CN111802518A - Formic acid type acidifier for feed, and preparation method and application method thereof - Google Patents
Formic acid type acidifier for feed, and preparation method and application method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/105—Aliphatic or alicyclic compounds
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
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Abstract
The invention provides a formic acid type acidifier for feed, which is divided into a liquid type acidifier and a powder type acidifier, wherein the liquid type acidifier comprises the following components in parts by weight: 10-50 parts of formic acid, 10-50 parts of ammonium formate and 0-80 parts of water; the powder-type acidifier comprises 10-50 parts of formic acid, 10-50 parts of ammonium formate, 0-80 parts of water and a carrier. The invention also provides a preparation method and a using method of the formic acid type acidifier. The formic acid in the acidulant provided by the invention has low volatility and good palatability.
Description
Technical Field
The invention belongs to the technical field of feed additives, and particularly relates to a formic acid type acidifier for feed, and a preparation method and a use method thereof.
Background
With the introduction of growth-promoting antibiotics in feed, animal health is reduced, such as increased incidence of diarrhea and mortality (especially in young animals), and there is a need for alternative antibiotic products that act like antibiotics, but reduce the incidence of diarrhea and mortality in animals.
There are many products on the market today, such as plant extracts, enzyme preparations, acidifying agents, probiotics, antimicrobial peptides, etc., where the acidifying agent acts to: inhibiting and killing harmful bacteria in gastrointestinal tract, promoting growth and reproduction of beneficial bacteria, reducing diarrhea incidence, lowering gastrointestinal pH, activating digestive enzymes such as pepsin, reducing intestinal microorganism metabolites (such as ammonia gas, polyamine substances or volatile fatty acid), and improving internal environment of digestive tract.
The influence of the prior acidifying agent on the palatability of the feed is not taken into consideration, but the smell of the animal is very sensitive in nature, if the acidifying agent has strong volatility and the palatability of the feed is poor, the appetite of the animal is reduced, the feed intake is reduced, the growth of the animal is influenced, and the health of the animal is influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a formic acid type acidifier for feed, which has low volatility and good palatability, and a preparation method and a use method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the formic acid type acidifier for the feed comprises a liquid acidifier, and the liquid acidifier comprises the following components in parts by weight: 10-50 parts of formic acid, 10-50 parts of ammonium formate and 0-80 parts of water.
The formic acid type acidifier for the feed comprises a powder type acidifier, wherein the powder type acidifier comprises the following components in parts by weight: 10-50 parts of formic acid, 10-50 parts of ammonium formate, 0-80 parts of water and a carrier, wherein the formic acid, the ammonium formate and the water form a liquid acidifier, and the weight part ratio of the liquid acidifier to the carrier is 1: 0.3-5.
The invention also provides a preparation method of the formic acid type acidifier for the feed, which comprises the following steps:
s1, putting 17.8-86.5 parts of formic acid and 0-80 parts of water into a reaction kettle, starting stirring, introducing liquid ammonia into the reaction kettle, adding the liquid ammonia into the reaction kettle, simultaneously opening cooling water for cooling, and controlling the temperature in the reaction kettle to be below 70 ℃ to obtain a mixture of formic acid, ammonium formate and water;
and S2, cooling by using cooling water after liquid ammonia is added, sampling and detecting the molar ratio of formic acid to ammonium formate, wherein if the molar ratio of formic acid to ammonium formate in the mixture of formic acid, ammonium formate and water is 1:0.5-1.5, the obtained mixture of formic acid, ammonium formate and water is a liquid acidifier, otherwise, liquid ammonia needs to be added into the reaction kettle.
The invention also provides a preparation method of the formic acid type acidifier for the other feeds, which comprises the following steps:
s1, adding 17.8-86.5 parts of water and 0-80 parts of water into a reaction kettle, starting stirring, introducing liquid ammonia into the reaction kettle, adding the liquid ammonia into the reaction kettle, simultaneously opening cooling water for cooling, and controlling the temperature in the reaction kettle to be below 70 ℃ to obtain a mixture of formic acid, ammonium formate and water;
s2, cooling by using cooling water after liquid ammonia is added, sampling and detecting the molar ratio of formic acid to ammonium formate, if the molar ratio of formic acid to ammonium formate in the mixture of formic acid, ammonium formate and water is 1:0.5-1.5, obtaining a mixture of formic acid, ammonium formate and water as a liquid acidifier, otherwise, continuously adding liquid ammonia into the reaction kettle;
s3, after the detection is qualified, mixing the liquid acidulant obtained in the step S2 with a carrier, and grinding to obtain a powder acidulant; the weight portion ratio of the liquid acidifier to the carrier is 1: 0.3-5.
The invention also provides a using method of the formic acid type acidifier for the feed, and the addition amount of the acidifier in the feed is 2-6 kg/t.
The principle and the beneficial effects of the technical scheme are as follows:
(1) the "component" in the "component including the following components in parts by weight" referred to in the present technical scheme means an ingredient contained in the acidulant.
(2) Formic acid in the technical scheme is a main provider of acid, ammonium formate is a formic acid slow-release agent, the ammonium formate can reduce the volatility of the formic acid, the palatability of the acidifying agent is improved, the acidifying agent enters the gastrointestinal tract of an animal to slowly release the formic acid, pathogenic microorganisms are killed, a barrier protection effect is achieved, intestinal microorganisms are regulated, the growth and the reproduction of beneficial bacteria are promoted, digestion and absorption are promoted, the resistance of the animal is enhanced, the diarrhea incidence and the death rate of the animal are reduced, and the risk of animal infection diseases is reduced.
(3) When the powdery acidulant is prepared, the powdery acidulant can be directly obtained by purchasing formic acid, ammonium formate and a carrier, but during preparation, the formic acid and the ammonium formate need to be dissolved and then mixed and ground with the carrier, and the process is relatively complex.
The technical scheme has high industrialization degree, and the whole preparation method is simple and is suitable for large-scale production.
(4) The technical scheme mainly comprises the following main reasons that the weight parts of components (10-50 parts of formic acid, 10-50 parts of ammonium formate and 0-80 parts of water) are controlled, the molar ratio of the formic acid to the ammonium formate in a mixture of the formic acid, the ammonium formate and the water is controlled to be 1:0.5-1.5, and the weight part ratio of a liquid acidifier to a carrier is controlled to be 1: 0.3-5: only when the value is taken within the corresponding range, the technical scheme can ensure the sterilization effect of the acidifier, ensure the palatability of the acidifier and improve the cost performance of the whole acidifier.
Preferably, the molar ratio of formic acid to ammonium formate is from 1:0.5 to 1.5. The acidifier obtained by the technical scheme has good bactericidal effect and palatability, can regulate intestinal microorganisms, promote the growth and reproduction of beneficial bacteria, promote digestion and absorption, and effectively reduce the diarrhea incidence and death rate of animals.
Preferably, the ammonium formate is obtained by purchasing or synthesizing by reacting formic acid with ammonia, wherein the ammonia is one or a mixture of more than two of ammonium carbonate, ammonium bicarbonate, ammonia water and liquid ammonia, and the ammonium formate is preferably synthesized by reacting formic acid with liquid ammonia. The acidifier obtained by the technical scheme has good bactericidal effect and palatability, can regulate intestinal microorganisms, promote the growth and reproduction of beneficial bacteria, promote digestion and absorption, and effectively reduce the diarrhea incidence and death rate of animals.
Preferably, the carrier is one or a mixture of more than two of silicon dioxide, sodium sulfate, zeolite powder, montmorillonite, sepiolite, bentonite and medical stone. The acidifier obtained by the technical scheme has good bactericidal effect and palatability, can regulate intestinal microorganisms, promote the growth and reproduction of beneficial bacteria, promote digestion and absorption, and effectively reduce the diarrhea incidence and death rate of animals.
Detailed Description
Formic acid used in the following examples was purchased from Shandong chat Luxi chemical group, Inc. or Chongqing Chundong chemical (group), Inc.; liquid ammonia was purchased from Guangan Jiu resource chemical Co., Ltd.
Example 1a
The invention provides a formic acid type acidifier for feed, which is liquid and specifically comprises the following components in parts by weight: 30 parts of formic acid, 30 parts of ammonium formate and 9.1 parts of water.
The carrier used in this embodiment may be one or a mixture of two or more of silica, sodium sulfate, zeolite powder, montmorillonite, sepiolite, bentonite and medical stone, and the preferred carrier in this embodiment is silica.
The embodiment also discloses a preparation method of the formic acid type acidifier for the liquid feed, which specifically comprises the following steps:
s1, putting 51.9 parts of formic acid and 9.1 parts of water, or directly putting 61 parts of 85% formic acid into a reaction kettle (water is added into a reaction system to prevent ammonium formate from being separated out), starting stirring, slowly introducing a plurality of liquid ammonia into the reaction kettle (the molar ratio of formic acid to ammonium formate in the reaction kettle is detected while adding the liquid ammonia to prevent the liquid ammonia from being excessive), adding the liquid ammonia into the reaction kettle, simultaneously opening cooling water to cool (because the reaction of formic acid and liquid ammonia is an exothermic reaction, the volatilization of formic acid and the incomplete reaction of ammonia are avoided, the temperature needs to be lowered in the reaction process, the cooling water continuously lowers the temperature of the reaction kettle in the reaction process), and controlling the temperature in the reaction kettle below 70 ℃ to obtain a mixture of formic acid, ammonium formate mixture and water.
S2, cooling by using cooling water after liquid ammonia is added, sampling and detecting the contents of formic acid and ammonium formate, wherein the obtained formic acid and ammonium formate mixture is a liquid acidifier with the components of 30 parts of formic acid, 30 parts of ammonium formate and 9.1 parts of water, otherwise, liquid ammonia needs to be added into the reaction kettle continuously.
The embodiment also discloses a using method of the formic acid type acidifier for the feed, and when the formic acid type acidifier is used, the addition amount of the formic acid type acidifier for the feed is 2-6kg per ton.
Example 1b
Compared with the embodiment 1a, the acidifying agent provided in the embodiment 1b is powder, and specifically comprises the following components in parts by weight: 30 parts of formic acid, 30 parts of ammonium formate, 9.1 parts of water and 30.9 parts of a carrier, wherein a mixture of 30 parts of formic acid, 30 parts of ammonium formate and 9.1 parts of water is a liquid acidifier.
The embodiment also discloses a preparation method of the powder-type acidulant, which specifically comprises the following steps:
s1, putting 51.9 parts of formic acid and 9.1 parts of water into a reaction kettle, starting stirring, slowly introducing a plurality of liquid ammonia into the reaction kettle, adding the liquid ammonia into the reaction kettle, simultaneously opening cooling water to cool, and controlling the temperature in the reaction kettle to be below 70 ℃ to obtain a mixture of formic acid, ammonium formate and water.
And S2, after the liquid ammonia is added, cooling by using cooling water, sampling to detect the contents of formic acid and ammonium formate, wherein the obtained mixture of formic acid, ammonium formate and water is a liquid acidifier containing 30 parts of formic acid, 30 parts of ammonium formate and 9.1 parts of water, otherwise, the liquid ammonia needs to be added into the reaction kettle continuously.
S3, mixing the liquid acidulant obtained in S2 with a carrier, and grinding the mixture to 20 mesh or less (the particle size is too large and affects the use effect of the whole acidulant), thereby obtaining a powder acidulant.
The term "polished to 20 mesh or less" in this embodiment means that the polishing can be performed to 20 mesh or less, 30 mesh or less, 40 mesh or less, and the like.
The weight ratio of the liquid acidulant to the carrier is 1:0.3-5, the carrier is preferably 30.9 parts in this embodiment, and the weight ratio of the liquid acidulant to the carrier is 1: 2.24.
The embodiment also discloses a using method of the formic acid type acidifier for the feed, and when the formic acid type acidifier is used, the addition amount of the formic acid type acidifier for the feed is 2-6kg per ton.
Comparative example 1
Comparative example 1 this comparative example 1 includes comparative example 1a and comparative example 1b, where comparative example 1a differs from example 1a only in that: the components do not contain ammonium formate, and the weight part of the formic acid component is 30 parts, and the specific comparative example 1a comprises 30 parts of formic acid and 9.1 parts of water.
Comparative example 1b differs from example 1b only in that: the components do not contain ammonium formate, and the formic acid component accounts for 30 parts by weight, specifically, comparative example 1b includes the following components in parts by weight: 30 parts of formic acid, 9.1 parts of water and 60.9 parts of carrier (the carrier does not have great influence on the using effect of the whole acidifier).
The acidulant prepared in comparative example 1a was used as a liquid formic acid control sample; the acidulant prepared in example 1a was used as a liquid type test sample.
The acidifier prepared in the comparative example 1b is used as a powder type formic acid control sample; the acidulant prepared in example 1b was used as a powder type test sample.
The whole experimental design simulates the pelletizing temperature and time of feed production, the content of free acid (counted by formic acid) in a liquid formic acid control sample, a liquid experimental sample, a powder formic acid control sample and a powder experimental sample is detected (the detection is carried out by adopting an acid-base titration method or perchloric acid non-aqueous titration method, compared with the detection by adopting gas chromatography or liquid chromatography, the detection by adopting the acid-base titration method or perchloric acid non-aqueous titration method has the advantages of high accuracy and rapid detection), concretely, the formic acid control sample and the experimental sample are placed in an open manner at 80 ℃, the content of free acid (counted by formic acid) is detected at intervals of 5 minutes and 10 minutes, 50g of the formic acid control sample and the experimental sample are respectively weighed in clean sample bottles, and each sample is 3 parts and marked.
The results of comparative example 1a, comparative example 1b, example 1a, example 1b are given in the table below.
The above experimental results show that:
the formic acid content in the liquid type formic acid control sample (comparative example 1a) was significantly decreased under the high temperature condition of 80 deg.C, whereas the formic acid content in the liquid type experimental sample (example 1a) was not significantly changed under the high temperature condition of 80 deg.C. Through statistical analysis, the volatilization loss of the liquid formic acid control sample is 30.3%, while the volatilization loss of the liquid experimental sample under the same test condition is 6.0%, and the volatilization loss of the liquid experimental sample is 20.0% of that of the liquid formic acid control sample, which indicates that the ammonium formate can effectively inhibit the volatilization of the formic acid.
The formic acid content in the powder type formic acid control sample (comparative example 1b) was significantly reduced under the high temperature condition of 80 ℃, whereas the formic acid content in the powder type experimental sample (example 1b) was not significantly changed under the high temperature condition of 80 ℃. Through statistical analysis, the volatilization loss of the powder type formic acid control sample is 29.9%, while the volatilization loss of the powder type experimental sample under the same test condition is 3.0%, and the volatilization loss of the powder type experimental sample is 9.9% of that of the powder type formic acid control sample, which indicates that the ammonium formate can effectively inhibit the volatilization of the formic acid, and particularly for the liquid type acidifying agent, the effect of the ammonium formate in inhibiting the volatilization of the formic acid is better.
Example 2 and example 3
Example 2 includes example 2a and example 2 b; this example 3 includes example 3a and example 3 b.
See table below for specific use cases of parts by weight of the components of examples 2 and 3, as well as the molar ratio of formic acid and ammonium formate, and the ratio of parts by weight of liquid-type acidulant to carrier.
Comparative examples 2 and 3
The present comparative example 2 includes comparative example 2a and comparative example 2b, and the present comparative example 3 includes comparative example 3a and comparative example 3 b.
See table below for specific use cases of parts by weight of components of comparative example 2 and comparative example 3, as well as molar ratio of formic acid and ammonium formate, and weight part ratio of liquid-type acidulant to carrier.
400 excellent yellow chickens (hens) with similar weight and age of 15 days are selected and randomly divided into 10 groups according to the test requirements, each group is provided with 4 repetitions, and each repetition comprises 10 chickens, namely a control group, an antibiotic group, a control group 2a, an experimental group 2a, a control group 2b, an experimental group 2b, a control group 3a, an experimental group 3a, a control group 3b and an experimental group 3 b.
The control group was fed a basal diet, the antibiotic group was fed a basal diet plus virginiamycin, and the control group 2a was fed a basal diet plus the formic acid type acidifying agent prepared in comparative example 2 a; experimental group 2a fed basal diet + formic acid-type acidifier made in example 2 a; comparative group 2b fed basal diet + formic acid-type acidulant prepared in comparative example 2 b; experimental group 2b fed basal diet + formic acid-type acidifier made in example 2 b; comparative group 3a was fed basal diet + formic acid-type acidifier made in comparative example 3 a; experimental group 3a fed basal diet + formic acid-type acidifier made in example 3 a; comparative group 3b fed basal diet + formic acid-type acidulant prepared in comparative example 3 b; experimental group 3b was fed a basal diet plus the formic acid-type acidulant prepared in example 3 b.
The feed is taken freely, the water is drunk freely, and the feeding test time is 30 days. And recording related data during the test period, and calculating to obtain average daily gain, average daily feed intake, feed consumption and weight gain ratio, diarrhea incidence rate and mortality rate. Fasted (free drinking) for 12h before each weighing. The experimental design of the control group, antibiotic group, control group 2a, experimental group 2a, control group 2b, experimental group 2b, control group 3a, experimental group 3a, control group 3b, experimental group 3b is specifically shown in the following table:
the experimental results of the control group, antibiotic group, control group 2a, experimental group 2a, control group 2b, experimental group 2b, control group 3a, experimental group 3a, control group 3b, experimental group 3b are shown in the following table:
note: the shoulder marks of the same row have significant difference of different letters a, b and c (p < 0.05).
As can be seen from the above table, compared with the control group, the antibiotic group, the control group 2a, the control group 2b, the control group 3a and the control group 3b, the average daily gain and the average daily food consumption of the experimental group 2a, the experimental group 2b, the experimental group 3a and the experimental group 3b are higher, wherein the average daily food consumption of the experimental group 2a, the experimental group 2b, the experimental group 3a and the experimental group 3b is significantly higher than those of the control group and the antibiotic group, which indicates that the acidifying agent composed of formic acid and ammonium formate can effectively promote the growth and food intake of animals; when the content of the formic acid is low, the growth of animals is not obviously changed, and when the content of the formic acid is high, the feeding and the growth of the animals are influenced.
Compared with the control group 2a and the control group 2b, the incidence rate and the death rate of the yellow chicken in the experimental group 2a and the experimental group 2b are obviously reduced, which shows that the acidifier can effectively protect the health of the yellow chicken when the molar ratio of formic acid to ammonium formate is less than 1: 1.5.
Compared with the comparison groups 3a and 3b, the average daily gain and the average daily feed intake of the yellow chickens of the experiment groups 3a and 3b are obviously increased, which indicates that the acidifier can effectively promote the feed intake and growth of the yellow chickens when the molar ratio of formic acid to ammonium formate is more than 1: 0.5.
In the comparison groups 2a and 2b, when the formic acid is less than 10 parts and the molar ratio of formic acid to ammonium formate is not in the range of 1:0.5-1.5, the feed intake and daily weight gain of yellow chickens are not obviously increased, but the diarrhea rate and the death rate are increased, which shows that when the formic acid is less than 10 parts and the molar ratio of formic acid to ammonium formate is not in the range of 1:0.5-1.5, the health of animals is affected.
Compared with the comparative groups 3a and 3b, when the formic acid is more than 50 parts and the molar ratio of the formic acid to the ammonium formate is not in the range of 1:0.5-1.5, the average feed intake and the average daily gain of the yellow chickens are reduced, which shows that when the formic acid is more than 50 parts, the feed intake of animals is influenced, and that high content of the formic acid influences the palatability of the feed and further influences the growth of the animals.
The described embodiments of the invention are only some embodiments of the invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The formic acid type acidifier for the feed is characterized by comprising a liquid acidifier, wherein the liquid acidifier comprises the following components in parts by weight: 10-50 parts of formic acid, 10-50 parts of ammonium formate and 0-80 parts of water.
2. The formic acid type acidifier for the feed is characterized by comprising a powder type acidifier, wherein the powder type acidifier comprises the following components in parts by weight: 10-50 parts of formic acid, 10-50 parts of ammonium formate, 0-80 parts of water and a carrier, wherein the formic acid, the ammonium formate and the water form a liquid acidifier, and the weight part ratio of the liquid acidifier to the carrier is 1: 0.3-5.
3. The feed formic acid-type acidifier according to claim 1 or 2, wherein the molar ratio of formic acid to ammonium formate is from 1:0.5 to 1.5.
4. The formic acid type acidifier for feed according to claim 1 or 2, wherein ammonium formate is obtained by purchasing or synthesizing formic acid by reacting with ammonia, the ammonia is one or a mixture of two or more of ammonium carbonate, ammonium bicarbonate, aqueous ammonia and liquid ammonia, and the ammonium formate is preferably synthesized by reacting formic acid with liquid ammonia.
5. The formic acid type acidifier for feed according to claim 3, wherein ammonium formate is obtained by purchasing or synthesizing formic acid by reacting with ammonia, the ammonia is one or a mixture of two or more of ammonium carbonate, ammonium bicarbonate, aqueous ammonia and liquid ammonia, and the ammonium formate is preferably synthesized by reacting formic acid with liquid ammonia.
6. The formic acid type acidifier for feed according to claim 1, 2 or 5, wherein the carrier is one or a mixture of two or more of silica, sodium sulfate, zeolite powder, montmorillonite, sepiolite, bentonite and maifanite.
7. The formic acid-type acidifier for feed according to claim 3, wherein the carrier is one or a mixture of two or more of silica, sodium sulfate, zeolite powder, montmorillonite, sepiolite, bentonite and maifanite.
8. A process for producing a formic acid type acidifier for feed, which comprises the formic acid type acidifier for feed according to any one of claims 1 to 7, characterized by comprising the steps of:
s1, putting 17.8-86.5 parts of formic acid and 0-80 parts of water into a reaction kettle, starting stirring, introducing liquid ammonia into the reaction kettle, adding the liquid ammonia into the reaction kettle, simultaneously opening cooling water for cooling, and controlling the temperature in the reaction kettle to be below 70 ℃ to obtain a mixture of formic acid, ammonium formate and water;
s2, cooling by using cooling water after liquid ammonia is added, sampling and detecting the molar ratio of formic acid to ammonium formate, if the molar ratio of formic acid to ammonium formate in the mixture of formic acid, ammonium formate and water is =1:0.5-1.5, the obtained mixture of formic acid, ammonium formate and water is a liquid acidifier, otherwise, liquid ammonia needs to be added into the reaction kettle.
9. The process for preparing a formic acid-type acidifier for feed according to claim 8, which further comprises the steps of: s3, after the detection is qualified, mixing the liquid acidulant obtained in the step S2 with a carrier, and grinding to obtain a powder acidulant; the weight portion ratio of the liquid acidifier to the carrier is 1: 0.3-5.
10. A method of using a formic acid type acidifier for feed, which comprises the step of adding 2 to 6kg/t of a formic acid type acidifier for feed as described in any one of claims 1 to 7.
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| CN101524118A (en) * | 2009-04-24 | 2009-09-09 | 安徽泰格生物技术有限公司 | Acidulant for feed and preparation method therefor |
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