Modified montmorillonite as well as preparation method and application thereof

Abstract

The invention belongs to the field of biology, and particularly relates to a preparation method of modified montmorillonite, which comprises the following steps: step 1, preparing sodium montmorillonite; step 2, modifying sodium montmorillonite by adopting cyclodextrin and organic acid; step 3, mixing the sodium-based montmorillonite obtained in the step 2, pypocholoride and chlorate; and step 4, mixing the probiotics, the enzyme and the mixture obtained in the step 3. The modified montmorillonite is subjected to sodium modification, cyclodextrin, hypochlorite and chlorate are loaded, and prebiotics are added, so that the breeding performance of the montmorillonite can be effectively improved. Meanwhile, the invention also provides a preparation method and application of the modified montmorillonite.

Description

Technical Field

[0001] The invention belongs to the field of feed, and in particular relates to a modified montmorillonite and a preparation method and application thereof. Background Art

[0002] Montmorillonite, a silicate mineral, is known for its excellent adsorption, cation exchange performance and gas-liquid barrier properties. This property makes montmorillonite have excellent flame retardancy and antibacterial properties. Montmorillonite is widely used in animal feed additives to reduce the incidence of diarrhea, replace zinc oxide and antibiotics, promote animal appetite, regulate body balance, and enhance immunity. Its cation exchange and adsorption capacity can effectively absorb harmful intestinal bacteria and toxins in the body, reduce body damage, and maintain health.

[0003] Publication No. CN111011610A, the subject is a manganese-loaded montmorillonite and its preparation method and application. It uses manganese ions to modify the montmorillonite, which can promote the improvement of chicken quality and enhance the immune ability of chicken.

[0004] In the existing technology, except for the modification of montmorillonite based on single sodium, manganese ions or organic solvents, these modification methods have improved the adsorption of polar chemicals to a certain extent, but the improvement of the adsorption capacity of non-polar components is limited. There are almost no other reports that use systematic thinking to modify montmorillonite to improve the modification efficiency.

[0005] Due to the important role of montmorillonite in aquaculture, further modification and optimization of montmorillonite is an important means to fully tap the aquaculture potential of montmorillonite.

[0006] In addition, in many feed raw materials and compound feeds, the high detection rate and excess rate of aflatoxins (AFB1), zearalenone (ZEN) and vomitoxin (DON) are the current situation that must be faced in the feed field, which means that some feed raw materials and compound feeds exceed the safety standards and pose a threat to animal health. After animals ingest contaminated feed, they will experience loss of appetite, indigestion, decreased immunity, growth inhibition, increased complications, and even lead to a large number of deaths. The intestine is one of the largest immune organs in the body. The invasion of mycotoxins can damage the immune function of the intestine and affect the health of the body. Mycotoxins can cause oxidative damage to the intestine of animals through the Nrf2 signaling pathway. The intake of mycotoxins will lead to increased metabolic activity of the intestinal microbiota, especially the metabolism of carbohydrates. Mycotoxins can affect the metabolism of intestinal microorganisms, thereby affecting intestinal function, resulting in changes in the homeostasis of intestinal flora, a decrease in the number of beneficial bacteria, and an increase in the number of harmful bacteria. The absorption of intestinal nutrients by mycotoxins mainly affects basal metabolism by affecting the gene and protein expression of nutrient transport carriers. The reduction in intestinal villi height leads to a reduction in absorption surface area, which also affects the intestinal absorption and metabolism of nutrients. Therefore, in the actual production process, we not only need to solve the problem of how to remove mycotoxins, but also need to solve the negative impact of mycotoxins on animal health, especially intestinal health.

[0007] The technical problem to be solved in this case is: how to modify and optimize montmorillonite to improve aquaculture performance. Summary of the invention

[0008] In view of the shortcomings of the prior art, the object of the present invention is to provide a modified montmorillonite, which is sodium-treated, loaded with cyclodextrin, hypochlorite and chlorate, and added with prebiotics, so as to effectively improve the breeding performance of montmorillonite.

[0009] At the same time, the invention also provides a preparation method and application of the modified montmorillonite.

[0010] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0011] A method for preparing modified montmorillonite comprises the following steps:

[0012] Step 1: preparing sodium montmorillonite using montmorillonite, soluble sodium salt and glucose as raw materials;

[0013] Step 2: Modifying sodium montmorillonite with cyclodextrin and organic acid;

[0014] Step 3: Mixing the sodium montmorillonite, hypochlorite and chlorate obtained in step 2;

[0015] Step 4: Mix the probiotics and enzymes with the mixture obtained in step 3.

[0016] The innovative features of the present invention are as follows:

[0017] 1. The modified montmorillonite of the present invention is a sodium-based modified montmorillonite;

[0018] Most of the montmorillonite in my country is calcium-based, and compared with sodium-based, the adsorption performance and effect are significantly different; through sodium-based modification, efficient adsorption performance can be achieved;

[0019] 2. The present invention doped glucose during the sodiumization process, which can significantly improve the adsorption performance of montmorillonite;

[0020] 3. The present invention adopts cyclodextrin and organic acid modification to improve the adsorption performance of montmorillonite, protect the prebiotics in montmorillonite, and improve the palatability;

[0021] Cyclodextrin is a type of macromolecule with a special ring structure, which is composed of multiple glucose units connected by α-1,4-glycosidic bonds. They have a hydrophobic inner cavity and a hydrophilic outer surface. This structure enables cyclodextrin to form inclusion complexes with various hydrophobic or medium-polar molecules, including amino acids. Amino acids, as small molecule hydrophobic compounds, can be embedded in the hydrophobic inner cavity of cyclodextrin and form stable complexes with cyclodextrin through non-covalent interactions such as hydrophobic effects, van der Waals forces, and possible hydrogen bonds. Cyclodextrin can combine with prebiotics added later to encapsulate prebiotics and prevent them from being destroyed by gastric acid; in addition, after cyclodextrin is loaded on montmorillonite, it can achieve better encapsulation of mycotoxins; using cyclodextrin loaded on montmorillonite can effectively improve the intestinal health of animals. In addition to being the nutrients required by the animal body, organic acids also react with subsequent hypochlorites and chlorates to slowly release chlorine dioxide to achieve control of intestinal pathogenic microorganisms;

[0022] 4. The present invention finally adopts prebiotics composed of probiotics and enzymes to improve intestinal health;

[0023] The probiotics used in the present invention are commercially available probiotics, which are in powder form and have a coating layer on the surface, and can be released into the intestine to increase the content of intestinal probiotics and regulate intestinal health.

[0024] At the same time, the organic acids loaded in montmorillonite can also regulate the acid-base balance of the intestine, create a more suitable growth environment for probiotics, and promote intestinal health.

[0025] In the above preparation method, the step 1 is specifically:

[0026] Step 11: heating the montmorillonite at 350-450° C. for activation;

[0027] Step 12: adding an aqueous solution containing glucose and a soluble sodium salt to the montmorillonite, and rolling at 70 to 90° C.;

[0028] Rolling operation can be done by wheel rolling extrusion, double screw extrusion, flow control extrusion, and double roller extrusion. Rolling operation mainly provides shear stress to separate the aggregated particles, and even push open the crystal layer, increase the specific surface area of ​​calcium montmorillonite, and accelerate the process of sodium ion exchange for calcium ion. During the extrusion process, part of the mechanical energy is converted into heat energy, which increases the temperature of montmorillonite and promotes the Na + and Ca 2+ The extrusion can also destroy the montmorillonite crystal structure and cause bond breakage. The exposed silicon ions, aluminum ions and oxygen ions absorb water, which is beneficial to the hydration of montmorillonite. While the bond breakage increases the negative charge on the surface of the original soil particles, the sodiumization is completed.

[0029] Rolling is a relatively economical and effective means of modification; the combination of high temperature activation and rolling can fully sodiumize montmorillonite, increase the specific surface area of ​​montmorillonite, and improve the modification effect and adsorption effect;

[0030] Step 13: Aging the montmorillonite obtained in step 12 at room temperature for 2 to 6 days to obtain preliminarily modified sodium-based montmorillonite.

[0031] In the above preparation method, the aqueous solution containing soluble sodium salt contains sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose; the mass ratio of sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose is 40-60:10-20:10-20:5-10:5-10;

[0032] Glucose is additionally used in the sodium modification process. As a reducing sugar, glucose can react chemically with the surface of montmorillonite to form a stable complex. This modification is mainly reflected in the following aspects: glucose molecules bind to the surface of montmorillonite through ion exchange, covalent bonds or non-covalent interactions, changing its surface properties, such as improving the adsorption efficiency of specific pollutants, and reacting with cations (such as Na + , Ca 2+ Glucose is an energy source that can provide additional nutrition to animals, especially to young or sick animals, and help improve their immunity and growth performance. Improve digestion: In animal feed, the combination of glucose and montmorillonite may help improve the digestion process of animals, because glucose can promote the growth of intestinal microorganisms, while montmorillonite helps maintain intestinal health.

[0033] The solute concentration of the aqueous solution containing the soluble sodium salt is 3 to 5 wt%;

[0034] The aqueous solution containing soluble sodium salt is equivalent to 10-30wt% of the weight of montmorillonite;

[0035] The aqueous solution containing the soluble sodium salt is sprayed onto the montmorillonite in the form of a spray.

[0036] In the above preparation method, the step 2 is specifically:

[0037] Step 21: adding cyclodextrin and organic acid into the polyvinyl alcohol solution to prepare a dextrin modifier;

[0038] Step 22: adding a dextrin modifier to the sodium montmorillonite and rolling the mixture at 70 to 90° C.;

[0039] Step 23: Dry the product of step 22.

[0040] In the above preparation method, the organic acid is one or more combinations of citric acid, succinic acid, and fumaric acid; the weight ratio of the cyclodextrin to the organic acid is 40-60:40-60;

[0041] The concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 0.5-1wt%;

[0042] The total concentration of cyclodextrin and organic acid in the dextrin modifier is 2 to 6 wt %;

[0043] The dextrin modifier is equivalent to 10-30wt% of the weight of montmorillonite;

[0044] The dextrin modifier is sprayed onto the montmorillonite in the form of a spray.

[0045] In the above preparation method, the step 3 is specifically:

[0046] Mixing hypochlorite, chlorate, calcium chloride and montmorillonite by rolling;

[0047] The weight ratio of the hypochlorite, calcium chloride and chlorate is 1:0.8-1.2:0.2-0.4;

[0048] The total weight of the hypochlorite, calcium chloride and chlorate is equivalent to 1-3 wt% of the weight of montmorillonite.

[0049] In the above preparation method, the probiotics are one or more combinations of yeast, Lactobacillus acidophilus, and Bacillus subtilis;

[0050] The probiotics are added to the mixture obtained in step 3 in the form of dry powder;

[0051] The weight of the probiotics is equivalent to 5-10 wt % of the weight of the mixture obtained in step 3.

[0052] In the above preparation method, the enzyme is glucose oxidase; the weight of the glucose oxidase is equivalent to 0.5-2wt% of the weight of the mixture obtained in step 3.

[0053] Meanwhile, the present invention also discloses a modified montmorillonite, which is prepared by any of the above methods.

[0054] Finally, the invention also discloses the use of the modified montmorillonite as described above in preparing chicken feed additives.

[0055] Compared with the prior art, the present invention has the following beneficial effects:

[0056] The modified montmorillonite of the present invention is sodiumized, loaded with cyclodextrin, hypochlorite and chlorate, and added with prebiotics, so as to effectively improve the breeding performance of the montmorillonite. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 is a bar graph showing the expression level of ileal claudin in the application evaluation experiment of the present invention. DETAILED DESCRIPTION

[0058] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0059] Source of raw materials:

[0060] Yeast: Angel Yeast, Fubon Saccharomyces cerevisiae;

[0061] Lactobacillus acidophilus: Challenge Group, Excellent C series lactic acid bacteria;

[0062] Bacillus subtilis: Challenge Group, Yiyou series products;

[0063] Glucose oxidase: Challenging group, thermostable glucose oxidase.

[0064] Example 1

[0065] The preparation method of modified montmorillonite comprises the following steps:

[0066] Step 1: preparing sodium montmorillonite;

[0067] Step 1 is as follows:

[0068] Step 11: heating the montmorillonite at 400° C. for 3 h;

[0069] Step 12: adding an aqueous solution containing a soluble sodium salt to the montmorillonite and rolling it at 80° C.;

[0070] The aqueous solution containing soluble sodium salt contains sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose; the mass ratio of sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose is 50:20:20:5:5;

[0071] The solute concentration of the aqueous solution containing the soluble sodium salt is 5wt%;

[0072] The specific operation of rolling is:

[0073] The aqueous solution containing soluble sodium salt is sprayed into the montmorillonite in a mist spraying method. The misted aqueous solution containing soluble sodium salt can easily contact with the montmorillonite particles to form water medium reaction conditions.

[0074] The double rollers rotate at a uniform speed to roll and mix the sodium-forming agent aqueous solution and montmorillonite. The rolling process temperature is about 80°C, which is more conducive to the degree of sodiumization.

[0075] Spraying and rolling are carried out simultaneously. After every five rounds of rolling, the blade scraper is used to scrape and mix to ensure that all montmorillonite materials can be evenly contacted and modified. The continuous rolling time is 20 minutes.

[0076] Step 13: aging the montmorillonite obtained in step 12 at room temperature for 4 days to obtain sodium montmorillonite;

[0077] Step 2: Modifying sodium montmorillonite with cyclodextrin and organic acid;

[0078] Step 2 is as follows:

[0079] Step 21: adding cyclodextrin and citric acid to the polyvinyl alcohol solution to prepare a dextrin modifier;

[0080] The weight ratio of the cyclodextrin and the organic acid is 1:1; the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 0.5wt%; the molecular weight of polyvinyl alcohol is 200000; the total concentration of cyclodextrin and the organic acid in the dextrin modifier is 3wt%;

[0081] Step 22: adding the dextrin modifier to the sodium montmorillonite and rolling at 80° C.;

[0082] For rolling operation, refer to step 12;

[0083] The dextrin modifier is equivalent to 20wt% of the weight of montmorillonite and is added in the form of spraying, and the spraying and rolling are carried out simultaneously;

[0084] Step 23: Dry the product of step 22 at 85°C for more than 6 hours, then grind the solid dry product and pass it through a 200-mesh sieve.

[0085] Step 3: rolling and mixing the sodium montmorillonite, hypochlorite, calcium chloride and chlorate obtained in step 2; the rolling operation is the same as step 12, except that in step 3, the sodium montmorillonite, hypochlorite, calcium chloride and chlorate are added in the form of dry mixing; the weight ratio of the hypochlorite, calcium chloride and chlorate is 1:1:0.3; the total weight of the hypochlorite, calcium chloride and chlorate is equivalent to 2wt% of the weight of the montmorillonite;

[0086] Step 4: Mix the probiotics, enzymes and the mixture obtained in step 3 at 50° C. for 2 hours; the probiotics are yeast, Lactobacillus acidophilus, and Bacillus subtilis; the above bacteria are added in the form of dry powder, and the weight ratio of each bacterial powder is 1:1:1; the weight of the probiotics is equivalent to 8wt% of the weight of the mixture obtained in step 3; the enzyme is glucose oxidase; the weight of the glucose oxidase is equivalent to 1.5wt% of the weight of the mixture obtained in step 3.

[0087] Example 2

[0088] The preparation method of modified montmorillonite comprises the following steps:

[0089] Step 1: preparing sodium montmorillonite;

[0090] Step 1 is as follows:

[0091] Step 11: heating the montmorillonite at 350° C. for 4 h;

[0092] Step 12: adding an aqueous solution containing a soluble sodium salt to the montmorillonite and rolling it at 90° C.;

[0093] The aqueous solution containing soluble sodium salt contains sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose; the mass ratio of sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose is 40:20:20:10:10;

[0094] The solute concentration of the aqueous solution containing the soluble sodium salt is 4wt%;

[0095] The specific operation of rolling is the same as that of Example 1;

[0096] Step 13: aging the montmorillonite obtained in step 12 at room temperature for 6 days to obtain sodium montmorillonite;

[0097] Step 2: Modifying sodium montmorillonite with cyclodextrin and organic acid;

[0098] Step 2 is as follows:

[0099] Step 21: adding cyclodextrin and citric acid to the polyvinyl alcohol solution to prepare a dextrin modifier;

[0100] The weight ratio of the cyclodextrin and the organic acid is 4:6; the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 1wt%; the molecular weight of polyvinyl alcohol is 200000; the total concentration of cyclodextrin and the organic acid in the dextrin modifier is 3wt%;

[0101] Step 22: adding a dextrin modifier to the sodium montmorillonite and rolling at 90° C.;

[0102] For rolling operation, refer to step 12;

[0103] The dextrin modifier is equivalent to 10wt% of the weight of montmorillonite and is added in the form of spraying, and the spraying and rolling are carried out simultaneously;

[0104] Step 23: Dry the product of step 22 at 85°C for more than 6 hours, then grind the solid dry product and pass it through a 200-mesh sieve.

[0105] Step 3: rolling and mixing the sodium montmorillonite, hypochlorite, calcium chloride and chlorate obtained in step 2; the rolling operation is the same as step 12, except that in step 3, the sodium montmorillonite, hypochlorite, calcium chloride and chlorate are added in the form of dry mixing; the weight ratio of the hypochlorite, calcium chloride and chlorate is 1:0.8:0.2; the total weight of the hypochlorite, calcium chloride and chlorate is equivalent to 2wt% of the weight of the montmorillonite;

[0106] Step 4: Mix the probiotics, enzymes and the mixture obtained in step 3 at 50° C. for 2 hours; the probiotics are yeast, Lactobacillus acidophilus, and Bacillus subtilis; the above bacteria are added in the form of dry powder, and the weight ratio of each bacterial powder is 1:1:1; the weight of the probiotics is equivalent to 6wt% of the weight of the mixture obtained in step 3; the enzyme is glucose oxidase; the weight of the glucose oxidase is equivalent to 2wt% of the weight of the mixture obtained in step 3.

[0107] Example 2

[0108] The preparation method of modified montmorillonite comprises the following steps:

[0109] Step 1: preparing sodium montmorillonite;

[0110] Step 1 is as follows:

[0111] Step 11: heating the montmorillonite at 450° C. for 2.5 h;

[0112] Step 12: adding an aqueous solution containing a soluble sodium salt to the montmorillonite and rolling it at 70° C.;

[0113] The aqueous solution containing soluble sodium salt contains sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose; the mass ratio of sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose is 60:20:10:5:5;

[0114] The solute concentration of the aqueous solution containing the soluble sodium salt is 4wt%;

[0115] The specific operation of rolling is the same as that of Example 1;

[0116] Step 13: aging the montmorillonite obtained in step 12 at room temperature for 3 days to obtain sodium montmorillonite;

[0117] Step 2: Modifying sodium montmorillonite with cyclodextrin and organic acid;

[0118] Step 2 is as follows:

[0119] Step 21: adding cyclodextrin and citric acid to the polyvinyl alcohol solution to prepare a dextrin modifier;

[0120] The weight ratio of the cyclodextrin and the organic acid is 6:4; the polyvinyl alcohol concentration of the polyvinyl alcohol solution is 0.8wt%; the molecular weight of the polyvinyl alcohol is 200000; the total concentration of the cyclodextrin and the organic acid in the dextrin modifier is 3wt%;

[0121] Step 22: adding the dextrin modifier to the sodium montmorillonite and rolling at 75° C.;

[0122] For rolling operation, refer to step 12;

[0123] The dextrin modifier is equivalent to 30wt% of the weight of montmorillonite and is added in the form of spraying, and the spraying and rolling are carried out simultaneously;

[0124] Step 23: Dry the product of step 22 at 85°C for more than 6 hours, then grind the solid dry product and pass it through a 200-mesh sieve.

[0125] Step 3: rolling and mixing the sodium montmorillonite, hypochlorite, calcium chloride and chlorate obtained in step 2; the rolling operation is the same as step 12, except that in step 3, the sodium montmorillonite, hypochlorite, calcium chloride and chlorate are added in the form of dry mixing; the weight ratio of the hypochlorite, calcium chloride and chlorate is 1:1.2:0.4; the total weight of the hypochlorite, calcium chloride and chlorate is equivalent to 3wt% of the weight of the montmorillonite;

[0126] Step 4: Mix the probiotics, enzymes and the mixture obtained in step 3 at 50°C for 2h; the probiotics are yeast, Lactobacillus acidophilus, and Bacillus subtilis; the above bacteria are added in the form of dry powder, and the weight ratio of each bacterial powder is 1:1:1; the weight of the probiotics is equivalent to 6wt% of the weight of the mixture obtained in step 3; the enzyme is glucose oxidase; the weight of the glucose oxidase is equivalent to 1.5wt% of the weight of the mixture obtained in step 3.

[0127] Comparative Example 1

[0128] The method is substantially the same as Example 1, except that the aqueous solution containing soluble sodium salt used in step 12 contains sodium chloride, sodium bicarbonate, sodium sulfate, and sodium butyrate; and the mass ratio of the sodium chloride, sodium bicarbonate, sodium sulfate, and sodium butyrate is 50:20:20:10.

[0129] Comparative Example 2

[0130] The method is substantially the same as Example 1, except that cyclodextrin is not used in step 21; cyclodextrin powder is added to montmorillonite in the form of an additive after step 4, and mixed and dried.

[0131] Performance Testing

[0132] Testing items include swelling capacity and mycotoxin adsorption rate;

[0133] 1. The method for detecting expansion capacity is:

[0134] Prepare the sample and solution: Weigh 1.000 g of sample and add 30-40 ml of distilled water into a 100 ml stoppered measuring cylinder, then add water to the 75 ml mark.

[0135] Mix and shake well: Cover the stopper tightly and shake for 3 minutes to disperse the sample thoroughly and mix it with water. Observe it in a bright place and make sure there are no obvious clumps of particles.

[0136] Add hydrochloric acid solution: open the stopper, add 25 ml of 1N hydrochloric acid solution, then close the stopper and shake for 1 minute.

[0137] Standing and reading: Place the measuring cylinder on a non-vibrating table and let it stand for 24 hours. Read the scale value at the sediment interface, which is the expansion capacity, expressed in ml / g sample.

[0138] The detection method for the adsorption rate of mycotoxins is: refer to NY / T 3803-2020 Determination of 37 mycotoxins in feed by liquid chromatography-tandem mass spectrometry.

[0139] The test results can be found in Tables 1 and 2;

[0140] Table 1 Expansion capacity results

[0141] Expansion Capacity CON 7.3 Example 1 17.6 Example 2 18.5 Example 3 18.2 Comparative Example 1 15.6 Comparative Example 2 16.4

[0142] Table 2 Mycotoxin adsorption rate

[0143]

[0144]

[0145] Note: CON is calcium montmorillonite.

[0146] Result analysis:

[0147] It can be seen from the results in Table 1 and Table 2 that the product of the present invention has significant advantages in terms of expansion capacity and mycotoxin adsorption rate. We believe that the generation of this advantage is closely related to the following factors: sodium-based modification of montmorillonite, cyclodextrin modification, and the use of repeated rolling to increase the specific surface area of ​​montmorillonite;

[0148] By comparing Comparative Example 1 with Comparative Example 2, it can be seen that the modification with glucose and the modification with cyclodextrin are important guarantees for improving the adsorption efficiency. The reason is that the glucose molecules bind to the surface of montmorillonite through ion exchange, covalent bonds or non-covalent interactions, changing its surface properties, such as improving the adsorption efficiency of specific pollutants, and reacting with the cations (such as Na + , Ca 2+ etc.) are exchanged, thereby inserting into the interlayer of montmorillonite, increasing the interlayer distance and improving its adsorption capacity;

[0149] Cyclodextrin additionally gives montmorillonite excellent coating ability for various substances. Through rolling modification, it can not only coat the effective ingredients it contains, but also can firmly and tightly coat hydrophobic toxins in the hydrophobic cavity, thereby further improving the adsorption capacity of montmorillonite.

[0150] Application evaluation experiment:

[0151] 1000 500-day-old Hy-Line Brown late-laying hens were selected, with a pre-test period of 7 days and a full test period of 90 days. The experiment used a three-layer full-step cage, with 5 chickens in each cage. The chicken house is semi-open, combined with natural light (16 hours / day, controlled by an intelligent light controller) and artificial light supplementation, and ventilation adopts a combination of natural and longitudinal negative pressure to maintain a house temperature of 25±2℃ and a humidity of 50% to 60%. Feed three times a day at 7:00, 14:00 and 17:30, and the chickens can eat and drink freely. Use a manure scraper to clean feces once a day. During the trial, eggs were collected at 16:30 every day, and the number of eggs laid, the number of soft and broken eggs, and the egg weight of each chicken were recorded. The weekly feed intake of each group and each repetition was measured every week. The egg production rate, soft and broken egg rate, average egg weight, average daily feed intake and feed efficiency were calculated. On the 60th day of the experiment, 20 egg samples were randomly taken from each repetition for egg analysis. On the 60th day, one chicken was randomly selected from each replicate. After fasting for 12 hours, 5 ml of blood was collected from the subwing vein. After standing for 30 minutes, the blood was centrifuged (3500 rpm, 15 minutes) and the supernatant was collected and stored at -20°C for serum antioxidant index detection. At the same time, intestinal samples were collected for bacterial count detection and QPCR analysis.

[0152] The diet formula can be seen in Table 3;

[0153] Table 3 Diet formula

[0154]

[0155]

[0156] The effects on production performance in the late egg-laying period can be seen in Table 4;

[0157] Table 4 Production performance in the late egg-laying period

[0158]

[0159] Compared with the control group (CON, calcium montmorillonite), the egg production rate of the supplemented group was significantly increased (P<0.05), and the rate of soft eggs was significantly reduced.

[0160] The effects on egg quality in the late laying period of laying hens can be seen in Table 5;

[0161] Table 5 Egg quality results of laying hens in the late laying period

[0162]

[0163] Eggshell strength and Haugh unit showed an increasing trend (P<0.10)

[0164] The effects of serum antioxidant capacity can be seen in Table 6 ;

[0165] Table 6 Serum antioxidant capacity results

[0166]

[0167] The expression level of ileal claudin is visible Figure 1 , Figure 1 It can be seen that the added group can increase the expression levels of tight proteins of the three types of ileum junctions.

[0168] The results of ileal bacteria detection can be seen in Table 7;

[0169] Table 7 Ileobacteria detection results

[0170]

[0171] Compared with the control group, the number of lactic acid bacteria in the intestines of laying hens in each experimental group increased (P<0.05), while the number of Escherichia coli and Salmonella decreased (P<0.05).

[0172] The applicant declares that the present invention illustrates the process method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned process steps, and it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing modified montmorillonite, characterized in that: The steps include: Step 1: preparing sodium montmorillonite using montmorillonite, soluble sodium salt and glucose as raw materials; Step 2: Modifying sodium montmorillonite with cyclodextrin and organic acid; Step 3: Mixing the sodium montmorillonite, hypochlorite and chlorate obtained in step 2; Step 4: Mix the probiotics and enzymes with the mixture obtained in step 3.

2. The preparation method according to claim 1, characterized in that: The step 1 is specifically as follows: Step 11: heating the montmorillonite at 350-450° C. for activation; Step 12: adding an aqueous solution containing soluble sodium salt and glucose to the montmorillonite, and rolling at 70-90° C.; Step 13: Aging the montmorillonite obtained in step 12 at room temperature for 2 to 6 days to obtain sodium montmorillonite.

3. The preparation method according to claim 2, characterized in that: The aqueous solution containing soluble sodium salt contains sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose; the mass ratio of sodium chloride, sodium bicarbonate, sodium sulfate, sodium butyrate and glucose is 40-60:10-20:10-20:5-10:5-10; The solute concentration of the aqueous solution containing the soluble sodium salt is 3 to 5 wt%; The aqueous solution containing soluble sodium salt is equivalent to 10-30wt% of the weight of montmorillonite; The aqueous solution containing the soluble sodium salt is sprayed onto the montmorillonite in the form of a spray.

4. The preparation method according to claim 1, characterized in that: The step 2 is specifically as follows: Step 21: adding cyclodextrin and organic acid into the polyvinyl alcohol solution to prepare a dextrin modifier; Step 22: adding a dextrin modifier to the sodium montmorillonite and rolling the mixture at 70 to 90° C.; Step 23: Dry the product of step 22.

5. The preparation method according to claim 1, characterized in that: The organic acid is one or more of citric acid, succinic acid, and fumaric acid; the weight ratio of the cyclodextrin to the organic acid is 40-60:40-60; The concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 0.5-1wt%; The total concentration of cyclodextrin and organic acid in the dextrin modifier is 2 to 6 wt %; The dextrin modifier is equivalent to 10-30wt% of the weight of montmorillonite; The dextrin modifier is sprayed onto the montmorillonite in the form of a spray.

6. The preparation method according to claim 1, characterized in that: The step 3 is specifically as follows: Mixing hypochlorite, chlorate, calcium chloride and montmorillonite by rolling; The weight ratio of the hypochlorite, calcium chloride and chlorate is 1:0.8-1.2:0.2-0.4; The total weight of the hypochlorite, calcium chloride and chlorate is equivalent to 1-3 wt% of the weight of montmorillonite.

7. The preparation method according to claim 1, characterized in that: The probiotics are one or more combinations of yeast, Lactobacillus acidophilus, and Bacillus subtilis; The probiotics are added to the mixture obtained in step 3 in the form of dry powder; The weight of the probiotics is equivalent to 5-10 wt % of the weight of the mixture obtained in step 3.

8. The preparation method according to claim 1, characterized in that: The enzyme is glucose oxidase; the weight of the glucose oxidase is equivalent to 0.5-2wt% of the weight of the mixture obtained in step 3.

9. A modified montmorillonite, characterized in that: The method is prepared by any one of claims 1 to 8.

10. Use of the modified montmorillonite as claimed in claim 9 in preparing feed additives for aged laying hens.

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