CN109349431B - Preparation method of diarrhea-preventing suckling pig feed additive - Google Patents
Preparation method of diarrhea-preventing suckling pig feed additive Download PDFInfo
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- CN109349431B CN109349431B CN201811568685.4A CN201811568685A CN109349431B CN 109349431 B CN109349431 B CN 109349431B CN 201811568685 A CN201811568685 A CN 201811568685A CN 109349431 B CN109349431 B CN 109349431B
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Abstract
The invention discloses a preparation method of a diarrhea-preventing suckling pig feed additive, belonging to the technical field of biological products for livestock, and the method comprises the following steps of (1) surface modification of palygorskite: gradient heating the palygorskite, and then modifying the palygorskite by using a high-efficiency active dispersant to obtain modified palygorskite; (2) compounding and cementing zinc oxide and palygorskite: mixing the modified palygorskite powder with the composite zinc oxide, then adding an adhesion promoter solution to perform functional compound cementation on the modified palygorskite and the zinc oxide, magnetically stirring uniformly, drying and grinding into powder to obtain the additive. In a word, the piglet feed additive prepared by the invention has a high-efficiency diarrhea prevention effect, can improve the gastrointestinal environment of piglets, and improves the gastrointestinal adaptability of piglets in the weaning period.
Description
Technical Field
The invention belongs to the technical field of biological products for livestock, and particularly relates to a preparation method and a device of a piglet antidiarrheal feed additive.
Background
Zinc is an essential trace element of animals, is a component of various enzymes, and participates in the metabolism of nutrients such as fat, carbohydrate, vitamins and the like. In a large number of researches in the fields of medicine and animal nutrition, zinc is found to have close relationship with the immune function of the body, influence the specificity, the non-specificity and the exertion of the immune function of intestinal mucosa, and have good effects on the aspects of maintaining the normal immune function of the body and preventing the invasion of bacteria and parasites. Research shows that the feed added with high-dose zinc oxide has the effects of reducing diarrhea and increasing daily gain for weaned pigs, and scholars at home and abroad widely research the application effect of adding high-dose zinc in the daily ration of weaned pigs. A large number of studies show that the addition of a proper amount of high zinc oxide in the piglet feed can effectively prevent early weaning stress syndrome of piglets, reduce the diarrhea rate of weaned piglets, improve the utilization rate of feed, promote the growth of piglets, improve the growth performance of piglets and enhance the immunologic function of piglets.
However, the use of high-dose zinc oxide also brings series adverse effects, 1) polluting the environment. Pigs have the ability to self-regulate zinc absorption and excretion to maintain zinc stability in the body. The zinc in the body is mainly excreted through intestinal tracts, and most of the zinc in the excrement comes from the unabsorbed exogenous zinc in the daily ration. In general, the zinc content in the excrement is about half of the added amount, so that high-dosage zinc is accumulated in soil to cause environmental pollution. Long term accumulation can result in soil that is no longer arable. And zinc has a great toxicity to fish and aquatic organisms. After the excessive zinc is excreted by the livestock body, the underground water can be seriously polluted, and the sustainable development of the animal husbandry is hindered. 2) Causing high zinc dependence of piglets and causing adverse effect on later growth. The phenomena of growth inhibition, feed intake reduction, pale skin, rough and curly fur and the like of the pigs can be caused by long-time high-zinc feeding. Mainly because the inhibition effect of zinc on bacteria in intestinal tracts plays a role in harmful bacteria and beneficial bacteria, when the zinc is used for a long time and is stopped, pathogenic bacteria are easier to colonize and propagate in the intestinal tracts than the beneficial bacteria, so that the intestinal flora is disordered to induce diarrhea, and the later growth is adversely affected.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method and a device of a diarrhea-preventing suckling pig feed additive.
The technical scheme of the invention is as follows: a preparation method of a diarrhea-preventing suckling pig feed additive comprises the following steps:
(1) the surface modification of the palygorskite is that the palygorskite clay is heated to the temperature of 100 ℃ and 150 ℃ in a gradient manner, then the mixture is ground into powder, the powder is added into the high-efficiency active dispersant with the mass ratio of 1 (0.1-0.5) for mixing, then deionized water with the volume ratio of 1.5 times is added, the mixture is stirred uniformly to form slurry, and the slurry is kept at the temperature of 30-40 ℃ for 2-6 hours; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 5-7 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder;
(2) and (2) compounding and cementing zinc oxide-palygorskite, namely mixing the modified palygorskite powder and the composite zinc oxide according to the mass ratio of 3:5, then adding 1.2 times of adhesion promoter solution, magnetically stirring for 8-12h at the temperature of 40-60 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain the additive.
The invention also provides a preparation method of the improved anti-diarrhea suckling pig feed additive, which comprises the following steps:
(1) surface modification of palygorskite: gradient heating the palygorskite clay to the temperature of 100-150 ℃, grinding the palygorskite clay into powder, adding the powder into the high-efficiency active dispersant with the mass ratio of 1 (0.1-0.5), mixing, then adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and preserving the temperature for 2-6h at the temperature of 30-40 ℃; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 5-7 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder;
(2) preparation of the carrier: adding the modified palygorskite powder into the composite solution for humidifying until the water content is 20-30%, transferring the modified palygorskite powder into a bulking machine for bulking under the condition of pressurization, wherein the bulking pressure is 4-10MPa, the bulking time is 1-2h, the temperature is 200-;
(3) preparing a composite zinc oxide dispersion liquid: mixing the composite zinc oxide and a dispersing agent according to a mass ratio of 100:1, and then ultrasonically oscillating and dispersing in water at a temperature of 60-100 ℃ to obtain a zinc oxide dispersion liquid;
(4) compounding and cementing zinc oxide and palygorskite: uniformly mixing the porous palygorskite carrier and the adhesion promoter in a mass ratio of 3:05, then adding 1.2 times of zinc oxide dispersion liquid, magnetically stirring for 8-12h at the temperature of 40-60 ℃ to obtain zinc oxide-palygorskite particles, drying, and grinding into powder to obtain the additive.
Furthermore, the composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1:1, and the rod-shaped body (0.5-1.0 micron) and the spindle-shaped body (1-1.5 micron) of the zinc oxide have the best bacteriostatic effect.
Further, the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 1-5 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 30-60min at the temperature of 90-110 ℃, concentrating and drying to obtain a high-efficiency active dispersant, and the high-efficiency active dispersant promotes the quick decomposition of palygorskite so as to greatly increase the effective adsorption surface area, thereby having the quick and high-efficiency adsorption effect on mycotoxin.
Further, the compound surface modifier comprises the following components in percentage by weight: 40-65% alkyl trimethyl ammonium halide, 0.1-1% cut mannase, 0.5-2% alpha-galactosidase, and the balance of sodium dodecyl sulfate, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate, and the cut mannase and the alpha-galactosidase can reduce the incidence rate of diarrhea caused by antigen factors.
Further, the composite solution comprises the following components in percentage by weight: 8-10% of porous starch, 1-3% of surfactant, 2-3% of nano silicon dioxide, 15-20% of ethanol, 9-11% of polyamino acid, 5-10% of vitamin complex, 6-12% of urea and the balance of deionized water. The porous starch is used as a pore-forming agent, and the pore-forming effect of the modified palygorskite after the swelling treatment can be obviously improved, so that the load of the palygorskite on zinc oxide is improved.
Further, gradient heating is carried out on the palygorskite, the temperature difference of 10-20 ℃ is used as a step, the temperature is increased to the maximum reaction temperature of 100-150 ℃ according to the temperature rise time of 20-40min and the heat preservation time of 60-180 min, the temperature is naturally reduced to the room temperature, and the thermal stability of the porous structure of the palygorskite can be improved through gradient heating.
Further, the modified palygorskite swelling treatment comprises the following specific steps:
s1: adding the modified palygorskite powder into the composite solution for humidifying until the water content is 20-30%, and transferring the modified palygorskite powder into a bulking machine;
s2: controlling the pressure of the bulking machine to be 2-4MPa according to the reading of a vacuum table, controlling the pressure to be 4-10MPa according to the reading of the vacuum table when the temperature reaches 200-400 ℃, keeping the pressure for 20-45min,
s3: quickly reducing the pressure to 0-1MPa, reducing the temperature to 80-100 ℃, drying at the temperature for 2-3h, stopping vacuumizing, reducing the temperature to 20-30 ℃, recovering the normal pressure, and then opening the bulking machine to take out the porous palygorskite carrier.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method heats the palygorskite clay to the temperature of 100-150 ℃ in a gradient manner, so that adsorbed water and zeolite water escape, and the palygorskite clay is mixed with the compound modifier to modify the palygorskite, so that the surface area of the palygorskite is increased; then under the conditions that the expansion pressure is 4-10MPa and the temperature is 200-400 ℃, the obtained modified palygorskite is expanded, the specific surface area of the modified palygorskite is improved, and the adsorption capacity of the palygorskite on zinc oxide is greatly improved.
(2) According to the invention, when the zinc oxide dispersion liquid is prepared, a high-efficiency active dispersing agent is added, and the zinc oxide dispersion liquid reacts with the porous palygorskite carrier, so that the product components contain a certain proportion of the high-efficiency active dispersing agent, and the dispersing agent promotes the natural mineral particles to be rapidly decomposed, thereby greatly increasing the effective adsorption surface area, and further playing a role in rapidly and efficiently adsorbing mycotoxin.
(3) The main component of the feed additive is zinc oxide-palygorskite powder, the palygorskite is specially like fish scale and the structure of a needle-shaped body overgrowing on the palygorskite powder, so that the feed additive can filter mycotoxin and nutrient components existing at the same time, and the components form selective adsorption due to different polarities. The palygorskite can completely achieve selective adsorption of mycotoxin and independently complete relatively comprehensive adsorption of mycotoxin on the premise of not adding any other components. The zinc oxide can treat the gastrointestinal diarrhea problem of pigs, and the functional compound of the palygorskite and the zinc oxide improves the antidiarrheal effect of the zinc oxide which is singly used, doubles the antidiarrheal effect, reduces the use of the zinc oxide, reduces the cost of the additive and is beneficial to environmental protection.
In a word, the piglet feed additive prepared by the invention has a high-efficiency diarrhea prevention effect, can improve the gastrointestinal environment of piglets, and improves the gastrointestinal adaptability of piglets in the weaning period.
Detailed Description
The present invention is further illustrated by the following examples 1-4 in order to more fully explain the present invention.
Example 1
A preparation method of a diarrhea-preventing suckling pig feed additive comprises the following steps:
(1) surface modification of the palygorskite, namely surface modification of the palygorskite: gradient heating is carried out on the palygorskite, the temperature difference of 10 ℃ is used as a step, the temperature rise time is 20min, the heat preservation time is 60min, the gradient heating is carried out to the highest reaction temperature of 100 ℃, the temperature is naturally reduced to the room temperature, the adsorbed water and zeolite water overflow, the internal surface area of the palygorskite is increased, meanwhile, the thermal stability of the porous structure of the palygorskite is improved, then the palygorskite is ground into powder, and the powder is added into a material with the mass ratio of 1: 0.1 of high-efficiency active dispersant, then adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and keeping the temperature for 2 hours at 30 ℃; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 5 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder; the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 1 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 30min at the temperature of 90 ℃, concentrating and drying to obtain the efficient active dispersant, and the efficient active dispersant promotes the quick decomposition of palygorskite so as to greatly increase the effective adsorption surface area, thereby having the quick and efficient adsorption effect on mycotoxin. The compound surface modifier comprises the following components in percentage by weight: 40% alkyl trimethyl ammonium halide, 0.1% cut mannase, 0.5 alpha-galactosidase, and the balance sodium dodecyl sulfate, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate, and the cut mannase and the alpha-galactosidase can reduce the incidence rate of diarrhea caused by antigen factors.
(2) And (3) compounding and cementing zinc oxide and palygorskite, namely mixing the modified palygorskite powder and the composite zinc oxide according to the mass ratio of 3:5, then adding 1.2 times of adhesion promoter solution, magnetically stirring for 8 hours at the temperature of 40 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain the additive. The composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1:1, and the rod-shaped body (0.5-1.0 micron) and the spindle-shaped body (1-1.5 micron) of the zinc oxide have the best bacteriostatic effect. The adhesion promoter is a mixture of urea-formaldehyde resin and algin according to the mass ratio of 1:1, can be suitable for various cold, hot and humid environments, prevents cracking and mildew, and can play an enteric effect and improve the stability of the powder additive.
Example 2
A preparation method of a diarrhea-preventing suckling pig feed additive comprises the following steps:
(1) surface modification of palygorskite: gradient heating is carried out on the palygorskite, the temperature difference of 10 ℃ is used as a step, the temperature rise time is 20min, the heat preservation time is 60min, the gradient heating is carried out to the highest reaction temperature of 100 ℃, the temperature is naturally reduced to the room temperature, the adsorbed water and zeolite water overflow, the internal surface area of the palygorskite is increased, meanwhile, the thermal stability of the porous structure of the palygorskite is improved, then the palygorskite is ground into powder, and the powder is added into a material with the mass ratio of 1: 0.1 of high-efficiency active dispersant, then adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and keeping the temperature for 2 hours at 30 ℃; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 5 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder; the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 1 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 30min at the temperature of 90 ℃, concentrating and drying to obtain the efficient active dispersant, and the efficient active dispersant promotes the quick decomposition of palygorskite so as to greatly increase the effective adsorption surface area, thereby having the quick and efficient adsorption effect on mycotoxin. The compound surface modifier comprises the following components in percentage by weight: 40% alkyl trimethyl ammonium halide, 0.1% cut mannase, 0.5% alpha-galactosidase, and the balance of sodium dodecyl sulfate, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate, and the cut mannase and the alpha-galactosidase in the compound surface modifier can reduce the incidence rate of diarrhea caused by antigen factors.
(2) Preparation of the carrier: adding the modified palygorskite powder into a composite solution for humidifying, controlling the water content to be 20%, transferring the modified palygorskite powder into a bulking machine for bulking by heating and pressurizing, controlling the pressure of the bulking machine to be 2MPa according to the reading of a vacuum degree gauge, controlling the pressure to be 4MPa according to the reading of the vacuum degree gauge when the temperature reaches 200 ℃, keeping the pressure for 20min, quickly reducing the pressure to 0MPa according to the reading of the vacuum degree gauge, reducing the temperature to 80 ℃, drying for 2h at the temperature, stopping vacuumizing, reducing the temperature to 20 ℃, recovering the normal pressure, and then opening the bulking machine to take out the porous palygorskite carrier, wherein the internal pore diameter of palygorskite is increased and uniformly distributed under the bulking action, and the specific surface area is increased. The composite solution comprises the following components in percentage by weight: 8% of porous starch, 1% of surfactant, 2% of nano silicon dioxide, 15% of ethanol, 9% of polyamino acid, 5% of vitamin complex, 6% of urea and the balance of deionized water. The porous starch is used as a pore-forming agent, and the pore-forming effect of the modified palygorskite after the swelling treatment can be obviously improved, so that the adsorption capacity of the palygorskite on zinc oxide is improved.
(3) Preparing a composite zinc oxide dispersion liquid: mixing the composite zinc oxide and a dispersing agent according to a mass ratio of 100:1, and then ultrasonically oscillating and dispersing in water at a temperature of 60 ℃ to obtain a zinc oxide dispersion liquid; the dispersants promote quick decomposition of the palygorskite, so that the effective adsorption surface area is greatly increased, and a quick and efficient adsorption effect on mycotoxin is achieved; the composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1:1, and the rod-shaped body (0.5-1.0 micron) and the spindle-shaped body (1-1.5 micron) of the zinc oxide have the best bacteriostatic effect.
(4) Compounding and cementing zinc oxide and palygorskite: uniformly mixing a porous palygorskite carrier and an adhesion promoter according to the mass ratio of 3:05, then adding 1.2 times of zinc oxide dispersion liquid, magnetically stirring for 8 hours at the temperature of 40 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain an additive; the adhesion promoter is a mixture of urea-formaldehyde resin and algin according to the mass ratio of 1:1, can be suitable for various cold, hot and humid environments, prevents cracking and mildew, and can play an enteric effect and improve the stability of the powder additive. The magnetic stirring accelerates the penetration of the zinc oxide dispersion liquid into the modified palygorskite, and the zinc oxide is embedded in the porous palygorskite, so that the stability of zinc oxide fixation is improved.
The addition amount of the product of the invention in the feed is 400 g/ton.
Example 3
A preparation method of a diarrhea-preventing suckling pig feed additive comprises the following steps:
(1) surface modification of palygorskite: gradient heating is carried out on the palygorskite clay, the temperature difference of 20 ℃ is used as a step, the temperature rise time is 40min, the heat preservation time is 180 min, the gradient heating is carried out to the maximum reaction temperature of 150 ℃, the temperature is naturally reduced to the room temperature, the adsorbed water and zeolite water overflow, the internal surface area of the palygorskite is increased, meanwhile, the thermal stability of the porous structure of the palygorskite is improved, then the palygorskite clay is ground into powder, and the powder is added into a material with the mass ratio of 1: 0.5 of high-efficiency active dispersant, then adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and keeping the temperature at 40 ℃ for 6 hours; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 7 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder; the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 3 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 45min at the temperature of 100 ℃, concentrating and drying to obtain the efficient active dispersant, and the efficient active dispersant promotes the quick decomposition of palygorskite so as to greatly increase the effective adsorption surface area, thereby having the quick and efficient adsorption effect on mycotoxin. The compound surface modifier comprises the following components in percentage by weight: 65% of alkyl trimethyl ammonium halide, 1% of mannase, 2% of alpha-galactosidase and the balance of sodium dodecyl sulfate, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate. The mannose cutting enzyme and the alpha-galactosidase in the compound surface modifier can reduce the diarrhea incidence caused by antigen factors.
(2) Preparation of the carrier: adding the modified palygorskite powder into a composite solution for humidifying, controlling the water content to be 30%, transferring the modified palygorskite powder into a bulking machine for pressurizing and bulking, controlling the pressure of the bulking machine to be 4MPa according to the reading of a vacuum degree gauge, controlling the pressure to be 10MPa according to the reading of the vacuum degree gauge when the temperature reaches 400 ℃, keeping the pressure for 45min, quickly reducing the pressure to be 1MPa according to the reading of the vacuum degree gauge, reducing the temperature to 100 ℃, drying for 3h at the temperature, stopping vacuumizing, reducing the temperature to 30 ℃, recovering the normal pressure, then opening the bulking machine to take out the porous palygorskite carrier, increasing the pore diameter in the palygorskite through the bulking action, uniformly distributing, and increasing the specific surface area. The composite solution comprises the following components in percentage by weight: 10% of porous starch, 3% of surfactant, 3% of nano silicon dioxide, 20% of ethanol, 11% of polyamino acid, 10% of vitamin complex, 12% of urea and the balance of deionized water. The porous starch is used as a pore-forming agent, and the pore-forming effect of the modified palygorskite after the swelling treatment can be obviously improved, so that the adsorption capacity of the palygorskite on zinc oxide is improved.
(3) Preparing a composite zinc oxide dispersion liquid: mixing the composite zinc oxide and a dispersing agent according to a mass ratio of 100:1, and then ultrasonically oscillating and dispersing in water at the temperature of 100 ℃ to obtain a zinc oxide dispersion liquid; the dispersants promote quick decomposition of the palygorskite, so that the effective adsorption surface area is greatly increased, and a quick and efficient adsorption effect on mycotoxin is achieved; the composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1:1, and the rod-shaped body (0.5-1.0 micron) and the spindle-shaped body (1-1.5 micron) of the zinc oxide have the best bacteriostatic effect.
(4) Compounding and cementing zinc oxide and palygorskite: uniformly mixing a porous palygorskite carrier and an adhesion promoter according to the mass ratio of 3:05, then adding 1.2 times of zinc oxide dispersion liquid, magnetically stirring for 10 hours at the temperature of 50 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain an additive; the adhesion promoter is a mixture of urea-formaldehyde resin and algin according to the mass ratio of 1:1, can be suitable for various cold, hot and humid environments, prevents cracking and mildew, and can play an enteric effect and improve the stability of the powder additive. The magnetic stirring accelerates the penetration of the zinc oxide dispersion liquid into the modified palygorskite, and the zinc oxide is embedded in the porous palygorskite, so that the stability of zinc oxide fixation is improved.
The addition amount of the product of the invention in the feed is 360 g/ton.
Example 4
A preparation method of a diarrhea-preventing suckling pig feed additive comprises the following steps:
(1) surface modification of palygorskite: gradient heating is carried out on the palygorskite clay, the temperature difference of 15 ℃ is used as a step, the temperature rising time is 30min, the heat preservation time is 120min, the gradient heating is carried out to the maximum reaction temperature of 125 ℃, the temperature is naturally reduced to the room temperature, the adsorbed water and zeolite water overflow, the internal surface area of the palygorskite is increased, meanwhile, the thermal stability of the porous structure of the palygorskite is improved, then the palygorskite clay is ground into powder, and the powder is added into the mixture according to the mass ratio of 1: 0.25 of high-efficiency active dispersant, then adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and keeping the temperature for 4 hours at 35 ℃; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 6 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder; the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 5 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 60min at the temperature of 110 ℃, concentrating and drying to obtain the efficient active dispersant, and the efficient active dispersant promotes the quick decomposition of palygorskite so as to greatly increase the effective adsorption surface area, thereby having the quick and efficient adsorption effect on mycotoxin. The compound surface modifier comprises the following components in percentage by weight: 55% of alkyl trimethyl ammonium halide, 0.5% of mannose, 1% of alpha-galactosidase and the balance of sodium dodecyl sulfate, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate. The mannose cutting enzyme and the alpha-galactosidase in the compound surface modifier can reduce the diarrhea incidence caused by antigen factors.
(2) Preparation of the carrier: adding the modified palygorskite powder into a composite solution for humidifying, controlling the water content to be 25%, transferring the modified palygorskite powder into a bulking machine for bulking under pressure, controlling the pressure of the bulking machine to be 7MPa according to the reading of a vacuum degree gauge, controlling the pressure to be 8MPa according to the reading of the vacuum degree gauge when the temperature reaches 300 ℃, keeping the pressure for 30min, quickly reducing the pressure to 0.5MPa according to the reading of the vacuum degree gauge, reducing the temperature to 90 ℃, drying the mixture for 2.5h at the temperature, stopping vacuumizing, reducing the temperature to 25 ℃, starting the bulking machine to take out the porous palygorskite carrier after the normal pressure is recovered, increasing the internal pore diameter of palygorskite by bulking action, uniformly distributing the pore diameter and the specific surface area. The composite solution comprises the following components in percentage by weight: 9% of porous starch, 2% of surfactant, 2.5% of nano silicon dioxide, 18% of ethanol, 10% of polyamino acid, 8% of vitamin complex, 9% of urea and the balance of deionized water. The porous starch is used as a pore-forming agent, and the pore-forming effect of the modified palygorskite after the swelling treatment can be obviously improved, so that the adsorption capacity of the palygorskite on zinc oxide is improved.
(3) Preparing a composite zinc oxide dispersion liquid: mixing the composite zinc oxide and a dispersing agent according to a mass ratio of 100:1, and then ultrasonically oscillating and dispersing in water at the temperature of 180 ℃ to obtain a zinc oxide dispersion liquid; the dispersants promote quick decomposition of the palygorskite, so that the effective adsorption surface area is greatly increased, and a quick and efficient adsorption effect on mycotoxin is achieved; the composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1:1, and the rod-shaped body (0.5-1.0 micron) and the spindle-shaped body (1-1.5 micron) of the zinc oxide have the best bacteriostatic effect.
(4) Compounding and cementing zinc oxide and palygorskite: uniformly mixing a porous palygorskite carrier and an adhesion promoter according to the mass ratio of 3:05, then adding 1.2 times of zinc oxide dispersion liquid, magnetically stirring for 12 hours at the temperature of 60 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain an additive; the adhesion promoter is a mixture of urea-formaldehyde resin and algin according to the mass ratio of 1:1, can be suitable for various cold, hot and humid environments, prevents cracking and mildew, and can play an enteric effect and improve the stability of the powder additive. The magnetic stirring accelerates the penetration of the zinc oxide dispersion liquid into the modified palygorskite, and the zinc oxide is embedded in the porous palygorskite, so that the stability of zinc oxide fixation is improved.
The addition amount of the product of the invention in the feed is 300 g/ton.
Verification of therapeutic efficacy
(1) Medicine
Comparative additives: a normal weaned piglet feed additive with zinc oxide;
test additives: the product prepared in example 2/3/4.
(2) Test method
Test subjects: 600 healthy and disease-free weaned piglets of 21-25 days old with similar gestational times and body weights and the same varieties are selected as test animals and randomly divided into 6 groups of 100 animals, wherein 3 control groups and 3 test groups.
The adding method comprises the following steps:
test group 1: mixed feeding, wherein 400g of the product in the example 2 is added into every 1000kg of feed;
test group 2: mixed eating, wherein 360g of the product in the example 3 is added into every 1000kg of feed;
test group 3: mixed feeding, wherein 300g of the product in the example 4 is added into every 1000kg of feed;
control group 1: mixed eating, 400g of contrast additive is added into every 1000kg of feed;
control group 2: mixed eating, wherein 360g of contrast additive is added into every 1000kg of feed;
control group 3: mixed feed, 300g of the comparative additive is added into every 1000kg of feed.
The measures of free ingestion, epidemic prevention and management are consistent with the daily measures. Mixing the materials according to the required dosage, wherein 5 days is one period, and two periods are continuously used.
The test data are as follows:
note: diarrhea rate (diarrhea number of head + number of days of diarrhea)/(number of head of pig tested + number of days of test) × 100%
The test result shows that: the feed for weaned piglets is added with the product of the invention, so that the diarrhea rate of the weaned piglets can be obviously reduced.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (1)
1. The preparation method of the diarrhea-preventing suckling pig feed additive is characterized by comprising the following steps:
(1) surface modification of palygorskite: taking the palygorskite clay as a step with the temperature difference of 10-20 ℃, heating for 20-40min according to the temperature rise time, keeping the temperature for 60-180 min, heating to the maximum reaction temperature of 100-150 ℃, naturally cooling to room temperature, grinding into powder, adding the powder into the efficient active dispersant with the mass ratio of 1 (0.1-0.5), mixing, adding deionized water with the volume ratio of 1.5 times, stirring uniformly to form slurry, and keeping the temperature at 30-40 ℃ for 2-6 h; after the heat preservation is finished, the slurry is dried in vacuum, the dried mixture is repeatedly washed for 5-7 times by using deionized water, and then the mixture is dried by absorbing water to obtain modified palygorskite powder;
(2) preparation of the carrier: adding the modified palygorskite powder into a composite solution for humidifying, controlling the water content to be 20-30%, transferring the modified palygorskite powder into a bulking machine, controlling the pressure of the bulking machine to be 2-4MPa according to the reading of a vacuum degree meter, controlling the pressure to be 4-10MPa according to the reading of the vacuum degree meter when the temperature reaches 200-400 ℃, keeping the pressure for 20-45min, quickly reducing the pressure to 0-1MPa according to the reading of the vacuum degree meter, reducing the temperature to 80-100 ℃, drying for 2-3h at the temperature, stopping vacuumizing, reducing the temperature to 20-30 ℃, and then opening the bulking machine to take out the porous palygorskite carrier after the temperature is restored to normal pressure;
(3) preparing a composite zinc oxide dispersion liquid: mixing the composite zinc oxide and a dispersing agent according to a mass ratio of 100:1, and then ultrasonically oscillating and dispersing in water at a temperature of 60-100 ℃ to obtain a zinc oxide dispersion liquid;
(4) compounding and cementing zinc oxide and palygorskite: uniformly mixing the porous palygorskite carrier and an adhesion promoter in a mass ratio of 3:5, then adding 1.2 times of zinc oxide dispersion liquid, magnetically stirring for 8-12h at the temperature of 40-60 ℃ to obtain zinc oxide-palygorskite particles, drying and grinding into powder to obtain an additive;
the composite zinc oxide is a mixture of rod-shaped zinc oxide and spindle-shaped zinc oxide according to the mass ratio of 1: 1;
the preparation method of the high-efficiency active dispersant comprises the following steps: dissolving a compound surface modifier in water, adding animal and vegetable gum, adding triethanolamine at the temperature of 1-5 ℃, wherein the mass ratio of the compound surface modifier to the animal and vegetable gum to the triethanolamine is 3:1:2, stirring and reacting for 30-60min at the temperature of 90-110 ℃, and concentrating and drying to obtain the efficient active dispersant;
the compound surface modifier comprises 40-65% of alkyl trimethyl ammonium halide, 0.1-1% of cutting mannase, 0.5-2% of alpha-galactosidase and the balance of sodium dodecyl sulfate according to weight percentage, wherein the sodium dodecyl sulfate can be replaced by sodium dodecyl sulfate or sodium dodecyl benzene sulfonate;
the composite solution consists of 8-10% of porous starch, 1-3% of surfactant, 2-3% of nano silicon dioxide, 15-20% of ethanol, 9-11% of polyamino acid, 5-10% of composite vitamin, 6-12% of urea and the balance of deionized water according to weight percentage;
the adhesion promoter is a mixture of urea-formaldehyde resin and algin according to the mass ratio of 1: 1.
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