CN101731451B - Compound mouldproof agent with acidizing effect and preparation method thereof - Google Patents
Compound mouldproof agent with acidizing effect and preparation method thereof Download PDFInfo
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- CN101731451B CN101731451B CN 201010019554 CN201010019554A CN101731451B CN 101731451 B CN101731451 B CN 101731451B CN 201010019554 CN201010019554 CN 201010019554 CN 201010019554 A CN201010019554 A CN 201010019554A CN 101731451 B CN101731451 B CN 101731451B
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Abstract
The invention provides a compound mouldproof agent with the acidizing effect and a preparation method thereof. The compound mouldproof agent comprises the following components in parts by weight: 20-50 parts of propionic acid-ammonium propionate-ammonium dipropionate mixture, 5-15 parts of glacial acetic acid-ammonium acetate-ammonium diacetate mixture, 2-10 parts of benzoic acid, 1-3 parts of dehydroacetic acid and/or sorbic acid and 37-55 parts of vectors. The invention also provides the preparation method of the compound mouldproof agent, which is characterized by evenly stirring the mixture of the 20-50 parts of propionic acid-ammonium propionate-ammonium dipropionate mixture, the 5-15 parts of glacial acetic acid-ammonium acetate-ammonium diacetate intermediate product components, the 2-10 parts of benzoic acid, the 1-3 parts of dehydroacetic acid and/or sorbic acid and the 37-55 parts of vectors, filtering, inspecting and packaging, thus obtaining the compound mouldproof agent. The compound mouldproof agent has double functions of mould proofing and acidizing, is synergistic, avoids antagonism and is simple in preparation, low in cost and high in application value.
Description
Technical field
The present invention relates to feed addictive, relate in particular to a kind of composite mildew inhibitor and preparation method thereof, belong to feed safety and preservation field with acidizing effect.
Background technology
Limited natural resource and the disease, poisoning and the pollution that become increasingly complex, and people's living standard improve constantly and require have contradiction between continuing to improve, this impels the feed industry must fast development, growth scale and require feed quality to improve constantly.But Global Climate worsens day by day, like the increasing of harsh arid, the heavy rain that falls by force, the temperature temperature difference, swift and violent typhoon etc., and frequent in addition changeable influenza, defeated the bringing on a disaster property influence of production, storing of giving feed: mouldy.Feed is mouldy, i.e. mould and corruptibility bacteria breed breeding produces toxin; Destroy nutritional labeling, resolve into small-molecule substance such as aldehyde, the ketone etc. of peculiar smell, palatability descends; Animal poisons, and also passes to human body through food chain and produces disease, to bringing on a disaster property of health of people consequence; Cause serious economy loss simultaneously, hinder the development of feed industry.For preventing the generation of feed mold, at present, the most simple and easy to do, cost-effective way is to add anti-mould fresh keeping agent.
In feeding, particularly the interior pH value of weaned piglet metenteron is higher for livestock and poultry, propepsin Tunization, and a little less than the digestion secretion, indigestion generally appears in livestock and poultry.The pathogenic microorganism breeding causes diarrhea in the alimentary canal.Gastric emptying is anti-soon stress be poor, and a little less than the immunity of organisms, but antibiotic use will bring pollution again.Overcoming the above problems the most at present, way is to add green organic type acidulant.
So far; Feed Enterprise all is to realize mildew-resistant and acidifying function through adding two products that separate of mould inhibitor and acidulant respectively aborning; Do not get up the design of a large amount of acid effect science of mould inhibitor come in dual-purpose acidifying and acidulant dual-purpose mildew-resistant effect from integration; Just be prone in use some sour abuse or vacancy, equally also can increase the probability that produces antagonistic effect.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of composite mildew inhibitor that has mildew-resistant and acidifying dual-use function simultaneously and preparation method thereof, and Synergistic between dual-use function is avoided antagonism, and this acidifying composite mildew inhibitor prepare simple and easy, cost is low, using value is high.
In order to realize the object of the invention, one aspect of the present invention provides a kind of composite mildew inhibitor with acidizing effect, it is characterized in that, each composition weight umber of said composite mildew inhibitor is respectively:
Propionic acid-propionic acid ammonium-two propionic acid ammonium mixture 20-50;
Glacial acetic acid-ammonium acetate-two ammonium acetate mixture 5-15;
Benzoic acid 2-10;
Dehydroacetic acid and/or sorbic acid 1-3;
Carrier 37-55.
" propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures " that the present invention adopted is meant, uses content >=99.0% propionic acid (commercially available) and liquefied ammonia or carbonic hydroammonium, ammonium carbonate to carry out the mixture that chemical reaction makes.This process is specially: liquefied ammonia is through 40-45 ℃ of ammonia preheater preheating, and pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of propionic acid, and, open water quench simultaneously with 60-80r/ minute speed stirring reaction; Make the interior exothermic temperature of still be no more than 100-110 ℃, free propionic acid weight percentage drops to the ratio that accounts for whole liquid in the sampling detection reaction still, stops to feed ammonia; Continue to stir 2-3 minute the cooling blanking.Detection method is preferably the conventional acid alkali titration.Free propionic acid content preferably is controlled at weight content 65%-80% in " propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures " system of being somebody's turn to do, and all the other are propionic acid ammonium, two propionic acid ammonium and water, and content is not limit.In addition; Propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures also can be meant; Through in propionic acid, dropping into propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that carbonic hydroammonium or ammonium carbonate make; Wherein, feed intake ratio of weight and number=(3.6-6.5) of propionic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(5.5-10) of propionic acid and ammonium carbonate: 1.
" glacial acetic acid-ammonium acetate-two ammonium acetate mixtures " that the present invention adopted is meant, uses content >=99.0% glacial acetic acid (commercially available) and liquefied ammonia or carbonic hydroammonium, ammonium carbonate to carry out the mixture that chemical reaction makes.This process is specially: liquefied ammonia is through 40-45 ℃ of ammonia preheater preheating, and pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of glacial acetic acid, and, open water quench simultaneously with 60-80r/ minute speed stirring reaction; Make the interior exothermic temperature of still be no more than 100-110 ℃, free acetic acid weight percentage drops to the ratio that accounts for whole liquid in the sampling detection reaction still, stops to feed ammonia; Continue to stir 2-3 minute the cooling blanking.Detection method is preferably the conventional acid alkali titration.Free acetic acid content preferably is controlled at weight content 70%-80% in " glacial acetic acid-ammonium acetate-two ammonium acetate mixtures " system of being somebody's turn to do, and all the other are ammonium acetate, two ammonium acetate and water, and content is not limit.In addition; Glacial acetic acid-ammonium acetate-two ammonium acetate mixtures also can be meant; Through in glacial acetic acid, dropping into glacial acetic acid-ammonium acetate-two ammonium acetate mixtures that carbonic hydroammonium or ammonium carbonate make; Wherein, feed intake ratio of weight and number=(3.1-5.6) of glacial acetic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(4.6-8.5) of glacial acetic acid and ammonium carbonate: 1.
The benzoic acid (commercially available) that the present invention adopts, requirement is feed grade or food-grade, content >=99.0%.
Dehydroacetic acid or sorbic acid (commercially available) that the present invention adopts, requirement is feed grade or food-grade, content >=99%.
Preferably, the carrier of the present invention's employing is one or more in activation silicon dioxide powder, fine perlite, zeolite powder, the water.More preferably, the carrier that the present invention adopts is activation silica (commercially available), requires absorption value>=2.5, moisture≤8%, pH value≤7; Fine perlite (commercially available), granularity>=40 orders; Zeolite powder (commercially available), pH value≤7.
Preferably, the present invention further comprises 1-3 weight portion ethoxyquinoline and 2-3 weight portion propane diols, and wherein, ethoxyquinoline is crude oil or pulvis (commercially available), ethoxyquinoline content >=95.0%.Prevention causes the approach that goes mouldy because of the oxidation factor, plays antioxidation; Propane diols (commercially available) is beneficial to liquid as wetting agent and in feed, mixes.
Composite mildew inhibitor of the present invention is solid powder or liquid preparation.The present invention can be used as livestock and poultry, feeding additive aquatic animal uses, and its addition in feed is the 0.05%-0.3% of feed weight.
The present invention provides a kind of preparation method of composite mildew inhibitor on the other hand, and step is following:
(1), feeds and be added with in the reactor of an amount of propionic acid stirring with after the liquefied ammonia preheating; Cooling when free propionic acid weight percentage accounts for the 65%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures.
(2), feed and be added with in the reactor of an amount of glacial acetic acid stirring with after the liquefied ammonia preheating; Cooling when free acetic acid weight percentage accounts for the 70%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures.
(3) take by weighing 20-50 weight portion propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5-15 weight portion glacial acetic acid-ammonium acetate-two ammonium acetate mixtures, mix;
(4) take by weighing 2-10 weight portion benzoic acid, 1-3 weight portion dehydroacetic acid or sorbic acid, 1-3 weight portion ethoxyquinoline oil and 2-3 weight portion propane diols; Put in the said mixture of step (3), stir, the water that adds the 37-55 weight portion again stirs; Filter; Check, can promptly gets the composite mildew inhibitor liquid preparation.
Wherein, propionic acid-propionic acid ammonium-two propionic acid ammonium preparation process of mixture are following in the step (1): through 40-45 ℃ of ammonia preheater preheating, pressure is controlled 1-1.5MPa with liquefied ammonia; Again after disperser disperses, evenly slowly feed and be added with in the agitated reactor of an amount of propionic acid, and with 60-80r/ minute speed stirring reaction; Open water quench simultaneously, make the interior exothermic temperature of still be no more than 100-110 ℃, sampling detects when free propionic acid weight percentage drops to the 65%-80% that accounts for whole liquid in (conventional acid alkali titration) agitated reactor; Stop to feed ammonia; Continue to stir 2-3 minute, the cooling blanking promptly gets;
Glacial acetic acid-ammonium acetate-two ammonium acetate preparation process of mixture are following in the step (2): through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5MPa is again after disperser disperses with liquefied ammonia; Evenly slowly feed and be added with in the agitated reactor of an amount of glacial acetic acid, and, open water quench simultaneously with 60-80r/ minute speed stirring reaction; Make the interior exothermic temperature of still be no more than 100-110 ℃; Sampling detects when free acetic acid weight percentage drops to the 70%-80% that accounts for whole liquid in (conventional acid alkali titration) agitated reactor, stops to feed ammonia, continues to stir 2-3 minute; The cooling blanking promptly gets.
The weight portion that adds entry in the step (4) is preferably 37-47.
In addition; Propionic acid in the step (1)-propionic acid ammonium-two propionic acid ammonium mixtures also can make through input carbonic hydroammonium or ammonium carbonate in propionic acid; Feed intake ratio of weight and number=(3.6-6.5) of propionic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(5.5-10) of propionic acid and ammonium carbonate: 1.
Glacial acetic acid-ammonium acetate in the step (2)-two ammonium acetate mixtures also can make through input carbonic hydroammonium or ammonium carbonate in glacial acetic acid; Feed intake ratio of weight and number=(3.1-5.6) of glacial acetic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(4.6-8.5) of glacial acetic acid and ammonium carbonate: 1.
Preferably, the carrier that adopts among the preparation method of composite mildew inhibitor of the present invention is one or more in activation silicon dioxide powder, fine perlite, zeolite powder, the water.More preferably, the carrier that the present invention adopts is activation silica (commercially available), requires absorption value>=2.5, moisture≤8%, pH value≤7; Fine perlite (commercially available), granularity>=40 orders; Zeolite powder (commercially available), pH value≤7.
Can take by weighing 20-40 weight portion activation silica or fine perlite in the step (4); Spray into the said mixed liquor of step (3) under stirring; Add powder thin 2-10 weight portion benzoic acid, 1-3 weight portion dehydroacetic acid or sorbic acid and 11-35 weight portion zeolite powder again after inhaling year completion, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.Dehydroacetic acid that will add in the step (4) or sorbierite also can add in step (3).Wherein, the weight portion of activation silica or fine perlite is preferably 20-28.
In the preparation process of propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and glacial acetic acid-ammonium acetate-two ammonium acetate mixtures; The control extent of reaction is to realize through detecting in the middle of (conventional acid alkali titration) in amalgam free propionic acid and free acetic acid content respectively, in excessive acid environment, generates required propionic acid ammonium, two propionic acid ammonium, water and ammonium acetate, two ammonium acetate and water respectively.
Preferably, the preparation method of composite mildew inhibitor of the present invention further adds 1-3 weight portion ethoxyquinoline oil and 2-3 weight portion propane diols in step (4), and wherein, ethoxyquinoline is crude oil or pulvis (commercially available), ethoxyquinoline content >=95.0%.Prevention causes the approach that goes mouldy because of the oxidation factor, plays antioxidation; Propane diols (commercially available) is beneficial to liquid as wetting agent and in feed, mixes.
Through the mould inhibitor that the method for the invention makes, merit has restrained the defective and the deficiency of existing mould inhibitor: the volatilization of single organic acid is fast, be added in the feed after particularly in feed granulating or the puffing process loss cause sooner losing efficacy at once; The conversion ratio that acylate such as calcium propionate, calcium acetate, sodium propionate, sodium acetate etc. are converted into the corresponding directly acid of a mildew-proof function is low, attacks heterodyne, and cost is high; Organic acid that simple physical process is composite and salt can not fine inhibition volatility with solve efficient conversion ratio; Natural and Chinese herbal medicine mould inhibitor does not more reach the needs of feed industry mildew-resistant, excellent its at plum rain season, simultaneously cost is expensive, is difficult to practicality.The present invention adopts product component amalgam in the controlled down chemical synthesis, efficiently solves above several types of drawbacks and deficiency, and it is fast better to have solved sour volatilization, the difficult problem that the salt conversion ratio is low." propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures " (molecular formula: CH
3-CH
2-COOH, CH
3-CH
2-COONH
4, CH
3CH
2COONH
4-CH
3CH
2COOHX H
2O) reached inherent a kind of dynamic equilibrium, need be by the propionic acid of mildew-resistant to the dissociate release of its direction.Its principle of dissociating, the mode of action are:
In water, dissociate:
Dissociating in feed with different in water; Further dissociate in the feed about extremely low relative moisture, pH=6, form the dissociative type propionic acid molecule of passivation and freely, the non-dissociative type propionic acid molecule of free state promptly discharges the effective ingredient that directly acts on mildew-resistant (what really bring into play mildew-proof function is non-dissociative type monomer propionic acid molecule rather than propionate, and the monomer propionic acid has the carboxyl of mycostatic nature; The dimer propionic acid does not have free carboxy; Must discharge monomeric form mildew-proof function is just arranged), contain the propionate ion in the propionate, there is not free carboxy; Do not have the mould effect of killing; But under the acid condition that moisture and low pH value are arranged, the propionate ion can change into free carboxy, finally plays bacteriostasis with the monomer molecule form.
Sufficient acid group (COOH) contact cells of microorganisms wall oozes out the content-cytoplasm of neutrality (pH=7) under the COOHR effect, microbial growth, propagation are affected, and COOH is degraded to the form of dissociating simultaneously---COO
-, promptly propionate is stocked with the form formation dissociative type of ammonium salt.Because COOH/COO in the feed
-Ratio determine that by pH the constant relatively pH value of feed makes dissociative type transform to non-dissociative type, to keep the two proportions constant.Feedstuff mildew is a process, and the COOH of excessive concentrations can only increase volatilization, promptly causes unnecessary loss, again can not be in the mildew-resistant of the intermediary and later stages of feed storage process.This dynamic equilibrium of propionic acid and salt system thereof has fully overcome the drawback that propionic acid volatilizees, and " propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures " the mildew-resistant initial stage has the monomer COOH of capacity to supply with, and the COOH that the intermediary and later stages consume stocks COO by dissociative type
-Again constantly with the need amount continue to transform to non-dissociative type, transform the most thoroughly (conversion ratio of the propionate of other Na, Ca is extremely low, and it is not high to tire), and avoided with feed in cation (like Ca
2+, Mg
2+, Na
+Deng) formation salt.
" glacial acetic acid-ammonium acetate-two ammonium acetate mixtures " (molecular formula: CH
3COOH, CH
3COONH
4, CH
3COONH
4-CH
3COOHX H
2O) mode of its principle and effect also together, has more been widened the inhibition to the corruptibility bacterium.Wider through composite antimicrobial spectrum again.
Two propionic acid ammoniums are that propionic acid ammonium and ammonium acetate combine through intermolecular very weak power with propionic acid and acetic acid respectively in the environment of polyacid with two ammonium acetates, and the bag that is beneficial to acid covers and discharges.Moisture provides the guarantee that the ammonium salt height is converted into acid in the amalgam, the height of moisture in the feed, and the conversion that impels the required monomer acids of mildew-resistant that is directly proportional is supplied with.
The present invention compared with prior art has the following advantages: acidifying and anti-mildew fresh-keeping double effects Synergistic, and the acidifying science, antibacterial power is strong, lasting, wide spectrum, and good stability, smell, excitant are little, and corrosivity is little, and good palatability is safe; Easy to use, through tagging and fumigation action, surface electrostatic power reduces, and good fluidity does not have influence to premixing feedstuffs such as mineral matter, trace element, microorganism formulations.And preparation method's raw material provided by the invention is easy to get, and technology is smart new, does not have any discharging, and residual, production cost is low, and cost performance is high.
The specific embodiment
Describe in the face of preferred implementation of the present invention down.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also do some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.Below umber described in each embodiment all refer to weight portion.
Embodiment one: the preparation method of composite mildew inhibitor solid powder, and step is following:
(1) with liquefied ammonia through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of propionic acid; And, open water quench simultaneously with 60-80r/ minute speed stirring reaction, make that exothermic temperature is no more than 100-110 ℃ in the still; Sampling detects the propionic acid weight content that dissociates in (conventional acid alkali titration) agitated reactor and drops at about 80% o'clock that accounts for whole liquid; Stop to feed ammonia, continue to stir 2-3 minute, the cooling blanking promptly gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2) with liquefied ammonia through 45-50 ℃ of ammonia preheater preheating, pressure control 1-1.5Mpa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of glacial acetic acid; And, open water quench simultaneously with 60-80r/ minute speed stirring reaction, make that exothermic temperature is no more than 100-110 ℃ in the still; Sampling detects the acetic acid weight content that dissociates in (conventional acid alkali titration) agitated reactor and drops at about 80% o'clock that accounts for whole liquid; Stop to feed ammonia, continue to stir 2-3 minute, the cooling blanking promptly gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) taking by weighing (1) the 50 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that make and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures that (2) make respectively drops in the liquid mixer and fully mixes; And
(4) take by weighing 28 weight portion activation silica in mixer; Stir the mixed liquor that sprays into (3) down, after suction is carried and accomplished, take by weighing 5 thin weight portion benzoic acid of powder, 1 weight portion dehydroacetic acid and 11 weight portion zeolite powders more respectively and add; Sieve after stirring; Check, packing promptly gets the composite mildew inhibitor solid powder.
Embodiment two
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1), (2) and (4) are with embodiment one, and the difference of step (3) only is to take by weighing 45 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 10 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures.
Embodiment three
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) are with embodiment one; The difference of step (3) only is to take by weighing 40 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is to take by weighing 24 weight portion activation silica in mixer, stirs the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing 4 thin weight portion benzoic acid of powder, 1 weight portion sorbic acid and 26 weight portion zeolite powders more respectively and add, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment four
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) same embodiment (); The difference of step (3) only is to take by weighing 35 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 8 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is: take by weighing 24 weight portion activation silica in mixer, stir the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing 6 thin weight portion benzoic acid of powder, 1 weight portion sorbic acid and 26 weight portion zeolite powders more respectively and add, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment five
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) same embodiment (); The difference of step (3) only is to take by weighing 30 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 8 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is: take by weighing 22 weight portion activation silica in mixer, stir the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing 6 thin weight portion benzoic acid of powder, 1 weight portion sorbic acid and 33 weight portion zeolite powders more respectively and add, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment six
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) same embodiment (); The difference of step (3) only is to take by weighing 25 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 10 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is: take by weighing 20 weight portion perlites in mixer, stir the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing adding powder thin 8 weight portion benzoic acid, 2 weight portion sorbic acids and 35 weight portion zeolite powders more respectively and add, sieve check after stirring; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment seven
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) same embodiment (); The difference of step (3) only is to take by weighing 20 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 12 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is: take by weighing 20 weight portion perlites in mixer, stir the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing 10 thin weight portion benzoic acid of powder, 3 weight portion dehydroacetic acids and 35 weight portion zeolite powders more respectively and add, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment eight
The preparation method of composite mildew inhibitor solid powder, step is following:
(1) with liquefied ammonia through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of propionic acid, and, open water quench simultaneously with 60-80r/ minute speed stirring reaction; Make the interior exothermic temperature of still be no more than 100-110 ℃; Sampling detects the propionic acid weight content that dissociates in (conventional acid alkali titration) agitated reactor and drops at about 65% o'clock that accounts for whole liquid, stops to feed ammonia, continues to stir 2-3 minute; Be cooled to 40-45 ℃, blanking promptly gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2) with liquefied ammonia through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of glacial acetic acid, and, open water quench simultaneously with 60-80r/ minute speed stirring reaction; Make the interior exothermic temperature of still be no more than 100-110 ℃; Sampling detects the acetic acid weight content that dissociates in (conventional acid alkali titration) agitated reactor and drops at about 70% o'clock that accounts for whole liquid, stops to feed ammonia, continues to stir 2-3 minute; Be cooled to 40-45 ℃, blanking promptly gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) taking by weighing (1) the 50 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that make and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures that (2) make respectively drops in the liquid mixer and fully mixes; And
(4) the carrier activation silica that takes by weighing 28 weight portions is in mixer; Stir the mixed liquor that sprays into (3) down, after suction was carried and accomplished, the benzoic acid, 1 weight portion dehydroacetic acid and the 11 weight portion carrier zeolite powders that take by weighing 5 thin weight portions of powder more respectively added; Sieve after stirring; Check, packing promptly gets the anti-removing mildew of solid.
Embodiment nine
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1), (2) and (4) same embodiment (eight), the difference of step (3) only is to take by weighing 45 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 10 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures.
Embodiment ten
The preparation method of composite mildew inhibitor solid powder, step is following:
Step (1) and (2) same embodiment (eight); The difference of step (3) only is to take by weighing 40 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures, and the difference of step (4) is: take by weighing 24 weight portion activation silica in mixer, stir the mixed liquor that sprays into (3) down; After inhaling year completion; Take by weighing 4 thin weight portion benzoic acid of powder, 2 weight portion sorbic acids and 25 weight portion zeolite powders more respectively and add, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
Embodiment 11
The preparation method of composite mildew inhibitor liquid preparation, step is following:
(1) with liquefied ammonia through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5MPa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of propionic acid; And, open water quench simultaneously with 60-80r/ minute speed stirring reaction, make that exothermic temperature is no more than 100-110 ℃ in the still; Sampling detects when free propionic acid weight percentage drops to the 65%-80% that accounts for whole liquid in (conventional acid alkali titration) agitated reactor; Stop to feed ammonia, continue to stir 2-3 minute, the cooling blanking promptly gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2) with liquefied ammonia through 40-45 ℃ of ammonia preheater preheating, pressure control 1-1.5Mpa is again after disperser disperses; Evenly slowly feed and be added with in the agitated reactor of an amount of glacial acetic acid; And, open water quench simultaneously with 60-80r/ minute speed stirring reaction, make that exothermic temperature is no more than 100-110 ℃ in the still; Sampling detects when free acetic acid weight percentage drops to the 70%-80% that accounts for whole liquid in (conventional acid alkali titration) agitated reactor; Stop to feed ammonia, continue to stir 2-3 minute, the cooling blanking promptly gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) taking by weighing (1) the 50 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that make and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures that (2) make respectively drops in the liquid mixer and mixes; And
(4) take by weighing 3 thin weight portion benzoic acid of powder, 1 weight portion dehydroacetic acid, 1 weight portion ethoxyquinoline oil and 2 weight portion propane diols respectively; Put in (3) and stir; Pulvis to adding dissolves fully; The water that adds 37 weight portions again stirs, and takes out filtration, check, can, promptly gets the composite mildew inhibitor liquid preparation.
Embodiment 12
The preparation method of composite mildew inhibitor liquid preparation, step is following:
Step (1) and (2) same embodiment (11); The difference of step (3) only is to take by weighing 45 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 10 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures; The difference of step (4) is: take by weighing 3 thin weight portion benzoic acid of powder, 1 weight portion sorbic acid, 1 weight portion ethoxyquinoline oil and 2 weight portion propane diols respectively; Put in (3) and stir, the pulvis that extremely adds dissolves fully, and the water that adds 38 weight portions again stirs; Take out filtration, check, can, promptly get the composite mildew inhibitor liquid preparation.
Embodiment 13
The preparation method of composite mildew inhibitor liquid preparation, step is following:
Step (1) and (2) same embodiment (11); The difference of step (3) only is to take by weighing 40 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures; The difference of step (4) is: take by weighing 3 thin weight portion benzoic acid of powder, 2 weight portion sorbic acids, 2 weight portion ethoxyquinolines oil and 3 weight portion propane diols respectively; Put in (3) and stir, the pulvis that extremely adds dissolves fully, and the water that adds 45 weight portions again stirs; Take out filtration, check, can, promptly get the composite mildew inhibitor liquid preparation.
Embodiment 14
The preparation method of composite mildew inhibitor liquid preparation, step is following:
Step (1) and (2) same embodiment (11); The difference of step (3) only is to take by weighing 35 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 8 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures; The difference of step (4) is: take by weighing 2 thin weight portion benzoic acid of powder, 2 weight portion sorbic acids, 3 weight portion ethoxyquinolines oil and 3 weight portion propane diols respectively; Put in (3) and stir, the pulvis that extremely adds dissolves fully, and the water that adds 47 weight portions again stirs; Take out filtration, check, can, promptly get the composite mildew inhibitor liquid preparation.
Embodiment 15
The preparation method of composite mildew inhibitor liquid preparation, step is following:
Step (1) and (2) same embodiment (11); The difference of step (3) only is to take by weighing 30 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 15 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures; The difference of step (4) is: take by weighing 2 thin weight portion benzoic acid of powder, 2 weight portion sorbic acids, 1 weight portion ethoxyquinoline oil and 3 weight portion propane diols respectively; Put in (3) and stir, the pulvis that extremely adds dissolves fully, and the water that adds 55 weight portions again stirs; Take out filtration, check, can, promptly get the composite mildew inhibitor liquid preparation.
Embodiment 16: the preparation method of composite mildew inhibitor solid powder, and step is following:
(1) in propionic acid, drop into carbonic hydroammonium or ammonium carbonate, feed intake ratio of weight and number=5.5: 1 of feed intake ratio of weight and number=3.6: 1 of propionic acid and carbonic hydroammonium, propionic acid and ammonium carbonate must propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2) in glacial acetic acid, drop into carbonic hydroammonium or ammonium carbonate, feed intake ratio of weight and number=4.6: 1 of feed intake ratio of weight and number=3.1: 1 of glacial acetic acid and carbonic hydroammonium, glacial acetic acid and ammonium carbonate must glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) taking by weighing (1) the 40 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that make and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures that (2) make respectively drops in the liquid mixer and fully mixes; And
(4) take by weighing 24 weight portion activation silica in mixer; Stir the mixed liquor that sprays into (3) down, after suction is carried and accomplished, take by weighing 4 thin weight portion benzoic acid of powder, 1 weight portion dehydroacetic acid and 26 weight portion zeolite powders more respectively and add; Sieve after stirring; Check, packing promptly gets the composite mildew inhibitor solid powder.
Embodiment 17: the preparation method of composite mildew inhibitor solid powder, and step is following:
(1) in propionic acid, drop into carbonic hydroammonium or ammonium carbonate, feed intake ratio of weight and number=10: 1 of feed intake ratio of weight and number=6.5: 1 of propionic acid and carbonic hydroammonium, propionic acid and ammonium carbonate must propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2) in glacial acetic acid, drop into carbonic hydroammonium or ammonium carbonate, feed intake ratio of weight and number=8.5: 1 of feed intake ratio of weight and number=5.6: 1 of glacial acetic acid and carbonic hydroammonium, glacial acetic acid and ammonium carbonate must glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) taking by weighing (1) the 40 weight portions propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures that make and 5 weight portion glacial acetic acid-ammonium acetates-two ammonium acetate mixtures that (2) make respectively drops in the liquid mixer and fully mixes; And
(4) take by weighing 24 weight portion activation silica in mixer; Stirring sprays into the mixed liquor of (3) down, after suction is carried and accomplished, takes by weighing adding powder thin 4 weight portion benzoic acid, 1 weight portion dehydroacetic acid and 26 weight portion zeolite powders more respectively and adds; Sieve after stirring; Check, packing promptly gets the composite mildew inhibitor solid powder.
Test Example one: mould inhibitor according to the invention and other type mildew-resistant anti-mold effect contrast test
Test material and method
1.1 test material
1.1.1 feed is used in test: baby pig feedstuff moisture 13.81% (Rui Kang feed corporation,Ltd in Guigang provides)
Feed ingredient is used in table 1 test
| Corn | Barley | Mai Fupi | Rape cake | Continuous seedcake | Oyster shell whiting | Salt | Add up to |
| 37.0 | 34.5 | 9.0 | 8.0 | 10.0 | 1.0 | 0.5 | 100 |
1.1.2 mould inhibitor is used in test
Table 2 test is with mould inhibitor recipe ingredient and percentage by weight
| Mould inhibitor | Recipe ingredient and part by weight (%) |
| The A group | The embodiment of the invention 3 |
| The B group | Propionic acid 50, active silica 25, zeolite powder 25 |
| The C group | Propionic acid 25, glacial acetic acid 25, active silica 25, zeolite powder 25 |
| The D group | Sodium acetate 15, calcium propionate 20, Sodium Benzoate 15, active silica 10, zeolite powder 40 |
| The E group | Citrus peel meal 20, northern fresh hide powder 20, fennel powder 20, ginger powder 20, ground cinnamon 20 |
| The F group | Natamycin 10, propionic acid 10, calcium propionate 20, sorbic acid 3, ground cinnamon 22, silica 8, zeolite powder 27 |
1.2 test method
1.2.1 test is divided into groups and design
Six groups and one control group of this experiment branch is totally seven groups,
Every group with above-mentioned pig starter feed 5000 grams; Adding mould inhibitor dosage is 0.12% (be every group and add 600 milligrams of above-mentioned test mould inhibitors) of feed weight, fully mixes, and prevents the cross-infection of different tests group; Not add mould inhibitor is control group; Be respectively charged in the clear PE bag and seal, place 30-35 ℃, leave standstill under the environmental condition of relative humidity about 75% (in case move seethe feed flow and be difficult for observing or observed result has error); Observe once record caking and mouldy time weekly.
2. logging is seen table 3
Table 3 logging
The level determinations of going mouldy is according to seeing table 4
Go mouldy level determinations result and according to explanation of table 4
3. result and discussion
Draw by above-mentioned result of the test, the pig starter feed that tries in moisture 13.81%, temperature is 30-35 ℃; Relative humidity is to store under 75% left and right sides environmental condition, and the mould inhibitor group that is added with 0.12% dosage is obviously mouldy than the control group delay, in several types of mould inhibitors of above-mentioned test; The poorest is natural plant kind, gathers mould and lumps in 21 days, secondly organic acid salt; Began caking and mouldy in 35 days, be furnished with 42 days cakings that gather mould of F group of organic acid, acylate and other components, composite B, the C of single organic acid and organic acid two groups of time omits length but does not also have 56 mouldy; But lump ahead of time, the speed of going mouldy is fast.The composite mildew inhibitor with acidifying and anti-mildew fresh-keeping double effects of A of the present invention group embodiment 3 preparations can make under equal conditions fresh-keeping 91 (the beginning caking) of feed storage more than the sky, gathered mould in 98 days, and the speed of going mouldy be slower.
Experimental example two
Composite mildew inhibitor with acidifying and anti-mildew fresh-keeping double effects according to the invention and citric acid, the phosphoric acid acidizing effect contrast test of feeding.
1. test material and method
1.1 test material
1.1.1 acidulant is used in test
A group: the embodiment of the invention 11;
B group: citric acid (trade Co., Ltd falls in the Guangzhou he to be provided);
C group: phosphoric acid (brilliance Industrial Co., Ltd. in Shenzhen provides);
1.2 test method
1.2.1 the test piglet is selected and divide into groups (experiment of Guigang Rui Kang feed corporation,Ltd)
It is close to choose term, and parity is identical, 240 of the long piglets of the wean that body weight is close; Be divided at random four greatly the group, a control group and three test group, every group establish again three parallel; Each parallel 20, the embodiment of the invention 11 of test group A group adds 0.2%, and test B group is added 1% citric acid; Test C group is added 0.5% phosphoric acid, and test group D group is contrast.Basal diet is:
Basal diet is formed and nutritional labeling is seen table 5
Table 5 basal diet is formed and nutritional labeling
| Raw material | Basal diet | The basal diet trophic level | Basal diet |
| Corn | 62 | Digestible energy | 13.45 |
| The wheat husband | 6 | Crude protein | 18.50 |
| Dregs of beans | 24 | Calcium | 0.93 |
| Fish meal | 4 | Available phosphorus | 0.56 |
| Premix | 4 | Lysine | 0.92 |
| Add up to | 100 | Egg+cystine | 0.45 |
1.2.2 feeding and management and record
Begin food calling age in piglet one week, 4 wean in ages in week, 8 week off-tests in age, free choice feeding, drinking-water, by conventional vaccine inoculation, every day record: search for food and disease condition, daily gain is calculated daily gain, the price of deed, diarrhea rate, the death rate.
The test data sheet statistics is seen table 6
Table 6 test data sheet statistics
| Number | Average day increment | Feedstuff-meat ratio | The diarrhoea number | Death toll | |
| Embodiment 11 | 60 | 398±75 | 1.61±0.31 | 4 | 2 |
| Citric acid | 60 | 379±58 | 1.66±0.25 | 11 | 4 |
| Phosphoric acid | 60 | 368±64 | 1.72±0.29 | 16 | 6 |
| Contrast | 60 | 354±61 | 1.74±0.27 | 38 | 9 |
3, result of the test and analysis
Draw by above-mentioned result of the test: in piglet diet, add different acidulants and compare with control group; The daily gain, the survival rate that improve piglet are all arranged; Reduce the obvious effect of feedstuff-meat ratio, reduction diarrhea rate, single acidulant citric acid and phosphoric acid effect are relatively poor, and citric acid is better than phosphoric acid; But cost is high, is best with 11 groups of the embodiment of the invention in three groups of acidulants.
This is because acidizing effect is acidulant preferably, and strong acid cushion effect in the feed can or be provided preferably; Overcome early weaning piglet when feeding and to have secreted enough hydrochloric acid in gastric juice, be difficult in the stomach keep suitable pH value and enough enzymatic activitys, caused that digestive function is disorderly; And cause weanling pig to the vegetable protein be main feed indigestion with influence microbial balance in the alimentary canal; Make unfavorable factors such as a large amount of breedings of harmful bacterium, acidizing effect well can be good at reducing intestines and stomach pH value and then has improved pepsin, the diastatic activity of trypsase; Promote digestion; Improve the digestibility of daily ration, also help the growth of lactic acid bacteria beneficial bacterium in the stomach and intestine, suppress Escherichia coli.The breeding of salmonella and shuttle shape bud bag bacillus, thus piglet is able to the health minimizing or has pressed down diarrhoea take place with dead.
Claims (8)
1. a composite mildew inhibitor is characterized in that, each composition weight umber of said composite mildew inhibitor is respectively:
Propionic acid-propionic acid ammonium-two propionic acid ammonium mixture 20-50;
Glacial acetic acid-ammonium acetate-two ammonium acetate mixture 5-15;
Benzoic acid 2-10;
Dehydroacetic acid and/or sorbic acid 1-3; And
Carrier 37-55;
Wherein, said carrier is one or more in activation silicon dioxide powder, fine perlite, zeolite powder, the water; The weight content of free propionic acid accounts for the 65%-80% of this mixture system in propionic acid-propionic acid ammonium-two propionic acid ammonium mixture systems; The weight content of free glacial acetic acid accounts for the 70%-80% of this mixture system in glacial acetic acid-ammonium acetate-two ammonium acetate mixtures.
2. composite mildew inhibitor as claimed in claim 1 is characterized in that, said composite mildew inhibitor further comprises 1-3 weight portion ethoxyquinoline and 2-3 weight portion propane diols.
3. according to claim 1 or claim 2 composite mildew inhibitor is characterized in that said composite mildew inhibitor is solid powder or liquid preparation.
4. the preparation method of a composite mildew inhibitor is characterized in that, comprises the steps:
(1), feeds and be added with in the reactor of an amount of propionic acid stirring with after the liquefied ammonia preheating; Cooling when free propionic acid weight percentage accounts for the 65%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2), feed and be added with in the reactor of an amount of glacial acetic acid stirring with after the liquefied ammonia preheating; Cooling when free acetic acid weight percentage accounts for the 70%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) take by weighing 20-50 weight portion propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5-15 weight portion glacial acetic acid-ammonium acetate-two ammonium acetate mixtures, mix;
(4) take by weighing 2-10 weight portion benzoic acid, 1-3 weight portion dehydroacetic acid or sorbic acid, 1-3 weight portion ethoxyquinoline oil and 2-3 weight portion propane diols; Put in the said mixture of step (3), stir, the water that adds the 37-55 weight portion again stirs; Filter; Check, can promptly gets the composite mildew inhibitor liquid preparation.
5. preparation method as claimed in claim 4; It is characterized in that; Propionic acid in the said step (1)-propionic acid ammonium-two propionic acid ammonium mixtures are in propionic acid, to drop into carbonic hydroammonium or ammonium carbonate prepares; Feed intake ratio of weight and number=(3.6-6.5) of propionic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(5.5-10) of propionic acid and ammonium carbonate: 1.
6. preparation method as claimed in claim 4; It is characterized in that; Glacial acetic acid-ammonium acetate in the said step (2)-two ammonium acetate mixtures are in glacial acetic acid, to drop into carbonic hydroammonium or ammonium carbonate prepares; Feed intake ratio of weight and number=(3.1-5.6) of glacial acetic acid and carbonic hydroammonium: 1, feed intake ratio of weight and number=(4.6-8.5) of glacial acetic acid and ammonium carbonate: 1.
7. preparation method as claimed in claim 4 is characterized in that, in said step (1), (2), controls the extent of reaction through free propionic acid and free acetic acid content in the acid-base titration detection mixture.
8. the preparation method of a composite mildew inhibitor is characterized in that, comprises the steps:
(1), feeds and be added with in the reactor of an amount of propionic acid stirring with after the liquefied ammonia preheating; Cooling when free propionic acid weight percentage accounts for the 65%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures;
(2), feed and be added with in the reactor of an amount of glacial acetic acid stirring with after the liquefied ammonia preheating; Cooling when free acetic acid weight percentage accounts for the 70%-80% of whole liquid in the reactor, stops to feed ammonia; Continue to stir, the cooling blanking gets glacial acetic acid-ammonium acetate-two ammonium acetate mixtures;
(3) take by weighing 20-50 weight portion propionic acid-propionic acid ammonium-two propionic acid ammonium mixtures and 5-15 weight portion glacial acetic acid-ammonium acetate-two ammonium acetate mixtures, mix;
(4) take by weighing 20-28 weight portion activation silica or fine perlite; Spray into the said mixed liquor of step (3) under stirring; Add powder thin 2-10 weight portion benzoic acid, 1-3 weight portion dehydroacetic acid or sorbic acid and 11-35 weight portion zeolite powder again after inhaling year completion, sieve after stirring, check; Packing promptly gets the composite mildew inhibitor solid powder.
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| CN103181452A (en) * | 2011-12-27 | 2013-07-03 | 北京资源亚太动物药品有限公司 | Feed mildew inhibitor and preparation method |
| CN103168974B (en) * | 2013-03-25 | 2014-06-11 | 重庆民泰香料化工有限责任公司 | Liquid mildewproof agent for feed and method for avoiding mildew of feed |
| CN104686796A (en) * | 2014-08-11 | 2015-06-10 | 武汉新农翔饲料有限公司 | Composite liquid acidification and mildew resistance agent and preparation method thereof |
| CN105285352A (en) * | 2015-11-10 | 2016-02-03 | 浏阳乐佰有机营养有限公司 | Specific-effect mildewproof agent and making method thereof |
| CN106699544B (en) * | 2015-11-12 | 2019-11-08 | 鲁昊 | A kind of preparation method of propionic acid ammonium crystal and its pulvis |
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| CN106962655A (en) * | 2017-05-17 | 2017-07-21 | 上海邦成生物工程有限公司 | It is a kind of that there is composite mildew inhibitor of acidizing effect and its preparation method and application to feed |
| CN107279675A (en) * | 2017-07-13 | 2017-10-24 | 上海邦成生物工程有限公司 | It is a kind of for mould inhibitor of expanded pellet diet and preparation method thereof |
| CN109619366A (en) * | 2018-12-29 | 2019-04-16 | 上海邦成生物工程有限公司 | A kind of efficient feed mildew inhibitor and preparation method thereof |
| CN110524658A (en) * | 2019-09-10 | 2019-12-03 | 兰州大学 | A kind of compound hay mould inhibitor and its preparation method and application |
| CN112106917A (en) * | 2020-09-25 | 2020-12-22 | 重庆民泰新农业科技发展集团有限公司 | Feed slow-release mildew inhibitor and using method thereof |
| CN114504058A (en) * | 2022-03-01 | 2022-05-17 | 吉林省农业科学院 | Efficient composite mildew inhibitor for feed and preparation method thereof |
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