CN115176879B - Preparation method of rumen-bypass methionine - Google Patents
Preparation method of rumen-bypass methionine Download PDFInfo
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- CN115176879B CN115176879B CN202211099652.6A CN202211099652A CN115176879B CN 115176879 B CN115176879 B CN 115176879B CN 202211099652 A CN202211099652 A CN 202211099652A CN 115176879 B CN115176879 B CN 115176879B
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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
- A23K20/142—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
- A23K20/163—Sugars; Polysaccharides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- 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
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/25—Shaping or working-up of animal feeding-stuffs by extrusion
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
- A23K40/35—Making capsules specially adapted for ruminants
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/10—Feeding-stuffs specially adapted for particular animals for ruminants
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Abstract
The invention discloses a preparation method of rumen-bypass methionine, methionine crystals are firstly pre-coated in a fluidized bed coating machine to change the surface physical properties of the methionine crystals; then uniformly mixing the pre-coated powder, the auxiliary agent and water, and then extruding and cutting in a double-screw extruder to obtain a regular core material; finally, the core material is coated for the second time in a fluidized bed coating machine to obtain the rumen bypass methionine finished product. The rumen bypass methionine prepared by the method has the following advantages: the extrusion process is stable and controllable, the repeatability of the release result is good, the product qualification rate is high, and the bioavailability is high.
Description
Technical Field
The invention belongs to the technical field of feed additives, and particularly relates to a preparation method of rumen bypass methionine.
Background
Ruminants are a sub-order of the artiodactyla. Rumination refers to eating and feeding food which is half digested in the stomach to return to the mouth for chewing again after a period of time, and ruminants are animals with such a digestion mode as ruminants, such as cows, sheep, giraffes and the like. Ruminants are generally some herbivores because the plant fibers are relatively indigestible. Ruminant feed intake is usually in a hurry, especially for roughage, most of which is swallowed into the rumen without being fully chewed, and after the rumen is soaked and softened for a period of time, the food returns to the oral cavity again through retching, and is mixed into saliva again through re-chewing and swallowed into the rumen.
Rumen bypass methionine belongs to one of rumen bypass proteins, and refers to a feed additive variety in which methionine in feed is not degraded by rumen microorganisms and can enter true stomach.
The rumen bypass methionine is prepared by two methods, namely a chemically improved method and a physically protected method, wherein the physically protected method is to wrap a layer of protective agent on the surface of a methionine core material to prevent methionine from being decomposed by microorganisms in rumen. Common wrapping materials are fats and polymers. The specific process is as follows: firstly, adding auxiliary materials into methionine, uniformly mixing, then carrying out extrusion granulation to obtain a core material, and finally coating the core material in a fluidized bed coating machine to obtain a rumen-protected methionine product.
In 2015, popply plum, a Zhejiang Wanfang Biotechnology Limited company, and the like, applied for invention patent of a preparation method of rumen bypass lysine, application publication No. CN 104970228A, and in the examples, the following technical schemes are disclosed:
1. pre-treating, namely performing superfine grinding pre-treatment on L-lysine hydrochloride (source: middle grain group), screening, sieving by using a 80-mesh sieve, and then sieving by using a 200-mesh sieve, wherein 80-200 meshes are required materials: the coating effect can be reduced by oversize raw materials which are not crushed;
2. the preparation method comprises the following specific steps:
the method comprises the following steps: preparation of pellet core
Putting 60kg of L-lysine hydrochloride and 2kg of starch which are crushed and sieved into a trough type mixer to be uniformly mixed, adding the mixture into a ball throwing machine, adding purified water through a spray gun of the ball throwing machine until a product forms spherical particles of 30-40 meshes, adding the spherical particles of the ball throwing machine into a boiling dryer, drying the spherical particles at the air inlet temperature of 80 ℃ for 0.5-1 hour to obtain a pill core, and detecting the water content on line to be not more than 3%.
Step two: primary coating
Adding the 62kg of pills into a coating machine, melting 16kg of food-grade hydrogenated vegetable oil (the source is industrial hydrogenation of palm oil, the manufacturer is Jiaxing Shanghai east daily chemical industry, the model is the melting point is 58 ℃) at 80 ℃, starting a fluidized coating machine, adjusting the air inlet temperature to be 45 to 50 ℃, carrying out isolated coating on the pills by the hydrogenated vegetable oil through a bottom spraying system of the coating machine until all the pills are completely sprayed, and continuously carrying out fluidized drying for 30 to 60 minutes to obtain a primary coating intermediate product 1;
step three: secondary coating
Carrying out swing arrangement on the primary coating intermediate product 1 through a 20-mesh net by using a YK160 series swing type granulator, and screening by using 40 meshes; the sieved particles with the particle size of more than 40 meshes are placed in a DPL60/120 multifunctional granulating and coating machine, and 22kg of melted carnauba wax (the manufacturer: jiaxing Shanghao Dong daily chemical company, model: melting point 58 ℃) is used as a coating material for coating in a bottom spraying mode.
Coating parameters: air inlet temperature: treating at 20 deg.C, material temperature 35-40 deg.C, atomization pressure 0.2-0.25MPa, and pump flow rate 15L/h for 30min; and (4) screening by 40 meshes after coating is finished to obtain a final product with more than 40 meshes: rumen bypass lysine.
The appearance of the rumen bypass lysine is in a strip shape, and the effective component of the rumen bypass lysine of the final product can reach 60 percent through detection.
The granulation process of the patent is carried out in a shot blasting machine, and when rumen-bypass DL-methionine is prepared, the problems that the particle density is low and the product cannot smoothly pass through the rumen and enter the true stomach exist. Although the patent adopts a double-layer coating technology, the problem of pressure relief in the granulation process of a double-screw extruder cannot be solved.
In 2020, von quieter, a product for rumen bypass and a production method thereof, which is filed by Wuxi great biology corporation and the like, the application publication No. CN 112544803A discloses the following technical characteristics in the claims, and the production method comprises the following specific steps:
step 1, auxiliary material pretreatment: heating and melting palm oil in a reaction kettle, controlling the temperature while stirring until the palm oil is uniformly stirred, adding a surfactant after the temperature is stable, and uniformly mixing for later use; the stirring temperature is 80-90 ℃;
step 2, preparing master batches from raw materials: adding the crushed and sieved raw materials into white carbon black and a binder, and granulating and rounding;
step 3, bottom spraying operation: and (3) putting the dried master batch in the step (2) into a fluidized bed coating machine, starting a fan, controlling the temperature in the fluidized bed to be about 35-45 ℃, then spraying the mixture of the palm oil and the surfactant in the step (1) onto the master batch in the step (2) at a constant speed through a spray gun, keeping the hot air temperature of the spray gun to be above 140-150 ℃, and sieving the granules through a 40-80-mesh sieve to finally obtain a finished product.
The specification describes: the specific gravity of the product is between 0.9 and 1.0, and the specific gravity of the rumen fluid is between 1.022 and 1.055, so that the product is suspended in the rumen fluid and smoothly passes through the rumen along with the peristalsis of the rumen. But in practice, ruminants are more likely to ruminate low-density material during the rumination process, causing the product to be damaged, since low-density products are more likely to float on the surface.
The inventor finds that even if the same granulating and coating process is adopted, the rumen bypass methionine prepared in different batches has unstable product quality, has poor reproducibility when testing release rate indexes, and is easily influenced by the quality of methionine crystallization raw materials in the process of preparing rumen bypass methionine.
Disclosure of Invention
The invention provides a preparation method of rumen-bypass methionine, and the rumen-bypass methionine product obtained by the preparation method has stable quality and high product percent of pass, and is not easily influenced by methionine crystallization raw materials.
The technical scheme of the invention is as follows:
a preparation method of rumen bypass methionine comprises the following steps:
(1) Pre-coating methionine crystals in a fluidized bed coating machine to obtain pre-coated powder;
the coating material used for the pre-coating is low-viscosity ethyl cellulose;
the Brookfield viscosity of the low-viscosity ethyl cellulose measured in a mixed solution of toluene and ethanol with the volume ratio of 80 to 11mPa.s is 6 to 11mPa.s;
the mass ratio of the methionine crystal to the ethyl cellulose is 1:0.002 to 0.015;
(2) Extruding and cutting a mixture of the pre-coating powder, the auxiliary agent and water in a double-screw extruder to obtain a cylindrical core material;
(3) Performing secondary coating on the cylindrical core material in a fluidized bed coating machine to obtain a finished rumen-protected methionine product;
the coating material used for the secondary coating is medium-viscosity ethyl cellulose;
the medium-viscosity ethyl cellulose has a Brookfield viscosity of 19 to 23mPa.s measured in a mixed solution of toluene and ethanol with a volume ratio of 80;
the mass ratio of the cylindrical core material to the medium-viscosity ethyl cellulose in the step (3) is 1:0.01 to 0.02.
The inventor finds that the pressure fluctuation is easy to occur when methionine crystals with different crystal forms and particle sizes and auxiliary materials are mixed and extruded and granulated in a double-screw extruder; the outlet speeds of the holes of the multi-hole die are different; the core materials obtained by cutting have different lengths and the like, thereby influencing the qualification rate of the core materials. When the core material is different in length, even if the coating material is uniformly coated, the problem of poor reproducibility in the release rate index test is necessarily caused by the fact that the surface area of the unit volume of the core material is different. In order to avoid the over-dependence of the rumen bypass methionine product release rate index on methionine crystallization raw materials, the invention solves the problem by a two-step coating method.
The invention wraps a little low viscosity ethyl cellulose on the surface of methionine crystal before granulating, and the layer of ethyl cellulose has two functions: 1. the surface physical property of methionine crystal is changed, and the adverse effect of particle size difference on the extrusion process is reduced; 2. the purpose of slow release is achieved. The purpose of the second core coating is to avoid the core being damaged in the rumen, and the surface of the core is damaged during the fluidized bed coating process due to the violent collision between the cores, and the damaged gaps inevitably cause part of the core to be damaged after entering the rumen. According to the invention, the surface of the methionine crystal is pre-coated with a layer of low-viscosity (molecular weight) ethyl cellulose, so that even if the coating layer of the core material is damaged, the methionine in the core material cannot be quickly damaged.
In the step (1), the amount of pre-coating and the viscosity of ethyl cellulose need to be strictly controlled, otherwise, the problem that methionine in the core material cannot be completely released after entering the true stomach will occur. Preferably, the ethyl cellulose is N7 ethyl cellulose or N10 ethyl cellulose, and the best effect can be achieved.
Preferably, the outlet pressure of the twin-screw extruder in the step (2) in the extrusion process is 5 to 15MPa.
Preferably, the temperature of the extrusion process in the twin-screw extruder in the step (2) is 80 to 100 ℃.
Preferably, the exhaust port of the twin-screw extruder in the step (2) is connected to a vacuum system for air suction.
The obtained granular rumen-bypass product must have certain density, otherwise, the product is easy to return to the mouth for chewing in the process of rumination, and the utilization rate of the effective components is greatly reduced. To obtain a denser core, it is necessary to control the exit of the powder from the twin-screw extruderThe pressure must be greater than 5MPa. The pressure resistance of the double-screw extruder is comprehensively considered, the maximum pressure is controlled not to exceed 15MPa, and the prepared product with the density of more than 1.1g/cm 3 The core material of (2) can completely meet the requirements of rumen bypass products on density. The temperature in the extrusion granulation process in the double-screw extruder needs to be controlled within 80 to 100 ℃, the viscosity of the powder is very high when the temperature is lower than 80 ℃, and the overpressure of the double-screw extruder is easily caused; the temperature is more than 100 ℃, the water loss is serious, and the surface smoothness of the core material is poor. The exhaust port of the double-screw extruder is connected to a vacuum system for air exhaust, so that air holes in the extruded and granulated product can be reduced, and the density is improved.
In the step (2), other auxiliary materials used for granulation have no particularly strict requirements, and auxiliary materials commonly used in the field can be adopted.
Preferably, in the step (3), the medium viscosity ethyl cellulose is N20 ethyl cellulose or N22 ethyl cellulose.
The coating process of the core material is carried out in a fluidized bed coating machine, the coating material is also selected from ethyl cellulose, but the specification of the ethyl cellulose coated by the core material is different relative to the ethyl cellulose pre-coated. The core material coating needs to adopt ethyl cellulose with the specification of medium viscosity. The higher the molecular weight, the higher the viscosity, the higher the coating hardness, the less breakage, but the release rate after entering the stomach also becomes very low; the molecular weight must not be too small, otherwise too much breakage occurs during the coating process and the proportion of methionine destroyed in the rumen will increase.
And finally: the amount of viscous ethylcellulose in the core coating process is as important as the molecular weight, and too thick a coating, while reducing breakage in the fluidized bed, also poses the problem of slow release. Comprehensively considering the molecular weight of the ethyl cellulose, when the mass ratio of the core material to the ethyl cellulose is 1:0.01 to 0.02, and the best effect can be achieved.
Compared with the prior art, the invention has the following beneficial effects:
1. the pressure is stable in the extrusion granulation process, the material outlet speeds of all holes of the multi-hole mouth mold are consistent, the products obtained by cutting are uniform, and the product percent of pass is higher;
2. the product release rate is convenient to adjust, and the bioavailability is high;
3. the rumen bypass methionine preparation process is not influenced by methionine crystallization raw materials, and the obtained rumen bypass methionine product has stable quality and good reproducibility when the release rate index is tested.
Drawings
FIG. 1 is a scanning electron microscope photograph of a DL-methionine crystalline starting material used in the present invention.
Detailed Description
The present invention will be specifically described below by way of examples, but the present invention is not limited to these examples.
Example 1
(1) Preparing a pre-coating solution:
in a 250ml beaker was added 95% ethanol: 100g, ethyl cellulose (having a Brookfield viscosity of 6 to 8 mPa.s as measured in toluene and ethanol of 80: 2g, stirring at normal temperature until the mixture is completely dissolved.
(2) Pre-coating:
a layer of 200 mesh stainless steel wire mesh was fixed in the orifice plate of FLP-3-type fluidized bed coating machine (Kyoho granulation drying apparatus Co., ltd.). Feeding DL-methionine into a coating machine: 1000g (see figure 1 for scanning electron microscope photo), and starting a draught fan of a fluidized bed coating machine, wherein DL-methionine in the coating machine is in a fluidized state. The electric heater of the air-conditioning box is opened, and the heating temperature is set as follows: 35 ℃ is carried out. And pumping the prepared ethyl cellulose ethanol solution into an atomizer of a fluidized bed coating machine by using a peristaltic pump, and adjusting the feeding speed of the peristaltic pump to be 5ml/min. The whole feeding process takes about 20 minutes. After coating, fluidized drying was continued for 30 minutes. And (5) obtaining pre-coating powder after drying.
The above operation was repeated 3 times to obtain about 3kg of precoated powder in total.
(3) Mixing materials:
pre-coating powder is put into a 50L three-dimensional mixer: 3kg, corn starch: 0.3kg, sodium stearate: 0.2kg, water: 0.6kg, start the three-dimensional mixer, mix for 30 minutes.
(4) Extruding and granulating:
opening a DSE32-II type double-screw extruder (Jinan Ding Run mechanical equipment limited, in the middle of 2.0X 25 porous die), opening heating modules for electric heating, and controlling the heating temperatures of the 6 groups of heating modules to be 85 ℃. When the temperature of the extruder is stabilized at 85 ℃, the mixed materials are fed into a feeding port of the extruder. The exhaust port is connected with water to flush and pump for vacuum, and the vacuum degree of the exhaust port is controlled to be more than-0.07 MPa. Starting a main engine motor, setting the frequency of the main engine motor: 10Hz, opening a feeding screw, and setting the motor frequency of the feeding screw: 15Hz, start the feed extrusion. When the material is conveyed to the vicinity of the mouth mold of the extruder by the screw, the pressure will rise rapidly, and when the pressure rises to more than 5MPa, the material will be extruded from the small hole of the mouth mold by the screw. At the moment, the frequency of the host machine and the frequency of the feeder are synchronously adjusted, and the outlet pressure is controlled within 5 to 6 MPa. And after the material speeds of all outlets of the porous mouth mold are consistent, cutting is started. And adjusting the rotating speed of the cutter. The length of the core material is controlled to be 3-5 mm. About 3.0kg of qualified core material (part of the core material is left in the extruder) is obtained, the material before being stably extruded by the extruder is crushed, the water content is adjusted to be 12-15%, and then extrusion granulation is repeatedly carried out.
(5) Preparing secondary coating liquid:
in a 2000ml beaker was added 95% ethanol: 1200g of ethyl cellulose with specification N20 (brookfield viscosity of 19 to 21 mpa.s measured in toluene and ethanol from santitant cellulose co., shandong, 80: 30g (slowly adding in portions to avoid sticking together), and stirring until the mixture is completely dissolved.
(6) Secondary coating:
the hole plate of the coating machine is replaced by a hole plate with the hole diameter of 1 to 1.5mm, and 3.0kg of core material is added into the coating machine. And starting a draught fan of the fluidized bed coating machine, wherein the DL-methionine in the coating cylinder is in a fluidized state. The motor heater of the air-conditioning box is opened for air inlet, and the heating temperature is set as follows: at 50 deg.C. And pumping the prepared ethyl cellulose ethanol solution into an atomizer of a fluidized bed coating machine by using a peristaltic pump, and adjusting the feeding speed of the peristaltic pump to be 10ml/min. The entire feed process takes about 2 hours. After the feeding is finished, the fluidized drying is continued for 30 minutes. After drying, the total amount of the finished rumen-protected DL-methionine product is about: 3.0kg, the specific gravity of the product is 1.115, the specific gravity is slightly higher than rumen fluid, and the product is not easy to be returned to the mouth for chewing in the rumination process, thereby meeting the requirement of the rumen bypass product on density. In-vitro experiment detection: 8-hour release rate: 25.1 percent; 24-hour release rate: 70.4 percent.
The in vitro experiment detection method comprises the following steps: taking a rumen bypass DL-methionine finished product: 1.00g, 100ml of dipotassium hydrogen phosphate/potassium dihydrogen phosphate buffer solution with pH =6.0 is added, the mixture is shaken for a certain time in a water bath shaker and then filtered, and a small amount of distilled water is added to wash a filter cake. And detecting the content of methionine in the filtrate by adopting a redox method, and converting to obtain the release rate of the oscillation time.
Example 2
The pre-coating specification in example 2 is the amount of ethylcellulose charged for N7: 10g, ethyl cellulose with specification N20 in the secondary coating: 30g, the rest process conditions are the same as the example 1, the specific gravity of the obtained product is 1.119, and the in vitro experiment detection: 8-hour release rate: 20.4 percent; 24-hour release rate: 68.3 percent.
Example 3
The pre-coating specification in example 3 is the amount of ethylcellulose charged for N7: 15g, ethyl cellulose with specification N20 in the secondary coating: 30g, the rest process conditions are the same as those in example 1, the specific gravity of the obtained product is 1.123, and the in vitro experiment detection is as follows: 8-hour release rate: 15.7 percent; 24-hour release rate: 65.6 percent.
Example 4
The pre-coating specification in example 4 is the amount of ethylcellulose charged with N7: 10g, ethyl cellulose with specification N20 in the secondary coating: 45g, the rest process conditions are the same as the example 1, the specific gravity of the obtained product is 1.127, and the in vitro experiment detection: 8-hour release rate: 12.8 percent; 24-hour release rate: and (4) percent.
Example 5
The pre-coating specification in example 5 is the amount of ethylcellulose charged for N7: 10g, ethyl cellulose with specification N20 in the secondary coating: 60g, the rest process conditions are the same as those in example 1, the specific gravity of the obtained product is 1.123, and in vitro experiment detection: 8-hour release rate: 12.9 percent; 24-hour release rate: and (4) 64.5%.
Example 6
The precoating specification of ethylcellulose of example 6, N10 (brookfield viscosity measured in toluene and ethanol from santopram cellulose, inc., 80, 20, 9 to 11 mpa.s), the amounts charged: 2g of ethyl cellulose with the specification of N20 in the secondary coating, and the input amount is as follows: 30g, the rest process conditions are the same as the example 1, the specific gravity of the obtained product is 1.125, and the in vitro experiment detection: 8-hour release rate: 23.6 percent; 24-hour release rate: 67.1 percent.
Example 7
Ethyl cellulose with the specification of N10 for the precoating in example 7, the input amount: 2g of ethyl cellulose with specification N22 in the secondary coating (Brookfield viscosity of 21 to 23mPa.s measured in toluene and ethanol of 80, from Tantay cellulose Co., ltd., shandong): 30g, the rest process conditions are the same as the example 1, the specific gravity of the obtained product is 1.128, and the in vitro experiment detection: 8-hour release rate: 22.1 percent; 24-hour release rate: 65.5 percent.
Example 8
(1) Preparation of pre-coating liquid:
in a 250ml beaker was added 95% ethanol: 100g, adding ethyl cellulose with specification of N7: 2g, stirred at room temperature until completely dissolved.
(2) Pre-coating:
a layer of 200-mesh stainless steel wire mesh is fixed in a hole plate of an FLP-3 type fluidized bed coating machine (good granulating and drying equipment, inc. of Changzhou city). Feeding DL-methionine into a coating machine: 1000g, starting a draught fan of a fluidized bed coating machine, and keeping DL-methionine in the coating machine in a fluidized state. The electric heater of the air-inlet air-conditioning box is set with the heating temperature: 35 ℃ is carried out. And pumping the prepared ethyl cellulose ethanol solution into an atomizer of a fluidized bed coating machine by using a peristaltic pump, and adjusting the feeding speed of the peristaltic pump to be 5ml/min. The whole feeding process takes about 20 minutes. After coating, the fluidized drying was continued for 30 minutes. And (5) obtaining pre-coating powder after drying.
The above operation was repeated 3 times to obtain about 3kg of precoated powder in total.
(3) Mixing materials:
pre-coating powder is put into a 50L three-dimensional mixer: 3kg, corn starch: 0.3kg, sodium stearate: 0.2kg, water: 0.6kg, start the three-dimensional mixer, mix for 30 minutes.
(4) And (3) extruding and granulating:
opening a DSE32-II type double-screw extruder (Jinan Ding Run mechanical equipment limited, in the middle of 2.0X 25 porous die), opening heating modules for electric heating, and controlling the heating temperatures of the 6 groups of heating modules to be 95 ℃. When the temperature of the extruder is stabilized at 95 ℃, the mixed materials are fed into a feeding port of the extruder. The exhaust port is connected with water to flush the pump for vacuum pumping, and the vacuum degree of the exhaust port is controlled to be more than-0.07 MPa. Starting a main engine motor, setting the frequency of the main engine motor: 10Hz, opening a feeding screw, and setting the motor frequency of the feeding screw: 15Hz, start the feed extrusion. When the material is conveyed to the position near the mouth die of the extruder by the screw, the pressure is quickly increased, and when the pressure is increased to be more than 9.5MPa, the material is extruded from the small holes of the mouth die by the screw. At the moment, the host frequency and the feeder frequency are synchronously adjusted, and the outlet pressure is controlled within 9.5 to 12.0 MPa. And after the material speeds of all outlets of the porous mouth mold are consistent, cutting is started. And adjusting the rotating speed of the cutter. The length of the core material is controlled to be 3-5 mm. About 3.0kg of qualified core material is obtained (partial residue exists in the extruder), the material before being stably extruded by the extruder is crushed, the water content is adjusted to 12 to 15%, and then the extrusion granulation is repeatedly carried out.
(5) Preparing secondary coating liquid:
in a 2000ml beaker was added 95% ethanol: 1200g, adding ethyl cellulose with specification N20: 30g (slowly adding in portions to avoid adhesion) and stirring until complete dissolution.
(6) Secondary coating:
the hole plate of the coating machine is replaced by a hole plate with the hole diameter of 1 to 1.5mm, and 3.0kg of core material is added into the coating machine. And starting a fluidized bed coating machine induced fan, wherein DL-methionine in the coating cylinder is in a fluidized state. The air-inlet air-conditioning box motor heater is set with the heating temperature: at 50 deg.C. And pumping the prepared ethyl cellulose ethanol solution into an atomizer of a fluidized bed coating machine by using a peristaltic pump, and adjusting the feeding speed of the peristaltic pump to be 10ml/min. The entire feeding process takes about 2 hours. After the feeding is finished, the fluidized drying is continued for 30 minutes. After drying, the total rumen bypass DL-methionine product is about: 3.0kg, the specific gravity of the obtained product is 1.116. In-vitro experiment detection: 8-hour release rate: 20.4 percent; 24-hour release rate: 67.3 percent.
Comparative example 1
(1) Mixing materials:
the DL-methionine crystals were put into a 50 liter three-dimensional mixer: 3kg, corn starch: 0.3kg, sodium stearate: 0.2kg, water: 0.6kg, start the three-dimensional mixer, mix for 30 minutes.
(4) And (3) extruding and granulating:
opening a DSE32-II type double-screw extruder (Jinan Ding Run mechanical equipment limited, in the middle of 2.0X 25 porous die), opening heating modules for electric heating, and controlling the heating temperatures of the 6 groups of heating modules to be 85 ℃. When the temperature of the extruder is stabilized at 85 ℃, the mixed materials are fed into a feeding port of the extruder. The exhaust port is connected with water to flush the pump for vacuum pumping, and the vacuum degree of the exhaust port is controlled to be more than-0.07 MPa. Starting a host motor, and setting the frequency of the host motor: 10Hz, opening a feeding screw, and setting the motor frequency of the feeding screw: 15Hz, start the feed extrusion. When the material is conveyed to the vicinity of the mouth mold of the extruder by the screw, the pressure will rise rapidly, and when the pressure rises to more than 5MPa, the material will be extruded from the small hole of the mouth mold by the screw. And synchronously adjusting the frequency of the host machine and the frequency of the feeder, and controlling the outlet pressure within 5-6 MPa. And after the material speeds of all outlets of the porous mouth mold are consistent, cutting is started. And adjusting the rotating speed of the cutter. Controlling the length of the core material to be 3-5mm. And (3) the outlet pressure is unstable in the extrusion process, the extrusion speed of materials in each hole of the multi-hole die is inconsistent, about 2.2kg of qualified core material is obtained through screening (part of residues exist in the extruder), the materials before the extruder is used for stabilizing extrusion and the materials which are independently and unstably connected in the extrusion process are crushed, the water content is adjusted to be 12 to 15%, and then the extrusion granulation is repeatedly carried out. Obtaining qualified core materials in total: 2.7kg.
(5) Preparing a coating solution:
in a 2000ml beaker was added 95% ethanol: 1200g, adding ethyl cellulose with specification N20: 45g (slowly adding in portions to avoid sticking together) and stirring until the mixture is completely dissolved.
(6) Coating:
an orifice plate with the aperture of 1 to 1.5mm is arranged on a coating machine, and 2.7kg of core material is put into the coating machine. And starting a draught fan of the fluidized bed coating machine, wherein the DL-methionine in the coating cylinder is in a fluidized state. The air-inlet air-conditioning box motor heater is set with the heating temperature: at 50 ℃. And pumping the prepared ethyl cellulose ethanol solution into an atomizer of a fluidized bed coating machine by using a peristaltic pump, and adjusting the feeding speed of the peristaltic pump to be 10ml/min. The entire feeding process takes about 2 hours. After the feeding is finished, the fluidized drying is continued for 30 minutes. After drying, the total amount of the finished rumen-protected DL-methionine product is about: 2.7kg. And (3) in-vitro experiment detection: 8-hour release rate: 17.7 percent; 24-hour release rate: 49.4 percent, the release rate of the product in 24 hours is smaller, but the absorption of the product is not facilitated.
Claims (5)
1. A preparation method of rumen bypass methionine is characterized by comprising the following steps:
(1) Pre-coating the methionine crystals in a fluidized bed coating machine to obtain pre-coated powder;
the coating material used for the pre-coating is low-viscosity ethyl cellulose;
the Brookfield viscosity of the low-viscosity ethyl cellulose measured in a mixed solution of toluene and ethanol with the volume ratio of 80 to 11mPa.s is 6 to 11mPa.s;
the mass ratio of the methionine crystals to the low-viscosity ethyl cellulose is 1:0.002 to 0.015;
(2) Extruding and cutting a mixture of the pre-coating powder, the auxiliary agent and water in a double-screw extruder to obtain a cylindrical core material;
(3) Performing secondary coating on the cylindrical core material in a fluidized bed coating machine to obtain a finished rumen-protected methionine product;
the coating material used for the secondary coating is medium-viscosity ethyl cellulose;
the medium-viscosity ethyl cellulose has a Brookfield viscosity of 19 to 23mPa.s measured in a mixed solution of toluene and ethanol with a volume ratio of 80;
the mass ratio of the cylindrical core material to the medium-viscosity ethyl cellulose is 1:0.01 to 0.02;
in the step (2), the outlet pressure of the twin-screw extruder in the extrusion process is 5 to 15MPa.
2. The method for preparing rumen bypass methionine according to claim 1, wherein, in the step (1), the low viscosity ethylcellulose is one or both of N7 ethylcellulose and N10 ethylcellulose.
3. The method for preparing rumen bypass methionine according to claim 1, wherein the temperature of the extrusion process in the twin-screw extruder in step (2) is 80 to 100 ℃.
4. The method for preparing rumen-bypass methionine according to claim 1, wherein, in step (2), the exhaust port of the twin-screw extruder is connected to a vacuum system for pumping.
5. The method for preparing rumen-bypass methionine according to claim 1, wherein: in the step (3), the medium-viscosity ethyl cellulose is N20 ethyl cellulose or N22 ethyl cellulose.
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