass of essence into the micro-nano zinc solution C, and stirring the mixture in a constant-temperature water bath at 20 ℃ for 10min to dissolve the mixture to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 0.1 part by mass of ethanol into the micro-nano zinc solution D, and magnetically stirring the mixture at normal temperature for 30min to prepare a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 0.1 part by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
In the step 3.2, the mass concentration of the citric acid is 50 percent;
in the step 3.3, the essence is a mixture of lavender essence and lemon essence, and the mass ratio of the lavender essence to the lemon essence is 1: 1.
The mass concentration of ethanol in step 3.4 is 95%.
The mass concentration of the copper sulfate solution in step 3.5 is 20%.
Example 3: preparation of micro-nano zinc deodorant for chicken farm
A preparation method of a chicken farm micro-nano zinc deodorant comprises the following specific steps:
step 3.1: adding 1 part by mass of the micro-nano zinc solution A prepared in the example 1 into 100 parts by mass of water, heating the solution to 30 ℃ in a constant-temperature water bath for 4 hours, and stirring and dispersing the solution to prepare a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 5 parts by mass of citric acid into the micro-nano zinc solution B, and stirring in a constant-temperature water bath at 30 ℃ for 10min to dissolve the citric acid to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 5 parts by mass of essence into the micro-nano zinc solution C, and stirring in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 10 parts by mass of ethanol into the micro-nano zinc solution D, and magnetically stirring the mixture for 30min at normal temperature to prepare a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 5 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
In the step 3.2, the mass concentration of the citric acid is 50 percent;
in the step 3.3, the essence is a mixture of lavender essence and citronella essence, and the mass ratio of the lavender essence to the citronella essence is 1: 1.
In the step 3.4, the mass concentration of the ethanol is 95 percent;
the mass concentration of the copper sulfate solution in step 3.5 is 20%.
Example 4: preparation of micro-nano zinc deodorant for chicken farm
A preparation method of a chicken farm micro-nano zinc deodorant comprises the following specific steps:
step 3.1: adding 140 parts by mass of water into 1 part by mass of the micro-nano zinc solution A prepared in example 1, heating to 30 ℃ in a constant-temperature water bath for 4 hours, and stirring and dispersing to prepare a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 10 parts by mass of citric acid into the micro-nano zinc solution B, and stirring the mixture in a constant-temperature water bath at the temperature of 30 ℃ for 10min to dissolve the citric acid to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 10 parts by mass of essence into the micro-nano zinc solution C, and stirring the mixture in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 20 parts by mass of ethanol, and magnetically stirring at normal temperature for 30min to prepare a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 10 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
In the step 3.2, the mass concentration of the citric acid is 50 percent;
in the step 3.3, the essence is a mixture of lavender essence and citrus essence, and the mass ratio of the lavender essence to the citrus essence is 1: 1.
In the step 3.4, the mass concentration of the ethanol is 95 percent;
the mass concentration of the copper sulfate solution in step 3.5 is 20%.
Example 5: preparation of micro-nano zinc deodorant for chicken farm
A preparation method of a chicken farm micro-nano zinc deodorant comprises the following specific steps:
step 3.1: adding 180 parts by mass of water into 1 part by mass of the micro-nano zinc solution A prepared in example 1, heating to 30 ℃ in a constant-temperature water bath for 4 hours, and stirring and dispersing to prepare a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 20 parts by mass of citric acid into the micro-nano zinc solution B, and stirring in a constant-temperature water bath at 30 ℃ for 10min to dissolve the citric acid to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 20 parts by mass of essence into the micro-nano zinc solution C, and stirring in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 30 parts by mass of ethanol, and magnetically stirring at normal temperature for 30min to prepare a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 15 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
In the step 3.2, the mass concentration of the citric acid is 50 percent;
and 3.3, the essence is a mixture of lemon essence and citronella essence, and the mass ratio of the lemon essence to the citronella essence is 1: 1.
In the step 3.4, the mass concentration of the ethanol is 95 percent;
the mass concentration of the copper sulfate solution in step 3.5 is 20%.
Example 6: preparation of micro-nano zinc deodorant for chicken farm
A preparation method of a chicken farm micro-nano zinc deodorant comprises the following specific steps:
step 3.1: adding 1 part by mass of the micro-nano zinc solution A prepared in the example 1 into 200 parts by mass of water, heating the solution to 30 ℃ in a constant-temperature water bath for 4 hours, and stirring and dispersing the solution to obtain a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 30 parts by mass of citric acid into the micro-nano zinc solution B, and stirring in a constant-temperature water bath at 30 ℃ for 10min to dissolve the citric acid to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 30 parts by mass of essence into the micro-nano zinc solution C, and stirring in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 50 parts by mass of ethanol, and magnetically stirring at normal temperature for 30min to prepare a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 20 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for chicken farms.
In the step 3.2, the mass concentration of the citric acid is 50 percent;
and 3.3, the essence is a mixture of citronella essence and citrus essence, and the mass ratio of the citronella essence to the citrus essence is 1: 1.
In the step 3.4, the mass concentration of the ethanol is 95 percent;
the mass concentration of the copper sulfate solution in step 3.5 is 20%.
Example 7:
the chicken farm micro-nano zinc deodorant prepared in the example 2-6 is detected, and the result is as follows:
test example 1
And (3) evaluating the deodorization effect by adopting an olfactory test, wherein the olfactory test method is a method for evaluating the odor intensity and the fit and discomfort according to the human olfactory, and measuring the characteristic parameters of the malodor, including an olfactory threshold value or concentration and sensory intensity. A10-person olfactory test group was established, which was 15-50 years old and had no smoking and normal olfactory sensation.
The effect evaluation indexes of the chicken manure after being treated by the micro-nano zinc deodorant for the chicken farm prepared in the embodiment 2-6 are as follows: the five indexes of 4-5 points, 3-4 points, 2-3 points, 1-2 points and 0 point are obvious, the total number of the five indexes is seven, the statistical average point of each group is 5 points optimally, the worst point is 0 point, after the test group is evaluated, the evaluation indexes exceeding more than 5 persons can be used as a test conclusion, otherwise, the evaluation is carried out again, and the specific result is shown in the following table 4.
Table 4 odor evaluation results of micro-nano zinc deodorization test of simulated chicken farm
As can be seen from the data in Table 4, the micro-nano zinc deodorant for chicken farms prepared in examples 2 to 6 can effectively deodorize, and the micro-nano zinc deodorant for chicken farms prepared in example 5 can more effectively deodorize chicken manure in chicken farms.
Test example 2
6 closable spaces each of 2m were selected3In each space, 1 barrel of chicken manure in a chicken farm which generates foul smell is placed, the weight of each barrel of chicken manure is 8kg, the indoor temperature is controlled to be 40-45 ℃, and 6 spaces are selected as examples2-6, directly spraying the micro-nano zinc deodorant on chicken manure in the chicken farm for a chicken farm micro-nano zinc deodorant deodorization test; after the micro-nano zinc deodorant is sprayed in a chicken farm, the ammonia gas concentration, the hydrogen sulfide concentration, the methyl mercaptan concentration and the methyl sulfide concentration in a room are detected every 5 days, the removal rates of the ammonia concentration, the hydrogen sulfide concentration and the odor concentration are respectively calculated by taking a blank room as a reference, the monitoring time is 30 days, and specific results are shown in a table 5 below. The detection method comprises GB/T14678-1993 air quality-hydrogen sulfide, methyl mercaptan and methyl sulfide determination-gas chromatography, GB/T14675-199 air quality-determination of malodor-three-point comparison type odor bag method.
TABLE 5 results of the micronano zinc deodorant test in simulated chicken farms
As can be seen from the data in table 5, the micro-nano zinc deodorant for chicken farms prepared in examples 2 to 6 can effectively deodorize, the micro-nano zinc deodorant for chicken farms of example 5 has the best effect, and the average removal rates of ammonia gas, hydrogen sulfide, methyl mercaptan and methyl sulfide in 30 days are respectively 98.6%, 98.2%, 98.3% and 98.4%.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the preferred embodiments of the invention and described in the specification are only preferred embodiments of the invention and are not intended to limit the invention, and that various changes and modifications may be made without departing from the novel spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of a chicken farm micro-nano zinc deodorant is characterized by comprising the following steps:
step 1: preparing a zinc particle solution by using a micro-emulsion method, wherein the particle size of zinc particles is 10nm-600 nm;
step 2: transferring the prepared zinc particle solution to the next reaction kettle, and preparing a micro-nano zinc solution A by utilizing the cavitation phenomenon;
step 3, comprising the following steps:
step 3.1: mixing and dispersing 1-5 parts by mass of the micro-nano zinc solution A and 50-200 parts by mass of water to prepare a micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of the micro-nano zinc solution B, adding 0.1-30 parts by mass of citric acid, and stirring to obtain a micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of the micro-nano zinc solution C, adding 0.1-30 parts by mass of essence, and stirring to obtain a micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of the micro-nano zinc solution D, adding 0.1-50 parts by mass of ethanol, and stirring to obtain a micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of the micro-nano zinc solution E, adding 0.1-20 parts by mass of copper sulfate solution, and stirring to obtain a micro-nano zinc solution F;
step 3.6: and (3) taking 50 parts by mass of the micro-nano zinc solution F, stirring at normal temperature for 30 minutes until the solution is clear and transparent, and finally preparing the micro-nano zinc deodorant for the chicken farm.
2. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: the mixing step in step 3.2 is as follows: heating to 30-40 deg.C in constant temperature water bath, and reacting for 10-20 min.
3. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: in step 3.3, the mixing steps are as follows: heating to 20-30 deg.C in constant temperature water bath, and reacting for 10-20 min.
4. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: in step 3.4, the mixing steps are as follows: magnetically stirring at room temperature for 30-50 min.
5. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: in the step 3.2, the mass concentration of the citric acid is 50 percent;
in the step 3.3, the essence is any one of lavender essence, lemon essence, citronella essence and citrus essence;
in the step 3.4, the mass concentration of the ethanol is 95 percent;
the mass concentration of the copper sulfate solution in step 3.5 is 20%.
6. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: the preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: step 1 also comprises step 1.1, preparing the microemulsion to form a WPO reverse microemulsion system: dissolving a surfactant in an organic solvent, mixing with a cosurfactant and deionized water, and stirring to prepare a WPO (waterborne polyurethane emulsion) reverse microemulsion system; the volume ratio of the total volume of the surfactant, the cosurfactant and the organic solvent to the deionized water is 1-4:1, and the volume ratio of the surfactant, the cosurfactant and the organic solvent is 1-5:1: 2-4.
7. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 6, which is characterized by comprising the following steps: in the step 1.1, the organic solvent is one or more of alkane and cyclane; the cosurfactant is one or more of isoamyl alcohol, n-heptanol, n-octanol, n-nonanol, n-decanol or cetyl alcohol;
the surfactant is a nonionic surfactant; the nonionic surfactant is one or more of polyoxyethylene nonyl phenyl ether, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether or high-carbon fatty polyoxyethylene ether.
8. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: step 1 also includes step 1.2, preparation of zinc particle solution: respectively adding a zinc salt aqueous solution with the concentration of 400-600 g/L and a hydrazine hydrate solution into a WPO reverse microemulsion system, stirring and mixing, and reacting for 5-8h to prepare a zinc particle solution with the particle size of 10-600 nm; wherein the reaction temperature is 40-80 ℃, and the stirring speed is 2000-5000 rpm.
9. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 8, characterized by comprising the following steps: the volume ratio of the zinc salt aqueous solution to the hydrazine hydrate solution is 1:1, and the volume ratio of the hydrazine hydrate solution to the WPO reverse microemulsion system is 1: 3.5-4; the zinc salt is one or more of zinc sulfate, zinc nitrate, zinc citrate and zinc gluconate.
10. The preparation method of the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized by comprising the following steps: the step 2 further comprises:
step 2.1: transferring the zinc particle solution prepared in the step 1 to the next reaction kettle, stirring at 60 ℃, wherein the stirring speed is 2000-5000rpm, and simultaneously introducing high-speed air flow to form a cavitation phenomenon;
step 2.2: reacting for 5 hours to prepare the micro-nano zinc solution.
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