CN110367439B - Method for preparing feed mildew removing agent by using low-grade clay mineral - Google Patents

Method for preparing feed mildew removing agent by using low-grade clay mineral Download PDF

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CN110367439B
CN110367439B CN201910810215.2A CN201910810215A CN110367439B CN 110367439 B CN110367439 B CN 110367439B CN 201910810215 A CN201910810215 A CN 201910810215A CN 110367439 B CN110367439 B CN 110367439B
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low
grade
bentonite
attapulgite clay
clay
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CN110367439A (en
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程飞飞
于阳辉
刘克起
杨启帆
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Suzhou Sinoma Design And Research Institute Of Non Metallic Minerals Industry Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/27Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
    • A23L5/273Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers

Abstract

The invention provides a method for preparing a feed mildew removing agent by using low-grade clay minerals. The method of the invention comprises the following steps: 1) Respectively crushing the low-grade bentonite and the low-grade attapulgite clay, and mixing to obtain a mixed material; 2) Adding water into the mixed material obtained in the step 1) and mashing the mixed material into slurry; 3) Grading the material subjected to the pulp tamping in the step 2), and removing coarse particles to obtain fine-grained ore pulp; 4) Adding tourmaline powder into the fine-fraction ore pulp obtained in the step 3), stirring and centrifuging; 5) And (3) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) to obtain the feed mildew removing agent. The method for preparing the feed mildew removing agent by using the low-grade clay minerals avoids energy consumption increase and cost reduction caused by repeated operation, expands deep processing application approaches of low-quality clay, and simultaneously has good synergistic adsorption effect on various mycotoxins.

Description

Method for preparing feed mildew removing agent by using low-grade clay mineral
Technical Field
The invention belongs to the technical field of mildew remover processing, relates to a preparation method of a feed mildew remover, and particularly relates to a method for preparing a feed mildew remover by using low-grade clay minerals.
Background
Mycotoxin is a secondary metabolite of mould generated in the storage and processing processes of feed, and not only can destroy effective components and nutrients in the feed, but also can cause damage and failure of internal organs and organs of animals due to accumulation of a large amount of mycotoxin in the animals, and also can inhibit the feed intake of the animals, weaken the immunity of the animals and further induce epidemic diseases or diseases of inflammation. For human beings, the livestock and poultry containing mycotoxin can cause certain damage to the bodies after being eaten for a long time. Therefore, it is necessary to remove the mold from the feed.
The feed mildew remover is an additive which can effectively inhibit or eliminate the activity of mycotoxin when being added into feed. At present, common feed mold removing agents mainly comprise clay, chinese herbal medicines, yeast cell walls and enzymolysis detoxication, wherein the clay feed mold removing agent is prepared by taking clay minerals with the characteristics of large specific surface area, strong adsorption force and the like as main raw materials.
CN 102178130A discloses a mineral compound from which mycotoxin is removed, and preparation prevention and application thereof, wherein montmorillonite and attapulgite with the purity of more than 95% are used as raw materials, and a compound mineral mold remover is prepared by preparing suspension, mixing, stirring, centrifuging, drying, sieving and the like, so that mycotoxin in feed can be effectively removed.
CN 107136388A discloses a compound mildew removing agent containing chitosan oligosaccharide and a preparation method thereof, the method takes montmorillonite with the purity of more than 95 percent as a main raw material, simultaneously compounds a small amount of chitosan oligosaccharide and potassium salt, prepares the compound mildew removing agent by a method of adding water, mixing and drying, and can effectively remove various harmful mycotoxins in feed.
CN 109511862A discloses a preparation method of a mineral feed mold remover, which takes attapulgite with the purity of more than 80 percent as a main raw material and rectorite and tourmaline as auxiliary materials to prepare the feed mold remover through wet ball milling and organic modification.
The preparation method of the mildew removal product can find that the existing clay feed mildew removal agent is mainly prepared by taking high-purity montmorillonite and attapulgite as main raw materials and compounding a small amount of auxiliary materials in an aqueous medium in a ball milling, stirring and other modes, but the mildew removal agent has the following two main defects:
the first is that: the quality of most clay ores in China is poor, a wet purification process is generally needed for obtaining high-purity products, and the purification cost is high, so the purchase cost of raw materials of the feed mildew removing agent is relatively high;
secondly, the following steps: when the clay mineral with high purity is obtained by adopting wet purification, the process of adding water, dehydrating, drying and grinding is needed; when the high-purity clay mineral is used as a raw material to prepare the feed mildew removing agent, the processes of adding water, dehydrating, drying and grinding are also carried out; repeated operation improves energy consumption, and does not meet the requirements of energy conservation and emission reduction.
Therefore, it is necessary to provide a method for preparing a feed mold remover by using low-grade clay minerals, which aims at the problems that the cost of high-purity clay minerals is relatively high, the processes of water adding, dehydration, drying and grinding are repeated in the processes of wet purification of the clay minerals and preparation of the feed mold remover, and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a feed mildew removing agent by using low-grade clay minerals, so that the energy consumption increase caused by repeated operation is avoided, the cost is reduced, the deep processing application approach of low-quality clay is expanded, and meanwhile, the prepared feed mildew removing agent has a good synergistic adsorption effect on various mycotoxins.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a feed mildew removing agent by using low-grade clay minerals, which comprises the following steps:
1) Respectively crushing the low-grade bentonite and the low-grade attapulgite clay, and mixing to obtain a mixed material;
2) Adding water into the mixed material obtained in the step 1) and mashing the mixed material into slurry;
3) Grading the material subjected to the pulp tamping in the step 2), and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder into the fine-fraction ore pulp obtained in the step 3), stirring and centrifuging;
5) And (3) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) to obtain the feed mildew removing agent.
According to the invention, low-grade clay minerals are used as raw materials, a preparation process of firstly compounding and then purifying is adopted, and the clay mineral purification and the compound preparation of the mold removing agent are effectively combined together, so that on one hand, the increase of energy consumption and the reduction of cost caused by repeated operation are avoided, on the other hand, the deep processing application approach of the low-grade clay is expanded, and meanwhile, the prepared feed mold removing agent also has a good synergistic adsorption effect on various mycotoxins.
In the step 1), the low-grade bentonite has the function of providing an effective component of montmorillonite, the low-grade attapulgite clay has the function of providing an effective component of attapulgite, the montmorillonite and the attapulgite have good adsorbability, the feed mildew such as aflatoxin and zearalenone are well adsorbed, and the two are compounded for use, so that the synergistic effect is achieved, and the total adsorption amount of the multiple mycotoxins can be increased.
The low-grade bentonite is bentonite with a montmorillonite content of less than 50%, especially bentonite with a montmorillonite content of 20-50%, for example, bentonite with a montmorillonite content of 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, etc.
Preferably, the low grade attapulgite clay is attapulgite clay with attapulgite content less than 50%, especially attapulgite with attapulgite content of 20-50%, such as attapulgite content of 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, etc.
In the step 1), the particle size of the crushed low-grade bentonite is less than 2 cm.
Preferably, the particle size of the crushed low-grade attapulgite clay is less than 2 cm.
In the step 1), the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is (5-8): (5-2), for example, the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is 5, 6, 7, 3, 8 and the like.
In the step 2), the mass ratio of the mixture to the water is 1 (5-12), for example, the mass ratio of the mixture to the water is 1.
Preferably, the time for mashing is 10-60 min, for example, the time for mashing is 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min.
In step 3), the classified particle size is 45 to 75 μm, for example, the classified particle size is 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, or the like.
In step 4), tourmaline powder is not only for Pb 2+ 、Cd 2+ The heavy metal toxin has better adsorption and removal effects, and can emit far infrared rays, promote the metabolism of animals and reduce the residue of the toxin in the bodies of the animals. The mass of the tourmaline powder accounts for the steps1) 2-10% of the total mass of the low-grade bentonite and the low-grade attapulgite clay, for example, the mass of the tourmaline powder accounts for 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10% of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1).
Preferably, the particle size of the tourmaline powder is 2 to 10 μm, for example, the particle size of the tourmaline powder is 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, etc.; the purity of the tourmaline powder is more than 60%.
In the step 4), the stirring time is 1-5 h, for example, the stirring time is 1h, 2h, 3h, 4h, 5h, and the like.
Preferably, the rotation speed of the centrifugation is 1000-3000 r/min, for example, the rotation speed of the centrifugation is 1000r/min, 1500r/min, 2000r/min, 2500r/min, 3000r/min, etc.; the centrifugation time is 2-10 min, for example, the centrifugation time is 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, 10min.
In the step 5), the number of the sieved meshes is 100-300 meshes, for example, the number of the sieved meshes is 100 meshes, 150 meshes, 200 meshes, 250 meshes or 300 meshes.
As a preferable scheme of the invention, the method for preparing the feed mildew removing agent by using the low-grade clay mineral comprises the following steps:
1) Respectively crushing low-grade bentonite with the montmorillonite content of less than 50% and low-grade attapulgite clay with the attapulgite content of less than 50% to the particle size of less than 2cm, and mixing the crushed low-grade bentonite and the crushed low-grade attapulgite clay with the attapulgite content of less than 50% according to the mass ratio of (5-8) to (5-2) to obtain a mixed material;
2) Adding water into the mixed material in the step 1) according to the mass ratio of 1 (5-12) and mashing for 10-60 min;
3) Classifying the material which is subjected to the pulp smashing in the step 2), wherein the classified particle size is 45-75 mu m, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 2-10 mu m and the purity of more than 60 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 2-10 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), stirring for 1-5 h, and centrifuging at the rotating speed of 1000-3000 r/min for 2-10 min;
5) And (5) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) by a 100-300-mesh sieve to obtain the feed mildew removing agent.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, low-grade clay minerals are used as raw materials, a preparation process of firstly compounding and then purifying is adopted, and the clay mineral purification and the compound preparation of the mold removing agent are effectively combined together, so that on one hand, the increase of energy consumption and the reduction of cost caused by repeated operation are avoided, on the other hand, the deep processing application approach of the low-grade clay is expanded, and meanwhile, the prepared feed mold removing agent also has a good synergistic adsorption effect on various mycotoxins.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The method for preparing the feed mildew removing agent by using the low-grade clay mineral comprises the following steps:
1) Respectively crushing low-grade bentonite with the montmorillonite content of 30% and low-grade attapulgite clay with the attapulgite content of 30% to the particle size of below 2cm, and mixing the materials according to the mass ratio of 7;
2) Adding water into the mixed material obtained in the step 1) according to a mass ratio of 1;
3) Grading the material subjected to the pulp smashing in the step 2), wherein the granularity of the grading is 45 mu m, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 5 microns and the purity of 80 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 6 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), and centrifuging for 6min at the rotating speed of 2000r/min after stirring for 4 h;
5) And (3) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) by a 200-mesh sieve to obtain the feed mildew removing agent.
Example 2
The method for preparing the feed mildew removing agent by using the low-grade clay mineral comprises the following steps:
1) Respectively crushing low-grade bentonite with the montmorillonite content of 20% and low-grade attapulgite clay with the attapulgite content of 20% to the particle size of below 2cm, and mixing the materials according to the mass ratio of 8;
2) Adding water into the mixed material obtained in the step 1) according to a mass ratio of 1;
3) Classifying the material subjected to the pulp tamping in the step 2), wherein the classified particle size is 75 mu m, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 8 mu m and the purity of 90 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 4 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), and centrifuging for 4min at the rotating speed of 3000r/min after stirring for 3 h;
5) And (5) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) by a 300-mesh sieve to obtain the feed mildew removing agent.
Example 3
The method for preparing the feed mildew removing agent by using the low-grade clay mineral comprises the following steps:
1) Respectively crushing low-grade bentonite with the montmorillonite content of 40% and low-grade attapulgite clay with the attapulgite content of 40% to the particle size of below 2cm, and mixing according to the mass ratio of 6;
2) Adding water into the mixed material in the step 1) according to a mass ratio of 1;
3) Grading the material subjected to the pulp smashing in the step 2), wherein the granularity of the grading is 50 microns, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 10 mu m and the purity of 70 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 8 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), and centrifuging for 8min at the rotating speed of 1500r/min after stirring for 5 h;
5) And (5) drying, grinding and screening the material precipitate obtained after the centrifugation in the step 4) by a 100-mesh sieve to obtain the feed mildew removing agent.
Example 4
The method for preparing the feed mildew removing agent by using the low-grade clay mineral comprises the following steps:
1) Respectively crushing low-grade bentonite with the montmorillonite content of 40% and low-grade attapulgite clay with the attapulgite content of 30% to the particle size of below 2cm, and mixing the materials according to the mass ratio of 5 to obtain a mixed material;
2) Adding water into the mixed material obtained in the step 1) according to a mass ratio of 1;
3) Classifying the material subjected to the pulp tamping in the step 2), wherein the classified particle size is 60 mu m, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 3 mu m and the purity of 60 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 10 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), stirring for 2h, and centrifuging for 10min at the rotating speed of 1000 r/min;
5) And (3) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) by a 200-mesh sieve to obtain the feed mildew removing agent.
Example 5
The difference between this example and example 1 is that in step 1), the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is 3.
Example 6
The difference between the embodiment and the embodiment 1 is that in the step 1), the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is 9.
Comparative example 1
The difference between the comparative example and the example 1 is that in the step 1), the low-grade attapulgite clay is not contained, the low-grade bentonite is adopted, in the step 4), the mass of the tourmaline powder accounts for 6% of the total mass of the low-grade bentonite in the step 1), and the rest is the same as that in the example 1.
Comparative example 2
The difference between the comparative example and the example 1 is that in the step 1), the low-grade bentonite is not contained, the low-grade attapulgite clay is completely adopted, in the step 4), the mass of the tourmaline powder accounts for 6 percent of the total mass of the low-grade attapulgite clay in the step 1), and the rest parts are the same as those in the example 1.
Comparative example 3
This comparative example is different from example 1 in that tourmaline powder was not added in step 4), and the rest was the same as example 1.
Comparative example 4
The difference between this example and example 1 is that in step 4), the mass of tourmaline powder is 20% of the total mass of the low-grade bentonite and the low-grade attapulgite clay in step 1), and the rest is the same as that in example 1.
The adsorption rates of the feed mold removers prepared in examples 1 to 6 and comparative examples 1 to 4 to various mycotoxins were measured, and the results are shown in table 1.
TABLE 1
Figure BDA0002184770250000091
Figure BDA0002184770250000101
As can be seen from Table 1, in examples 5 and 6, the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is too low or too high, the prepared feed mold remover has poor synergistic effect, and the adsorption effect on each mycotoxin is better than that of the feed mold remover prepared by a single mineral (comparative example 1 and comparative example 2) and is worse than that of the feed mold remover with proper mass ratio (examples 1 to 4).
In comparative example 1 and comparative example 2, comparative example 1 contained no low-grade attapulgite clay, and comparative example 2 contained no low-grade montmorillonite, and the mold remover for feed made of a single mineral had no synergistic effect and had a poor adsorption effect on each mycotoxin.
In comparative example 3, the feed mold remover prepared without tourmaline powder did not exert a ternary synergistic effect, and the adsorption effect on each mycotoxin was slightly inferior to that of examples 1 to 4.
In comparative example 4, the consumption of tourmaline powder was too high, and the adsorption effect of the prepared feed mold remover on various mycotoxins was not significantly improved compared with example 1, indicating that tourmaline powder was in a supersaturated state.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (11)

1. A method for preparing a feed mildew removing agent by using low-grade clay minerals is characterized by comprising the following steps:
1) Respectively crushing the low-grade bentonite and the low-grade attapulgite clay, and mixing to obtain a mixed material; the low-grade bentonite is bentonite with montmorillonite content of less than 50%, and the low-grade attapulgite clay is attapulgite clay with attapulgite content of less than 50%; the mass ratio of the low-grade bentonite to the low-grade attapulgite clay is (5-8) to (5-2);
2) Adding water into the mixed material obtained in the step 1) and mashing the mixed material into slurry;
3) Grading the material subjected to the pulp tamping in the step 2), and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder into the fine-fraction ore pulp obtained in the step 3), stirring and centrifuging; the mass of the tourmaline powder accounts for 2-10% of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1);
5) And (5) drying, grinding and sieving the material precipitate obtained after the centrifugation in the step 4) to obtain the feed mildew removing agent.
2. The method according to claim 1, wherein in step 1), the particle size of the crushed low-grade bentonite is 2cm or less.
3. The method according to claim 1, wherein the crushed low-grade attapulgite clay in step 1) has a particle size of 2cm or less.
4. The method as claimed in claim 1, wherein in the step 2), the mass ratio of the mixed material to the water is 1 (5-12).
5. The method as claimed in claim 1, wherein in the step 2), the time for mashing is 10-60 min.
6. The method according to claim 1, wherein in step 3), the classified particle size is 45 to 75 μm.
7. The method according to any one of claims 1 to 6, wherein in step 4), the particle size of the tourmaline powder is 2 to 10 μm, and the purity of the tourmaline powder is 60% or more.
8. The method according to claim 1, wherein in the step 4), the stirring time is 1-5 h.
9. The method according to claim 1, wherein in the step 4), the centrifugal rotating speed is 1000-3000 r/min, and the centrifugal time is 2-10 min.
10. The method as claimed in claim 1, wherein in the step 5), the number of the sieved meshes is 100 to 300 meshes.
11. Method according to claim 1, characterized in that it comprises the following steps:
1) Respectively crushing low-grade bentonite with the target mineral content of less than 50% and low-grade attapulgite clay with the target mineral content of less than 50% until the particle size is less than 2cm, and mixing the crushed low-grade bentonite and the crushed low-grade attapulgite clay with the target mineral content of less than 50% according to the mass ratio of (5-8) to (5-2) to obtain a mixed material;
2) Adding water into the mixed material obtained in the step 1) according to the mass ratio of 1 (5-12) and mashing for 10-60 min;
3) Classifying the material which is subjected to the pulp smashing in the step 2), wherein the classified particle size is 45-75 mu m, and removing coarse particles to obtain fine-grained ore pulp;
4) Adding tourmaline powder with the granularity of 2-10 mu m and the purity of more than 60 percent into the fine-fraction ore pulp obtained in the step 3), wherein the mass of the tourmaline powder accounts for 2-10 percent of the total mass of the low-grade bentonite and the low-grade attapulgite clay in the step 1), stirring for 1-5 h, and centrifuging at the rotating speed of 1000-3000 r/min for 2-10 min;
5) And (3) drying, grinding and sieving the material precipitate obtained after centrifugation in the step 4) by a 100-300-mesh sieve to obtain the feed mildew removing agent.
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CN108516562A (en) * 2018-06-07 2018-09-11 苏州中材非金属矿工业设计研究院有限公司 A kind of purifying technique of Concave-convex clay rod

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