CN113599988B - 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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- CN113599988B CN113599988B CN202110742003.2A CN202110742003A CN113599988B CN 113599988 B CN113599988 B CN 113599988B CN 202110742003 A CN202110742003 A CN 202110742003A CN 113599988 B CN113599988 B CN 113599988B
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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
-
- 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
-
- 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
-
- 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
-
- 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 zinc particle solution by using a microemulsion method; transferring the prepared zinc particle solution into a next reaction kettle, and preparing a micro-nano zinc solution A by utilizing cavitation; 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, dissolving 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 chicken farm micro-nano zinc deodorant; the invention can reduce the odor concentration inside and outside the chicken farm and improve the surrounding environment, has no corrosion, quick deodorizing effect and lasting effect, meets the requirements of environmental protection and has high cost performance.
Description
Technical Field
The invention relates to the technical field of chicken farm deodorization, in particular to a preparation method of a chicken farm micro-nano zinc deodorant.
Background
In recent years, with the continuous improvement of urban and rural residents in China, the number of chicken farms is increased year by year, and the number of chickens is increased rapidly, but due to the fact that the chicken manure in the chicken farms is not well known and managed by a plurality of farms, the chicken manure in the chicken farms is not well treated, and the environmental pollution, especially the odor pollution, is serious. The chicken manure is more easy to breed germs, flies, mosquitoes and other pests, and a plurality of diseases are transmitted and spread to surrounding villages, crowds through the flies and mosquitoes, so that the chicken manure can cause safe influence on the health of workers in a chicken farm and nearby living crowds, and can also cause pollution of nearby soil, water sources, air and the like. On the basis, the method is particularly important to solve the problem of odor of chicken farms and environmental protection for treating both principal and secondary aspect of disease, and adopts the latest developed chicken farm micro-nano zinc deodorant technology of our department. The feed additive is low in cost and can better solve the problems of frequent occurrence of intestinal diseases, odor, flies, fecal sewage, sewage and dead chickens in chicken farms.
Disclosure of Invention
The invention aims to solve the technical problem of providing the chicken farm micro-nano zinc deodorant which can be used for rapidly and effectively deodorizing, is harmless to the environment and human health, and can make up for the defects existing in the prior art.
In order to achieve the above 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 zinc particle solution by using a microemulsion method, wherein the particle size of zinc particles is 10nm-600nm;
step 2: transferring the prepared zinc particle solution into a next reaction kettle, and preparing a micro-nano zinc solution A by utilizing cavitation;
step 3, comprising the following steps:
step 3.1: taking 1-5 parts by mass of micro-nano zinc solution A and 50-200 parts by mass of water, mixing and dispersing to obtain micro-nano zinc solution B;
step 3.2: adding 50 parts by mass of micro-nano zinc solution B into 0.1-30 parts by mass of citric acid, and stirring to obtain micro-nano zinc solution C;
step 3.3: adding 50 parts by mass of micro-nano zinc solution C into 0.1-30 parts by mass of essence, and stirring to obtain micro-nano zinc solution D;
step 3.4: adding 50 parts by mass of micro-nano zinc solution D into 0.1-50 parts by mass of ethanol, and stirring to obtain micro-nano zinc solution E;
step 3.5: adding 50 parts by mass of micro-nano zinc solution E into 0.1-20 parts by mass of copper sulfate solution, and stirring to obtain micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
Further, in step 3.2, the mixing step is as follows: heating to 30-40 ℃ in a constant-temperature water bath, and reacting for 10-20min.
Further, in step 3.3, the mixing step is as follows: heating to 20-30 ℃ in a constant-temperature water bath, and reacting for 10-20min.
Further, in step 3.4, the mixing step is as follows: magnetically stirring at room temperature for 30-50min.
Further, the mass concentration of the citric acid in the step 3.2 is 50%;
further, the essence in the step 3.3 is any one of lavender essence, lemon essence, citronella essence and orange essence;
further, the mass concentration of ethanol in the step 3.4 is 95%;
further, the mass concentration of the copper sulfate solution in step 3.5 was 20%.
Further, step 1 also includes step 1.1, modulating the microemulsion to form a WPO inverse microemulsion system: dissolving a surfactant in an organic solvent, mixing with a cosurfactant and deionized water, and stirring to prepare a uniform transparent WPO reverse microemulsion system with stable thermodynamic properties; the volume ratio of the total volume of the surfactant, the cosurfactant and the organic solvent to the deionized water is 1-4:1, 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 head inward and hydrophobic organic chain outward is formed, the inner core of which can solubilize water molecules or hydrophilic substances.
Further, the organic solvent in the step 1.1 is one or more of alkane and cycloalkane;
the surfactant is a nonionic surfactant; the nonionic surfactant is one or more of polyepoxy vinyl nonylphenyl 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 further 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 5-8 hours to prepare a zinc particle solution with the particle size of 10-600 nm; the reaction temperature is 40-80 ℃, and the stirring rotation speed is 2000-5000rpm;
wherein, the volume ratio of the zinc salt aqueous solution to the hydrazine hydrate solution is 1: 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.
Further, the step 2 further includes:
step 2.1: transferring the zinc particle solution prepared in the step 1 into a next reaction kettle, stirring at 60 ℃ at 2000-5000rpm, and simultaneously introducing high-speed air flow to form cavitation; forming a fine interface between liquid and gas by utilizing the processes of forming, developing, collapsing and rebounding of cavitation bubbles in the liquid, and corroding the surface of zinc particles by utilizing the micro-jet and impact generated during collapsing of the cavitation bubbles;
step 2.2: and reacting for 5 hours to obtain the micro-nano zinc solution.
When the micro-nano zinc is prepared, cavitation is adopted to corrode the surface of zinc particles to form irregularly-shaped acute angles, and when the micro-nano zinc contacts bacteria or viruses, the micro-nano zinc shows positive charge effect and generates coulomb force with bacterial cell walls or virus cells showing negative charge effect; the attraction of coulomb force and the edge of the spike can quickly kill bacteria and viruses, which cannot continue to multiply or transfer 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 that the micro-nano zinc can continuously and permanently kill the bacteria and the viruses, and the defect of the nano zinc in the aspect of rapid sterilization performance is overcome.
The chicken farm micro-nano zinc deodorant prepared by using the micro-nano zinc as a raw material has extremely high surface energy and extremely good activity, can simultaneously perform chemical reactions such as catalysis, oxidation, complexation, adsorption and decomposition after being contacted with hydrogen sulfide and ammonia gas, and can instantaneously decompose ammonia (NH 3) and hydrogen sulfide to generate nontoxic and harmless gas. The zinc ions can react with hydrogen sulfide and ammonia in the odor and react with-NH, -COOH, -SH and the like in bacteria, so that the structure of the cells is destroyed, the effect of inhibiting the bacterial growth is achieved, and the surface of the chicken farm micro-nano zinc deodorant solution can show positive charge effect and generate coulombic force with bacterial cell walls or virus cells showing negative charge effect when contacting bacteria or viruses; the attraction of coulomb force, coupled with the edges of the spike, can rapidly kill bacteria and viruses. Meanwhile, the chicken farm micro-nano zinc deodorant can not only effectively adsorb odor molecules in the air, but also destroy the activity of cell synthetase in the adsorbed odor molecules, thereby destroying an energy metabolism system and a propagation system thereof to generate harmless substances such as N2, CO2, H2O and the like. The lavender essence, lemon essence, citronella essence, orange essence and other substances in the formula also have good auxiliary effects on deodorizing and deodorizing to a certain extent.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
1. the chicken farm micro-nano zinc deodorant prepared by the invention can inhibit bacterial growth in chicken farms and remove odor of chicken manure; the product is nontoxic, harmless, tasteless and non-irritating, can replace most disinfection and smell removal products, is beneficial to environmental protection, improves the healthy living standard, and achieves the effects of truly lasting, effective, stable, efficient, environment-friendly and tasteless disinfection and smell removal.
2. The chicken farm micro-nano zinc deodorant prepared by the method has short time and quick response, and the removal rate of hydrogen sulfide and ammonia can reach more than 99 percent;
3. the chicken farm micro-nano zinc deodorant prepared by the invention has high economic and practical cost performance and wide market application prospect.
Drawings
FIG. 1 is a microstructure of micro-nano zinc with pits obtained by cavitation effect in example 1;
FIG. 2 is a graph showing the particle size distribution of micro-nano zinc in example 1.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by persons skilled in the art without making creative efforts based on the embodiments in the present invention are all within the protection scope of the present invention.
Example 1: preparation and performance effects of micro-nano zinc solution A
(1) The preparation method of the micro-nano zinc solution A comprises the following steps:
step 1.1: 50mL of nonylphenol polyoxyethylene ether and 30mL of n-octanol are dissolved in 120mL of cyclohexane, and are stirred with 20mL of isoamyl alcohol and 200mL of deionized water to prepare a WPO reverse microemulsion system;
step 1.2: 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 are added into 3600mLWPO reverse microemulsion to be mixed, and the mixture reacts for 6.5 hours at the temperature of 65 ℃ and the rotating speed of 4600rpm to prepare zinc particle solution with the particle size of 10nm-600nm;
step 2.1: transferring the prepared zinc particle solution into a next reaction kettle, stirring at 60 ℃ and 4600rpm, and simultaneously introducing high-speed air flow to form cavitation;
step 2.2: the reaction time is 5 hours, and the micro-nano zinc solution A is prepared.
TEM images of the prepared micro-nano zinc are shown in FIG. 1.
As shown in fig. 2, zinc with particle size between micron and nanometer is prepared by microemulsion method, and the reaction condition is controlled to prepare zinc particle size:
preferred results:zinc particles 1 of (2) account for 50% of the total number, the particle size of zinc particles 1 +.> Accounting for 30% of the total.
The invention prepares the particles with the particle size in the following range by controlling the reaction conditionsAnd cavitation effect is applied to form etching pits on the particle surfaces of zinc particles so as to improve the effect of rapidly sterilizing and inactivating viruses.
It is accepted at home and abroad that when the average diameter of the nanoparticle isWhen the particles are referred to as nanoparticles. The micro-nano zinc is prepared based onThe diameter of the zinc particles is between nanometer and micrometer, so the zinc particles are called micrometer nanometer zinc, and the zinc particles are called micrometer nanometer zinc for short.
(2) Micro-nano zinc solution A sterilization effect
Preparing the prepared micro-nano zinc solution A 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 micro-nano zinc aqueous solutions with the concentration of 1000mg/kg, 800mg/kg, 500mg/kg, 400mg/kg and 300mg/kg are marked as group 5, group 4, group 3, group 2 and group 1 in sequence, the sterilization rate of the micro-nano zinc aqueous solution is measured according to a suspension quantitative method of disinfection technical Specification, and the test strains are escherichia coli, staphylococcus aureus, candida albicans and pseudomonas aeruginosa, and the test time is 20s, 30s and 60s respectively; the test results are shown in Table 1.
TABLE 1 sterilizing Effect of micro sodium Zinc solution A at different time of action
(3) Effect of inactivating virus by micro-nano zinc solution A
(a) Preparing the prepared micro-nano zinc solution A 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 micro-nano zinc aqueous solutions with the concentration of 1000mg/kg, 800mg/kg, 500mg/kg, 400mg/kg and 300mg/kg are marked as group 5, group 4, group 3, group 2 and group 1 in sequence, the virus inactivation rate of the micro-nano zinc aqueous solution is measured according to the disinfection technical Specification, and the test viruses are poliovirus, influenza A virus H1N1, enterovirus and avian influenza virus H5N1, and the test time is 10s, 20s and 30s respectively; the test results are shown in Table 2.
TABLE 2 effect of micro-nano zinc solution A on different time-inactivated viruses
(b) Preparing the prepared micro-nano zinc solution A into an aqueous solution with the concentration of 1000mg/kg, diluting the micro-nano zinc aqueous solution 10000 times to obtain a micro-nano zinc aqueous solution with the concentration of 100 mug/kg, and marking 5 parallel samples as follows: group 1, group 2, group 3, group 4 and group 5, groups 1 to 5 being associated with a concentration of 10, respectively 6 Pseudorabies virus (TCID) 50/ml and coronavirus (PEDV) are contacted and mixed for 30min, and the virus inactivation rate is measured; the test results are shown in Table 3.
TABLE 3 effect of micro-nano zinc solution A on inactivating Virus
Example 2: preparation of chicken farm micro-nano zinc deodorant
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 50 parts by mass of water, 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 micro-nano zinc solution B, adding 0.1 part by mass of citric acid into the solution B, stirring the solution in a constant-temperature water bath at 30 ℃ for 10min to dissolve the solution B, and preparing micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 0.1 part by mass of essence into the micro-nano zinc solution C, stirring the mixture in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence, and preparing micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 0.1 part by mass of ethanol into the solution D, and magnetically stirring the solution D for 30 minutes at normal temperature to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of 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 prepare micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
The mass concentration of the citric acid in the step 3.2 is 50%;
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 was 95%.
The mass concentration of the copper sulfate solution in step 3.5 was 20%.
Example 3: preparation of chicken farm micro-nano zinc deodorant
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 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 micro-nano zinc solution B, adding 5 parts by mass of citric acid into the solution B, stirring the solution in a constant-temperature water bath at 30 ℃ for 10min to dissolve the solution B, and preparing micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 5 parts by mass of essence into the solution, stirring the solution in a constant-temperature water bath at 20 ℃ for 10min to dissolve the solution, and preparing micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 10 parts by mass of ethanol into the solution D, and magnetically stirring the solution D for 30min at normal temperature to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of micro-nano zinc solution E, adding 5 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to prepare micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
The mass concentration of the citric acid in the step 3.2 is 50%;
the essence in the step 3.3 is a mixture of lavender essence and citronella essence, and the mass ratio of the lavender essence to the citronella essence is 1:1.
the mass concentration of the ethanol in the step 3.4 is 95%;
the mass concentration of the copper sulfate solution in step 3.5 was 20%.
Example 4: preparation of chicken farm micro-nano zinc deodorant
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 140 parts by mass of water, 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 micro-nano zinc solution B, adding 10 parts by mass of citric acid into the solution B, stirring the solution in a constant-temperature water bath at 30 ℃ for 10 minutes, and dissolving the solution to obtain micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 10 parts by mass of essence into the solution, stirring the solution in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence, and preparing micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 20 parts by mass of ethanol into the solution D, and magnetically stirring the solution D for 30min at normal temperature to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of micro-nano zinc solution E, adding 10 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to prepare micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
The mass concentration of the citric acid in the step 3.2 is 50%;
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.
the mass concentration of the ethanol in the step 3.4 is 95%;
the mass concentration of the copper sulfate solution in step 3.5 was 20%.
Example 5: preparation of chicken farm micro-nano zinc deodorant
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 180 parts by mass of water, 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 micro-nano zinc solution B, adding 20 parts by mass of citric acid into the solution B, stirring the solution in a constant-temperature water bath at 30 ℃ for 10min to dissolve the solution B, and preparing micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 20 parts by mass of essence into the solution, stirring the solution in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence, and preparing micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 30 parts by mass of ethanol into the solution D, and magnetically stirring the solution D for 30 minutes at normal temperature to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of micro-nano zinc solution E, adding 15 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to prepare micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
The mass concentration of the citric acid in the step 3.2 is 50%;
in the step 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.
the mass concentration of the ethanol in the step 3.4 is 95%;
the mass concentration of the copper sulfate solution in step 3.5 was 20%.
Example 6: preparation of chicken farm micro-nano zinc deodorant
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 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 micro-nano zinc solution B, adding 30 parts by mass of citric acid into the solution B, stirring the solution in a constant-temperature water bath at 30 ℃ for 10min to dissolve the solution B, and preparing micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 30 parts by mass of essence into the solution, stirring the solution in a constant-temperature water bath at 20 ℃ for 10min to dissolve the essence, and preparing micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 50 parts by mass of ethanol into the solution D, and magnetically stirring the solution D for 30min at normal temperature to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of micro-nano zinc solution E, adding 20 parts by mass of copper sulfate solution into the micro-nano zinc solution E, and stirring to prepare micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally obtaining the chicken farm micro-nano zinc deodorant.
The mass concentration of the citric acid in the step 3.2 is 50%;
in the step 3.3, the essence is a mixture of citronella essence and orange essence, and the mass ratio of the citronella essence to the orange essence is 1:1.
the mass concentration of the ethanol in the step 3.4 is 95%;
the mass concentration of the copper sulfate solution in step 3.5 was 20%.
Example 7:
the chicken farm micro-nano zinc deodorant prepared in examples 2-6 was tested and the results were as follows:
test example 1
The deodorizing effect is evaluated by an olfactory test, wherein the olfactory test method is a method for evaluating the odor intensity and the discomfort according to the smell of a person, and the characteristic parameters of malodor, including the olfactory threshold value or concentration and the sensory intensity, are measured. 10 person olfactory test groups are established, and the person is 15-50 years old and does not smoke and smell normally.
The evaluation indexes of the effect of chicken manure after being treated by the chicken farm micro-nano zinc deodorant prepared in the examples 2-6 are as follows: five indexes of 4-5 minutes, 3-4 minutes, 2-3 minutes, 1-2 minutes worse and 0 minutes ineffective are obviously used, seven groups are used, each group is counted to be equally divided, namely the optimal value is 5 minutes, the worst value is 0 minutes, after the test group is evaluated, more than 5 people of evaluation indexes can be used as test conclusion, otherwise, the test results are re-evaluated, and the specific results are shown in the following table 4.
Table 4 results of odor evaluation of the simulation of the chicken farm micro-nano zinc deodorization test
As can be seen from the data of Table 4, the chicken farm micro-nano zinc deodorant prepared in examples 2-6 can effectively deodorize chicken manure, and the chicken farm micro-nano zinc deodorant prepared in example 5 can more effectively deodorize chicken manure.
Test example 2
Selecting 6 sealable spaces, wherein each space is 2m < 3 >, 1 barrel of chicken manure of a chicken farm with malodor is placed in each space, each barrel of chicken manure weighs 8kg, the indoor temperature is controlled at 40-45 ℃, 6 spaces are selected as the deodorizing test of the chicken farm micro-nano zinc deodorant prepared in the embodiment 2-6, and the chicken farm micro-nano zinc deodorant is directly sprayed on the chicken manure of the chicken farm; after the chicken farm micro-nano zinc deodorant is sprayed, detecting ammonia gas, hydrogen sulfide concentration, methyl mercaptan concentration and dimethyl sulfide concentration in a room every 5 days, respectively calculating ammonia concentration, hydrogen sulfide concentration and odor concentration removal rate by taking a blank room as a reference, and monitoring for 30 days, wherein the specific results are shown in the 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-malodor determination-three-point comparison type stinky bag method.
Table 5 results of the simulation of the chicken farm micro-nano zinc deodorant test
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As can be seen from the data in Table 5, the chicken farm micro-nano zinc deodorant prepared in examples 2-6 can effectively deodorize, the chicken farm micro-nano zinc deodorant in example 5 has the best effect, 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%, and the chicken farm micro-nano zinc deodorant has excellent deodorizing and mosquito and fly repelling effects, and the deodorizing duration time can reach at least 30 days.
The foregoing has shown and described the basic principles, principal 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 foregoing embodiments, and that the foregoing embodiments and description are merely preferred embodiments of the invention, and are not intended to limit the invention, but that various changes and modifications may be made therein without departing from the novel spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The preparation method of the chicken farm micro-nano zinc deodorant is characterized by comprising the following steps of: step 1: preparing zinc particle solution by using a microemulsion method, wherein the particle size of zinc particles is 10nm-600nm;
step 2: transferring the prepared zinc particle solution into a next reaction kettle, and preparing a micro-nano zinc solution A by utilizing cavitation;
step 3, comprising the following steps:
step 3.1: taking 1-5 parts by mass of micro-nano zinc solution A and 50-200 parts by mass of water, mixing and dispersing to obtain micro-nano zinc solution B;
step 3.2: taking 50 parts by mass of micro-nano zinc solution B, adding 0.1-30 parts by mass of citric acid, and stirring to obtain micro-nano zinc solution C;
step 3.3: taking 50 parts by mass of micro-nano zinc solution C, adding 0.1-30 parts by mass of essence, and stirring to obtain micro-nano zinc solution D;
step 3.4: taking 50 parts by mass of micro-nano zinc solution D, adding 0.1-50 parts by mass of ethanol, and stirring to obtain micro-nano zinc solution E;
step 3.5: taking 50 parts by mass of micro-nano zinc solution E, adding 0.1-20 parts by mass of copper sulfate solution, and stirring to obtain micro-nano zinc solution F;
step 3.6: taking 50 parts by mass of micro-nano zinc solution F, stirring for 30 minutes at normal temperature until the solution is clear and transparent, and finally preparing the chicken farm micro-nano zinc deodorant;
step 2 further comprises: step 2.1: transferring the zinc particle solution prepared in the step 1 into a next reaction kettle, stirring at 60 ℃ at 2000-5000rpm, and simultaneously introducing high-speed air flow to form cavitation;
step 2.2: and reacting for 5 hours to obtain the micro-nano zinc solution.
2. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: the mixing step in step 3.2 is as follows: heating to 30-40 ℃ in a constant-temperature water bath, and reacting for 10-20min.
3. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: in step 3.3, the mixing step is as follows: heating to 20-30 ℃ in a constant-temperature water bath, and reacting for 10-20min.
4. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: in step 3.4, the mixing step is as follows: magnetically stirring at room temperature for 30-50min.
5. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: the mass concentration of the citric acid in the step 3.2 is 50%;
the essence in the step 3.3 is any one of lavender essence, lemon essence, citronella essence and orange essence;
the mass concentration of the ethanol in the step 3.4 is 95%;
the mass concentration of the copper sulfate solution in step 3.5 was 20%.
6. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: the method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: step 1 also includes step 1.1, microemulsion modulation to form WPO inverse microemulsion system: dissolving a surfactant in an organic solvent, mixing with a cosurfactant and deionized water, and stirring to prepare a WPO 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, the volume ratio of the surfactant, the cosurfactant and the organic solvent is 1-5:1:2-4.
7. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 6, which is characterized in that: the organic solvent in the step 1.1 is cycloparaffin; 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 polyepoxyvinyl nonylphenyl ether, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether or high-carbon fatty polyoxyethylene ether.
8. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 1, which is characterized in that: 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 5-8 hours 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 2000-5000rpm.
9. The method for preparing the chicken farm micro-nano zinc deodorant according to claim 8, which is characterized in that: the volume ratio of the zinc salt aqueous solution to the hydrazine hydrate solution is 1: 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.
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