CN112868913A - Microencapsulated feed enzyme preparation and preparation method thereof - Google Patents
Microencapsulated feed enzyme preparation and preparation method thereof Download PDFInfo
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/10—Organic substances
- A23K20/189—Enzymes
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/142—Amino acids; Derivatives thereof
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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
- A23K20/158—Fatty acids; Fats; Products containing oils or fats
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/163—Sugars; Polysaccharides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/00—Accessory food factors for animal feeding-stuffs
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- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
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Abstract
The invention discloses a microencapsulated feed enzyme preparation and a preparation method thereof, wherein the enzyme preparation comprises the following raw material components in parts by weight: 20-60 parts of feed enzyme; 10-40 parts of an inert carrier framework; 1-10 parts of cysteine; 1-5 parts of hydroxypropyl methyl cellulose; 5-30 parts of sucrose fatty acid ester; 15-70 parts of coating material. The invention adopts the cysteine, the hydroxypropyl methylcellulose and the sucrose fatty acid ester as the raw material components to participate in the granulating and coating process of the microencapsulated feed enzyme preparation, not only can improve the stability of the product in the processing process, but also can ensure that the product is not damaged by the environments of high humidity, high heat, strong shearing force and the like in the processing processes of transportation, storage and steam conditioning and granulating, and plays an important role in improving the enzyme activity of the product before application.
Description
Technical Field
The invention relates to the technical field of animal feed addition, in particular to a microencapsulated feed enzyme preparation and a preparation method thereof.
Background
China is a world wide corn planting country, and 70% of corns are used for producing feed. 50 to 80 percent of phosphorus in the corn exists in the form of phytic acid, but the phosphorus in the form can not be digested and utilized by monogastric animals such as pigs, poultry and the like, and the environment can be seriously polluted after excrement of animals is excreted. The phytase is a generic name of enzymes which catalyze phytic acid and salts thereof to be hydrolyzed into inositol and phosphate, can degrade phytic acid with rich content in feed, can release inorganic phosphorus beneficial to the growth and development of animals, and can release other nutrient substances combined with the phytic acid, thereby being beneficial to better absorption and utilization of monogastric animals such as pigs, poultry and the like, reducing the feed cost, reducing the discharge amount of phosphorus in animal wastes and lightening the environmental pollution.
Therefore, the phytase is a green feed additive which is more in application and better in prospect at present. The main problems of the phytase in the application are that the phytase has poor heat resistance, the enzyme activity is reduced or even inactivated during the storage and the feed processing, the enzyme waste is caused, and the use cost is increased.
In China, the pellet feed accounts for about 70% of the total feed yield, and the market demand is huge. Generally, the production of the feed needs a high-temperature granulation process, generally 75-80 ℃, particularly for inactivating some pathogenic bacteria in the feed, the common treatment temperature reaches 85 ℃, the treatment time is 30s-3min, and the phytase easily loses partial activity or even completely inactivates at the temperature. Therefore, obtaining phytase with high thermal stability is a research hotspot and difficulty of phytase industry in recent years.
At present, the following methods can be used for obtaining the high-temperature resistant phytase: (1) the heat resistance of the phytase can be improved to a certain extent by changing the molecular structure of the phytase and chemically modifying the phytase molecules with glycosyl. (2) The new phytase strain is cultivated by utilizing biotechnology and gene site-directed mutagenesis technology. The new phytase variety is obtained by chemical or biological methods, which can fundamentally improve the high temperature resistance of phytase and obtain some research results, such as technical schemes disclosed in patent application publications with application publication numbers of CN10659256A, CN106434850A, CN10638890A, 106323964A, CN106260584A, CN10601102A, CN10601101A, CN10601000A and CN 106119223A. However, the mechanism of phytase thermotolerance is still unclear, and therefore, there is no theoretical basis for the development of new phytase varieties. In addition, the development of new phytase varieties has the defects of large investment, long time, difficult screening and high risk, and is not suitable for the national conditions of China, and the developed new varieties are easily influenced by process conditions due to immature processes to generate variation, so that the performance of the phytase products is unstable, and the large-scale industrial production is difficult.
The coating process is an effective means for improving the high-temperature and high-humidity resistance of the phytase, and the stress resistance of the coated phytase product to steam conditioning granulation can be greatly enhanced. However, the degree of difference in the activity retention of phytase treated by different coating processes relative to the phytase after conditioned granulation at 75 ℃ and 85 ℃ is to be evaluated by steam conditioned granulation.
Disclosure of Invention
The invention provides a microencapsulated enzyme preparation for feed and a preparation method thereof, and the microencapsulated enzyme preparation for feed can not only improve the stability of enzyme preparations such as feed enzyme and the like in the processing process, but also ensure that the enzyme preparations are prevented from being damaged by environments such as high humidity, high heat, strong shearing force and the like in the processing processes of transportation, storage and steam conditioning and granulation, and play a beneficial role in improving the enzyme activity of products before application.
The specific technical scheme is as follows:
a microencapsulated feed enzyme preparation comprises the following raw material components in parts by weight:
tests show that the cysteine not only has the functions of protecting active groups of the enzyme preparation and maintaining the active structure of the enzyme preparation, but also can keep the activity of the enzyme preparation from being reduced all the time in the granulation process with high temperature, high humidity and strong shearing force, thereby improving the quality of the enzyme preparation. If other antioxidant substances such as mercaptoethanol or tea polyphenol are replaced, the activity of the enzyme preparation is obviously reduced in the granulation process with high temperature, high humidity and strong shearing force. The hydroxypropyl methylcellulose and the sucrose fatty acid ester are used together, so that the function of maintaining the spatial structure of the enzyme preparation is realized, and the stress resistance of the enzyme preparation to strong shearing force during granulation is improved in the steam granulation process.
Further, the feeding enzyme is one of xylanase, glucanase, mannase, protease, amylase, lipase, cellulase, glucose oxidase, lysozyme and phytase.
Preferably, the feeding enzyme is phytase.
Preferably, the mass ratio of the hydroxypropyl methyl cellulose to the sucrose fatty acid ester is 1: 5-10. The retention rate of the product in the granulation process is higher under the proportion, and the retention rate of the product in the granulation process is greatly reduced outside the proportion range.
Specifically, the inert carrier backbone comprises: 5-20 parts of alpha-starch and 5-20 parts of diatomite. The alpha-starch forms a layer of protective film around the enzyme preparation molecules, and is used together with diatomite, so that the enzyme preparation has about water resistance, when the enzyme preparation is subjected to steam tempering and granulation, the enzyme preparation can be isolated from water, and inert carrier materials such as silicon dioxide, anhydrous sodium sulphate and the like cannot play a role in water resistance.
Specifically, the coating material comprises: 5-30 parts of polyethylene glycol glyceryl ricinoleate and 10-40 parts of stearic acid. Stearic acid can improve the stability of the enzyme preparation as a stabilizer, the effect is limited when the stearic acid is used alone, and the polyethylene glycol glyceryl ricinoleate can protect the enzyme preparation from being damaged by temperature. The amount of the polyethylene glycol glyceryl ricinoleate and the amount of the stearic acid are required to be careful and should be matched with each other, and if the amount of the polyethylene glycol glyceryl ricinoleate is too small, the temperature resistance of the product is deteriorated. The combined use of the polyethylene glycol glyceryl ricinoleate and the stearic acid avoids the defect that other skeleton type coating materials can only maintain the physical structure of the effective components, and increases the stability of the effective components to temperature.
Preferably, the microencapsulated enzyme preparation for feed comprises the following components in parts by weight:
preferably, the microencapsulated enzyme preparation for feed comprises the following components in parts by weight:
preferably, the microencapsulated enzyme preparation for feed comprises the following components in parts by weight:
the invention also provides a preparation method of the microencapsulated enzyme preparation for feed, which comprises the following steps:
(1) mixing feeding enzyme, an inert carrier skeleton and cysteine, and uniformly mixing to obtain a mixture;
(2) dissolving hydroxypropyl methylcellulose and sucrose fatty acid ester in an organic solvent I to obtain a spray;
(3) spraying and granulating the mixture by adopting the spraying agent in the step (2) to obtain a granular product;
(4) dissolving the coating material in an organic solvent II to prepare a coating liquid;
(5) and (4) coating the granular product obtained in the step (3) by using the coating liquid obtained in the step (4) to obtain the microencapsulated enzyme preparation for feeding.
Further, in the step (2), the organic solvent I is alcohol with the mass fraction of 70-80%; in the step (3), the conditions for spray granulation are as follows: the rotating speed is 10-20 Hz, the atomizing pressure is 0.1-0.2 MPa, and the flow rate of the peristaltic pump is 20-30 r/min.
Further, in the step (4), the organic solvent II is diethyl ether; in the step (5), the conditions of the coating treatment are as follows: the air inlet temperature is 30-40 ℃, the air outlet temperature is 30-40 ℃, the atomization pressure is 0.1-0.2 MPa, and the flow rate of the coating liquid is 0.1-2L/min.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts the cysteine, the hydroxypropyl methylcellulose and the sucrose fatty acid ester as the raw material components to participate in the granulating and coating process of the microencapsulated feed enzyme preparation, not only can improve the stability of the product in the processing process, but also can ensure that the product is not damaged by the environments of high humidity, high heat, strong shearing force and the like in the processing processes of transportation, storage and steam conditioning and granulating, and plays an important role in improving the enzyme activity of the product before application.
Detailed Description
The present invention will be further described with reference to the following specific examples, which are only illustrative of the present invention, but the scope of the present invention is not limited thereto.
Materials in the following examples are mixed by a V-shaped mixer, granulated by a high-speed mixing, granulating and rounding machine and coated by a coating machine of a cyclone fluidized bed; and sieving the granules by using a vibrating sieving machine.
Example 1
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
25 parts of phytase; 6.5 parts of alpha-starch; 5 parts of diatomite; 5 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 15 parts of polyethylene glycol glycerol ricinoleate; and 35 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 50kg of phytase (5 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 10kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 70kg of stearic acid and 30kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Example 2
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
20 parts of phytase; 6.5 parts of diatomite; 5 parts of alpha-starch; 10 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 10 parts of polyethylene glycol glycerol ricinoleate; and 40 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 40kg of phytase (5 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 20kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 80kg of stearic acid and 20kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Example 3
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
60 parts of phytase; 5 parts of diatomite; 5 parts of alpha-starch; 5 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 5 parts of sucrose fatty acid ester; 9 parts of polyethylene glycol glycerol ricinoleate; 10 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 120kg of phytase (5 ten thousand IU/g), 10kg of diatomite, 10kg of alpha-starch and 10kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 10kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 20kg of stearic acid and 18kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Comparative example 1
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
25 parts of phytase; 6.5 parts of diatomite; 5 parts of alpha-starch; 5 parts of mercaptoethanol; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 15 parts of polyethylene glycol glycerol ricinoleate; and 35 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 50kg of phytase (5 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 10kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 70kg of stearic acid and 30kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Comparative example 2
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
25 parts of phytase; 6.5 parts of diatomite; 5 parts of alpha-starch; 5 parts of tea polyphenol; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 15 parts of polyethylene glycol glycerol ricinoleate; and 35 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 50kg of phytase (5 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 10kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 70kg of stearic acid and 30kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Comparative examples 3 to 5
The following comparative examples are the same as example 1 except that the amounts of the raw materials used were different.
Comparative example 3: the microencapsulated feed enzyme preparation is prepared from the following raw materials in parts by weight: 25 parts of phytase; 6.5 parts of diatomite; 5 parts of alpha-starch; 5 parts of cysteine; 10 parts of hydroxypropyl methyl cellulose; 2.5 parts of sucrose fatty acid ester; 30 parts of polyethylene glycol glycerol ricinoleate; and 16 parts of stearic acid.
Comparative example 4: the microencapsulated feed enzyme preparation is prepared from the following raw materials in parts by weight: 25 parts of phytase; 5 parts of diatomite; 10 parts of alpha-starch; 15 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 3 parts of polyethylene glycol glycerol ricinoleate; 33.5 parts of stearic acid.
Comparative example 5: the microencapsulated feed enzyme preparation is prepared from the following raw materials in parts by weight: 30 parts of phytase; 1 part of diatomite; 20 parts of alpha-starch; 0 part of cysteine; 1 part of hydroxypropyl methyl cellulose; 3 parts of sucrose fatty acid ester; 15 parts of polyethylene glycol glycerol ricinoleate; 30 parts of stearic acid.
The retention rates of the preparations obtained in examples 1 to 3 and comparative examples 1 to 5 after hardening and tempering at 75 ℃/85 ℃ and the retention rate after granulation at 75 ℃/85 ℃ were measured.
The specific detection method comprises the following steps: the steam conditioning and ring die granulating unit adopts a granulating unit with the yield of 100kg/h of Jiangsu shepherd. The conditioner is a double-shaft differential conditioner, the length of a conditioning cylinder is 1.2 meters, the diameter of a double cylinder is 22cm, the conditioning time of a first test is 70s, the conditioning time of a second test is 35s, the conditioning temperature is set to be 75 ℃ and 85 ℃ (the temperature at the outlet of the conditioner, and a temperature probe is used for probing on the lower side of the conditioner). The compression ratio of the granulating ring die is 6:1, and the aperture is 4 mm. The feeding frequency is 3HZ, and the yield is 100 kg/h. Electronic temperature sensors are arranged at the conditioner and the granulating outlet, and temperature data are collected through a program-controlled computer.
The quenching, tempering and granulating processes are as follows: and opening a steam main valve and a compressed air valve, mixing the premixed raw materials in a mixer for 55s, entering a granulation buffer bin, and sequentially opening a steam valve and a drain valve (closing after discharging cold water). And then opening the granulator, the conditioner and the granulating feeder in sequence in a computer system to start granulating. And (4) collecting a sample after the quenching and tempering temperature reaches 75 ℃ of a set value and the granulation system normally operates for 15 min. And then changing the set value of the quenching and tempering temperature to 85 ℃, reaching the set value of 85 ℃, and collecting a sample after the granulation system normally operates for 15 min. During sampling, the samples are continuously collected for 10min respectively at a sampling port of a feeder before tempering, after tempering and after granulation, and the samples collected every 1min are put into a self-sealing bag to be 1 sample, and 10 samples are counted. Storing in a refrigerator at 4 deg.C.
And recording the temperature of quenching, tempering and granulating by using a temperature sensor at the discharge hole of the quenching and tempering device. And (4) determining the content of water in the feed according to GB/T6435-2006. The activity of the phytase is determined according to GB/T18634-2009, the activity unit of which is defined as: at 37 deg.C and pH 5.50, 1 μmol inorganic phosphorus is released from sodium phytate solution with concentration of 5.0mmol/L per minute, and the unit of phytase activity is expressed in U/g.
The retention rate after enzyme activity modification is equal to the active concentration of phytase after modification (U/g DM)/the active concentration of phytase before modification (U/g DM). times.100%.
The retention after enzymatic activity pelletization (U/g DM) of phytase after pelletization)/the active concentration of phytase before pelletization (U/g DM) × 100%.
The results are shown in Table 1.
TABLE 1 Retention rates of the products of each of the examples and comparative examples after 75 deg.C/85 deg.C tempering and after 75 deg.C/85 deg.C granulation
Example 4
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
20 parts of xylanase; 6.5 parts of diatomite; 5 parts of alpha-starch; 10 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 10 parts of polyethylene glycol glycerol ricinoleate; and 40 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 40kg of xylanase (10 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 20kg of cysteine, and uniformly mixing to obtain 83kg of a mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 80kg of stearic acid and 20kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Example 5
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
20 parts of protease; 6.5 parts of diatomite; 5 parts of alpha-starch; 10 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 10 parts of polyethylene glycol glycerol ricinoleate; and 40 parts of stearic acid.
The preparation method comprises the following steps:
(1) 40kg of protease (10 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 20kg of cysteine are mixed and evenly mixed to obtain 83kg of mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 80kg of stearic acid and 20kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Example 6
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
20 parts of glucose oxidase; 6.5 parts of diatomite; 5 parts of alpha-starch; 10 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 10 parts of polyethylene glycol glycerol ricinoleate; and 40 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 40kg of glucose oxidase (10 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 20kg of cysteine, and uniformly mixing to obtain 83kg of mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 80kg of stearic acid and 20kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
Example 7
A microencapsulated feed enzyme preparation is composed of the following raw materials in parts by weight:
20 parts of lysozyme; 6.5 parts of diatomite; 5 parts of alpha-starch; 10 parts of cysteine; 1 part of hydroxypropyl methyl cellulose; 7.5 parts of sucrose fatty acid ester; 10 parts of polyethylene glycol glycerol ricinoleate; and 40 parts of stearic acid.
The preparation method comprises the following steps:
(1) mixing 40kg of lysozyme (500 ten thousand IU/g), 10kg of diatomite, 13kg of alpha-starch and 20kg of cysteine, and uniformly mixing to obtain 83kg of mixture;
(2) dissolving 2kg of hydroxypropyl methylcellulose and 15kg of sucrose fatty acid ester in 65kg of 75% alcohol to obtain a spray;
(3) spraying and granulating the mixture I obtained in the step (1) by adopting the spraying agent obtained in the step (2), setting the air inlet temperature to 50 ℃, slowly spraying the spraying agent while rotating and mixing, discharging when dry particles with the diameter of 1mm are formed, obtaining a particle product, and recovering alcohol;
(4) sieving the granular product obtained in the step (3) (a 10-mesh sieve), removing large granules, and reserving undersize to obtain a sieved granular product;
(5) dissolving 80kg of stearic acid and 20kg of polyethylene glycol glycerol ricinoleate in 90kg of diethyl ether to prepare a coating liquid;
(6) and (3) carrying out coating treatment on the screened granular product obtained in the step (4) by adopting the coating liquid obtained in the step (5), controlling the air speed to enable the material to keep a height of 45cm above a material gun, setting the air inlet temperature to be 50 ℃ and the fan frequency to be 50hz, slowly spraying the prepared coating liquid, uniformly spraying the coating liquid on the surface of granules to obtain the microencapsulated enzyme preparation for feeding, and recovering diethyl ether.
The retention rate of the preparation obtained in examples 4 to 7 after tempering at 75 ℃/85 ℃ and the retention rate of the preparation after granulation at 75 ℃/85 ℃ are detected. The results are shown in Table 2.
TABLE 2 Retention rates of the products of the examples after 75 deg.C/85 deg.C tempering and after 75 deg.C/85 deg.C granulation
Claims (10)
2. a microencapsulated feed enzyme preparation as claimed in claim 1 wherein the feed enzyme is one of xylanase, glucanase, mannanase, protease, amylase, lipase, cellulase, glucose oxidase, lysozyme and phytase.
3. A microencapsulated feed enzyme preparation as claimed in claim 1 wherein the feed enzyme is a phytase.
4. A microencapsulated enzyme preparation for feed as claimed in claim 1 wherein the inert carrier matrix comprises: 5-20 parts of alpha-starch and 5-20 parts of diatomite; the coating material comprises: 5-30 parts of polyethylene glycol glyceryl ricinoleate and 10-40 parts of stearic acid.
8. a method of preparing a microencapsulated enzyme preparation for feed use as claimed in any of claims 1 to 7 which comprises the steps of:
(1) mixing feeding enzyme, an inert carrier skeleton and cysteine, and uniformly mixing to obtain a mixture;
(2) dissolving hydroxypropyl methylcellulose and sucrose fatty acid ester in an organic solvent I to obtain a spray;
(3) spraying and granulating the mixture by adopting the spraying agent in the step (2) to obtain a granular product;
(4) dissolving the coating material in an organic solvent II to prepare a coating liquid;
(5) and (4) coating the granular product obtained in the step (3) by using the coating liquid obtained in the step (4) to obtain the microencapsulated enzyme preparation for feeding.
9. A method for preparing a microencapsulated enzyme preparation for feed as claimed in claim 8 wherein in step (2), the organic solvent I is alcohol with a mass fraction of 70-80%; in the step (3), the conditions for spray granulation are as follows: the rotating speed is 10-20 Hz, the atomizing pressure is 0.1-0.2 MPa, and the flow rate of the peristaltic pump is 20-30 r/min.
10. A process for the preparation of a microencapsulated enzyme preparation for feed as claimed in claim 8 wherein in step (4) the organic solvent II is diethyl ether; in the step (5), the conditions of the coating treatment are as follows: the air inlet temperature is 30-40 ℃, the air outlet temperature is 30-40 ℃, the atomization pressure is 0.1-0.2 MPa, and the flow rate of the coating liquid is 0.1-2L/min.
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