LU502824B1 - Chitosan-copper-loaded montmorillonite intercalation composite material and preparation method and application - Google Patents
Chitosan-copper-loaded montmorillonite intercalation composite material and preparation method and application Download PDFInfo
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- LU502824B1 LU502824B1 LU502824A LU502824A LU502824B1 LU 502824 B1 LU502824 B1 LU 502824B1 LU 502824 A LU502824 A LU 502824A LU 502824 A LU502824 A LU 502824A LU 502824 B1 LU502824 B1 LU 502824B1
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- chitosan
- copper
- loaded montmorillonite
- loaded
- intercalation
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- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 174
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 239000010949 copper Substances 0.000 title claims abstract description 145
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 130
- 239000002131 composite material Substances 0.000 title claims abstract description 112
- 238000009830 intercalation Methods 0.000 title claims abstract description 87
- 230000002687 intercalation Effects 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 122
- 229920001661 Chitosan Polymers 0.000 claims abstract description 94
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 47
- 208000022559 Inflammatory bowel disease Diseases 0.000 claims abstract description 8
- 239000003674 animal food additive Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 17
- 239000011148 porous material Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000013329 compounding Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims 1
- 206010012735 Diarrhoea Diseases 0.000 abstract description 27
- 230000000694 effects Effects 0.000 abstract description 22
- 241000282887 Suidae Species 0.000 abstract description 18
- 230000002265 prevention Effects 0.000 abstract description 9
- 230000002195 synergetic effect Effects 0.000 abstract description 7
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 230000008439 repair process Effects 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000001142 anti-diarrhea Effects 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 57
- 238000012360 testing method Methods 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 29
- 150000001875 compounds Chemical class 0.000 description 28
- 239000002244 precipitate Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 230000001225 therapeutic effect Effects 0.000 description 10
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 9
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 9
- 229910021642 ultra pure water Inorganic materials 0.000 description 9
- 239000012498 ultrapure water Substances 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 5
- 230000003449 preventive effect Effects 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 241000282898 Sus scrofa Species 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000002361 compost Substances 0.000 description 4
- 235000005911 diet Nutrition 0.000 description 4
- 230000037213 diet Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000003115 biocidal effect Effects 0.000 description 3
- 239000002778 food additive Substances 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000011217 control strategy Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000035622 drinking Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000014102 seafood Nutrition 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 208000035473 Communicable disease Diseases 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000004596 appetite loss Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003640 drug residue Substances 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000003832 immune regulation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 210000005027 intestinal barrier Anatomy 0.000 description 1
- 230000004673 intestinal mucosal barrier function Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 235000021266 loss of appetite Nutrition 0.000 description 1
- 208000019017 loss of appetite Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000015816 nutrient absorption Nutrition 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 108700012359 toxins Proteins 0.000 description 1
Classifications
-
- 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
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
-
- 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
- A23K50/60—Feeding-stuffs specially adapted for particular animals for weanlings
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
- A61K31/716—Glucans
- A61K31/722—Chitin, chitosan
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/34—Copper; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/12—Antidiarrhoeals
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- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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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
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Abstract
The invention discloses a chitosan-copper-loaded montmorillonite intercalation composite material and preparation method and application. Chitosan-Cu-loaded montmorillonite powder is used as the main material of intercalation, and chitosan is used for intercalation, in which the copper content of Cu-loaded montmorillonite powder is 0.5 percent-5 percent and the molecular weight of chitosan is 10-50 kDa. The chitosan-copper-loaded montmorillonite powder intercalation composite material disclosed by the invention has a large specific surface area, adopts copper-loaded montmorillonite powder as the main body of the intercalation composite material, utilizes chitosan for intercalation fusion, and combines chitosan with antibacterial, astringent, mucosal repair and immune enhancement activities with copper-loaded montmorillonite powder with adsorption, antidiarrheal and antibacterial effects, so that the two materials are synergistic, can be better used for prevention and control of porcine inflammatory bowel diseases, and can reduce diarrhea rate of weaned piglets and adult pigs to 20 percent.
Description
DESCRIPTION LU502824 CHITOSAN-COPPER-LOADED MONTMORILLONITE INTERCALATION
TECHNICAL FIELD The invention relates to the technical field of feed additives, in particular to a chitosan-copper- loaded montmorillonite intercalation composite material and a preparation method and application.
BACKGROUND Inflammatory Bowel Disease (IBD) is widespread in recent years, and its etiology is complex, and its prevention and control are difficult, which seriously threatens the safety of China's pig industry. Generally, it is mainly infectious diseases caused by bacteria and viruses, including swine epidemic diarrhea, dysentery, infectious gastroenteritis, etc. The main manifestation is diarrhea, accompanied by symptoms such as increased body temperature, loss of appetite, dehydration, etc, which causes slow growth of pigs, decreased feed remuneration, decreased production performance, and even caused the death of pigs, seriously affecting the economic benefits of the breeding industry. Antibiotic-dependent prevention and control strategies have caused serious ecological problems such as antibiotic residues and increased bacterial resistance. It is urgent to develop a green and ecological prevention and control strategy that does not depend on antibiotics.
SUMMARY The purpose of the present invention is to provide a chitosan-copper-loaded montmorillonite intercalation composite material, as well as its preparation method and application in feed additives and pig feeds for preventing or treating porcine inflammatory bowel disease.
The purpose of the invention is realized by the following technical scheme: A technical scheme of the invention provides a chitosan-copper-loaded montmorillonite intercalation composite material, the intercalated composite material adopts copper-loaded montmorillonite powder as the main material of intercalation, and chitosan is used for intercalation compounding. The two materials cooperate with each other to play a synergistic role, which is safe and reliable.
Preferably, the copper content of the copper-loaded montmorillonite powder is 0.5%-5%, and the molecular weight of the chitosan is 10-50 kDa.
The copper content selected by the invention can ensure the antibacterial activity of copper//502824 reduce the copper content, and avoid the obstacle of nutrient absorption in feed and the accumulation of copper in pigs caused by high copper content. Chitosan with specific molecular weight is selected because chitosan with too low molecular weight has toxicity, while chitosan with too high molecular weight has lower anti-inflammatory activity.
Preferably, the pore diameter of the intercalated composite material is 5-100 pm.
Preferably, the expansion index of the intercalation composite material is 60-95%.
Preferably, the bulk density of the intercalation composite material is 0.3-1 g/em*.
Another technical scheme of the present invention provides a preparation method of the chitosan-copper-loaded montmorillonite intercalation composite material, which comprises the following steps: Dispersing montmorillonite into Cu**-containing solution, adjusting pH value to acidity, heating, stirring, centrifuging, precipitating, drying, and grinding to obtain copper-loaded montmorillonite powder, and preparing the copper-loaded montmorillonite powder into suspension; adding chitosan solution with pH value of 4-6, heating, stirring, filtering and drying to obtain chitosan-copper-loaded montmorillonite intercalation composite material.
Preferably, the mass ratio of chitosan to copper-loaded montmorillonite powder is (1-4):(1- 4).
Preferably, the concentration of copper-loaded montmorillonite suspension is 2-6%, and the concentration of chitosan solution is 1-5%.
Preferably, the solvent of the copper-loaded montmorillonite powder suspension is tertiary water, and the copper-loaded montmorillonite powder suspension is allowed to stand overnight to fully swell.
Preferably, the concentration of the Cu** solution is 0.005-0.05 mol/L.
Preferably, the mass-volume ratio of montmorillonite to Cu** solution is 10 g:200 mL.
Preferably, the heating and stirring temperature is 60-65°C and the time is 6 h.
Preferably, the rotating speed of the centrifugation is 3000 rpm and the time is 20 minutes.
Preferably, the copper-loaded montmorillonite powder used to prepare the suspension is powder with a 300-mesh sieve.
Preferably, montmorillonite is dispersed into the solution containing Cu”*, and then the pED502824 value is adjusted to 5.5.
Preferably, the chitosan solution uses 2% acetic acid solution to adjust the pH value.
Preferably, the adding speed is 20-60 drops/min.
Too slow dropping speed prolongs the preparation time and affects the preparation efficiency; if the dripping speed is too fast, the medicine cannot be fully dispersed, which affects the efficacy.
Another technical scheme of the present invention is to provide an application of the chitosan- copper-loaded montmorillonite dispersed intercalation composite material in a feed additive for preventing or treating porcine inflammatory bowel disease.
Another technical scheme of the present invention is to provide a pig feed which contains the chitosan-copper-loaded montmorillonite intercalation composite material.
Compared with the prior art, the invention has the advantages that: The chitosan used in the invention is extracted from the by-products of seafood processing such as shrimp and crab, and has strong mucosal repair activity and immune regulation function. As a functional biomaterial, it has inherent biocompatibility and biodegradability, no toxicity to biological tissues, antibacterial and anti-tumor activities, polyelectrolyte reaction functional groups, certain gel-forming capacity, high adsorption capacity and biodegradability, and is listed as a coating agent (GB-2760) that can be used for national food additives. Copper-loaded montmorillonite powder is a layered mineral composed of water-containing aluminosilicate with extremely fine particles. Its unique crystal structure has adsorption and antibacterial effects on bacteria, viruses and various toxins, and has certain protective effect on the intestinal mucosal barrier of animals.
According to the invention, chitosan and copper-loaded montmorillonite powder are intercalated and compounded, the copper-loaded montmorillonite powder is used as the main material of intercalation, and chitosan is used for intercalation and compounding, so that the antibacterial, astringent, mucosal repair and immune enhancement activities of chitosan are combined with the functions that the copper-loaded montmorillonite can absorb toxic and harmful substances and resist bacteria on the premise of not destroying the biological activities of the two. The prepared chitosan-copper-loaded montmorillonite intercalation composite material can be mixed in that daily ration, lay a foundation for the green and ecological prevention and control of porcine inflammatory bowel disease, is also an effective method for solving the high-valh/502824 utilization of the by-products of seafood processing, is an important way for promote the development of marine economy, and has obvious ecological, social and economic benefits.
The chitosan-copper-loaded montmorillonite powder intercalation composite material of the invention integrates the characteristics of chitosan and copper-loaded montmorillonite powder such as antibiosis, convergence, mucosa repair, immune enhancement and antidiarrheal, and forms a synergistic effect. It has a good preventive and/or therapeutic effect on porcine inflammatory bowel disease, can reduce the diarrhea rate of weaned piglets and adult pigs to 10%, improve the growth efficiency of pigs, and can be widely used in the field of feed additives. In addition, the used raw materials are cheap and easily available, and have no residue, drug resistance and toxic side effects.
BRIEF DESCRIPTION OF THE FIGURES Fig. 1 is the SEM image of copper-loaded montmorillonite powder in the preparation process of Example 1.
Fig. 2 is the SEM image of chitosan-copper-loaded montmorillonite intercalation composite prepared in Example 1.
DESCRIPTION OF THE INVENTION Now, various exemplary embodiments of the present invention will be described in detail. This detailed description should not be taken as a limitation of the present invention, but should be understood as a more detailed description of some aspects, characteristics and embodiments of the present invention. It should be understood that the terms mentioned in the present invention are only used to describe specific embodiments, and are not used to limit the present invention.
In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Every smaller range between any stated value or the intermediate value within the stated range and any other stated value or the intermediate value within the stated range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded from the range.
Unless otherwise stated, all technical and scientific terms used herein have the same meanings commonly understood by those of ordinary skill in the field to which this invention relates.
Although the present invention only describes preferred methods and materials, any methods addJ502824 materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
Example 1 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 10 kDa.
The preparation method comprises the following steps: S1, weigh 10 g montmorillonite, disperse it into 200 mL CuSO4 (0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with a 300-mesh sieve, take 5 g of the sieved fine powder, and add 10% water.
S2, take 5 g of chitosan, dissolve it in 100 mL of water, adjust the pH to 4 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 20 drops/min, heat it to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite material.
When the mass ratio of chitosan to Cu-loaded montmorillonite powder is 1:1, the swelling index of chitosan-Cu-loaded montmorillonite powder intercalation composite is 86.3%, the pore diameter is 12.8+0.9 um, and the bulk density is 0.54+0.11 g/cm’.
Example 2 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 10 kDa.
The preparation method comprises the following steps: S1, weigh 10 g montmorillonite, disperse it into 200 mL CuSO4(0.005 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight,
then grind it into fine powder, sieve it with 300 mesh sieve, take 5 g of the sieved fine powder, and)502824 add water.
S2, take 5 g of chitosan, dissolve it in 100 mL of water, adjust the pH to 4 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 20 drops/min, heat to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 1:1, the expansion index of chitosan-copper-loaded montmorillonite powder intercalation composite is
88.3%, the pore diameter is 12.9+0.9 um, and the bulk density is 0.56+0.11 g/cm’.
Example 3 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 50 kDa.
The preparation method comprises the following steps: S1, weigh 10 g of montmorillonite, disperse it into 200 mL of CuSO4(0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 60°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with 300 mesh sieve, take 5 g of the sieved fine powder, and add 20% water.
S2, take 5 g of chitosan, dissolve it in 500 mL of water, adjust the pH to 6 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 60 drops/min, heat to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.8, and dry for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 1:1, the expansion index of chitosan-copper-loaded montmorillonite powder intercalation composite is
78.1%, the pore diameter is 8.8+1.0 um, and the bulk density is 0.39+0.11 g/cm’.
Example 4
A kind of chitosan-copper-loaded montmorillonite powder intercalation composite materidly502824 which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 10 kDa.
The preparation method comprises the following steps: S1, weigh 10 g montmorillonite, disperse it into 200 mL CuSO4(0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with a 300-mesh sieve, take 5 g of the sieved fine powder, and add 10% water.
S2, take 20 g of chitosan, dissolve it in 400 mL of water, adjust the pH to 4 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 20 drops /min, heat it to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite material.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 4:1, the expansion index of chitosan-copper-loaded montmorillonite powder intercalation composite is
95.3%, the pore diameter is 14.8+0.8 um, and the bulk density is 0.45+0.12 g/cm’.
Example 5 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 30 kDa.
The preparation method comprises the following steps: S1, weigh 10 g of montmorillonite, disperse it into 200 mL of CuSO4(0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with 300 mesh sieve, take 5g of the sieved fine powder, and add 20% water.
S2, take 20 g of chitosan, dissolve it in 1200 mL of water, adjust the pH to 5 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 40 drops/min, heat it to 65°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hout$/502824 to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 4:1, the swelling index of chitosan-copper-loaded montmorillonite powder intercalation composite is 90.3%, the pore diameter is 12.9+0.9 um, and the bulk density is 0.55+0.09 g/cm’.
Example 6 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 50 kDa.
The preparation method comprises the following steps: S1, weigh 10 g of montmorillonite, disperse it into 200 mL of CuSO4(0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 60°C, stir it for 6 hours, centrifuge it at 3000 rpm for 20 minutes to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with 300 mesh sieve, take 5 g of the sieved fine powder, and add 20% water.
S2, take 20 g of chitosan, dissolve it in 2000 mL of water, adjust the pH to 6 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 60 drops/min, heat it to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 4:1, the expansion index of chitosan-copper-loaded montmorillonite powder intercalation composite is
86.8%, the pore diameter is 11.5+1.1 um, and the bulk density is 0.62+0.11 g/cm’.
Example 7 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 10 kDa.
The preparation method comprises the following steps: S1, weigh 40 g of montmorillonite, disperse it into 400 mL of CuSO4 (0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, and centrifuge it at 3000 rpm for 20 min to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70 CU502824 overnight, then grind it into fine powder, sieve it with a 300-mesh sieve, take 20 g of the sieved fine powder and add water.
S2, take 5 g of chitosan, dissolve it in 100 mL of water, adjust the pH to 4 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 20 drops/min, heat it to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite material.
When the mass ratio of chitosan to Cu-loaded montmorillonite powder is 1:4, the swelling index of chitosan-Cu-loaded montmorillonite powder intercalation composite is 80.2%, the pore diameter is 10.8+0.9 um, and the bulk density is 0.48+0.12 g/cm’.
Example 8 A kind of chitosan-copper-loaded montmorillonite powder intercalation composite material, which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 30 kDa.
The preparation method comprises the following steps: S1, weigh 40 g of montmorillonite, disperse it into 800 mL of CuSO4 (0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 65°C, stir it for 6 hours, and centrifuge it at 3000 rpm for 20 min to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with a 300-mesh sieve, take 20 g of the sieved fine powder and add water.
S2, take 5 g of chitosan, dissolve it in 300 mL of water, adjust the pH to 5 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 40 drops /min, heat it to 65°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry it for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to Cu-loaded montmorillonite powder is 1:4, the swelling index of chitosan-Cu-loaded montmorillonite powder intercalation composite is 69.2%, the pore diameter is 9.4+0.9 um, and the bulk density is 0.42+0.08 g/cm’.
Example 9
A kind of chitosan-copper-loaded montmorillonite powder intercalation composite materidlJ502824 which uses copper-loaded montmorillonite powder as the main material of intercalation, and uses chitosan for intercalation compound. The molecular weight of chitosan is 50 kDa.
The preparation method comprises the following steps: S1. weigh 40 g of montmorillonite, disperse it into 1000 mL of CuSO4(0.05 mol/L) solution, adjust the pH value to 5.5, heat it to 60°C, stir it for 6 hours, and centrifuge it at 3000 rpm for 20 min to get a precipitate, wash it with distilled water for 3 times, dry the precipitate at 70°C overnight, then grind it into fine powder, sieve it with a 300-mesh sieve, take 20 g of the sieved fine powder, and add water.
S2, take 5 g of chitosan, dissolve it in 500 mL of water, adjust the pH to 6 with 2% acetic acid solution, drop the chitosan acetic acid solution into the copper-loaded montmorillonite suspension in S1 at a speed of 60 drops/min, heat to 60°C, stir for 6 hours, filter, wash the formed composite with ultrapure water until the pH of the washing solution is 6.5, and dry for 12 hours to obtain the chitosan-copper-loaded montmorillonite intercalation composite.
When the mass ratio of chitosan to copper-loaded montmorillonite powder is 1:4, the expansion index of chitosan-copper-loaded montmorillonite powder intercalation composite is
65.2%, the pore diameter is 8.8+1.2 um, and the bulk density is 0.29+0.12 g/cm’.
Example 10 Compared with Example 4, the step of copper loading on montmorillonite is omitted, and the dosage of other reagents and the preparation method are the same.
When the mass ratio of chitosan to montmorillonite powder is 4:1, the expansion index of chitosan-montmorillonite powder composite is 87.5%, the pore diameter is 13.2+0.9 um, and the bulk density is 0.50+0.08 g/cm’.
Fig. 1 is the SEM image of the copper-loaded montmorillonite powder obtained by drying the copper-loaded montmorillonite suspension prepared in S1 during the preparation of Example
1.
As can be seen from Figure 1, the interlayer spacing of montmorillonite before intercalation is small and the layer wall is thick.
Fig. 2 is the SEM image of chitosan-copper-loaded montmorillonite intercalation composite prepared in Example 1.
It can be seen from Figure 2 that after intercalation, the interlayer spacing of montmorillonité/502824 powder obviously increases and the layer wall becomes thinner.
Result detection
1. Application in weaned piglets (1) Preventive effect test method: 280 weaned piglets were selected and divided into 14 groups, one of which was a blank control group, one of which was a common control group, three of which were comparative groups, and the rest were experimental groups. The control group and the common control group were fed with common feed. The feed of the comparative group was fed with chitosan, copper-loaded montmorillonite and chitosan-montmorillonite powder composite respectively, while the feed of the experimental group was fed with chitosan-copper-loaded montmorillonite powder intercalation composite granular feed additives with different mass ratios. The feeding method was free drinking and eating. After 24 hours, the normal control group, the comparative group and the experimental group were inoculated with Escherichia coli, while the blank control group was not inoculated. The illness situation was recorded for 120 hours.
(2) Test results: The test groups, feed types and test results are shown in Table 1. In comparative proportion 1, only 0.3% chitosan was added to the diet, and copper-loaded montmorillonite powder was not added. Comparative proportion 2 is that only 0.3% Cu-loaded montmorillonite powder is added to the diet, and chitosan is not added; comparative proportion 3 is to add 0.3% chitosan- montmorillonite powder composite prepared in Example 10 to the diet; In the test group, 0.3% chitosan-copper-loaded montmorillonite composite prepared in different mass ratios of Examples 1-9 was added to the diet as an additive, and chitosan-montmorillonite composite additive was added.
Table 1 LU502824 Diarrhea rate Group Feed Feed additive (%) Ordi trol | OS EE | comm | w group Comparative i | Common feed Chitosan 70 proportion 1 C ti C -loaded Om para ve Common feed OPper oa © 50 proportion 2 montmorillonite powder C ti E le 10 it ompara ve Common feed xample compost © 55 proportion 3 material E le 1 it material E le 2 it material Example 3 composite Test group 3 Common feed ; 35 material Example 4 composite Test group 4 Common feed ; 20 material Example 5 composite Test group 5 Common feed ; 20 material Example 6 composite Test group 6 Common feed ; 30 material Example 7 composite Test group 7 Common feed ; 35 material Example 8 composite Test group 8 Common feed ; 30 material Example 9 composite material From the above results, it can be seen that the compound feed additive of the present invention has obvious effect on preventing piglet diarrhea, and the diarrhea rate of piglets added with the compound feed additive is reduced by at least 40% compared with the common control group.
Compared with single addition of chitosan, copper-loaded montmorillonite powder or chitosan- montmorillonite powder composite materials, the effect of adding compound feed additives on preventing piglet diarrhea is more obvious.
When the mass ratio of chitosan to montmorillonite powder is 4:1, the granular feed additive has the most obvious preventive effect on piglet diarrhea,
and the effect of using copper-loaded montmorillonite powder is obviously better thad502824 montmorillonite powder.
The above results show that the components in the compound feed additive of the present invention have synergistic effect, which is better than the prevention effect of adding chitosan or copper-loaded montmorillonite powder alone. Moreover, the compound feed additive made of chitosan and copper-loaded montmorillonite with a mass ratio of 4:1 has the best effect and the most obvious prevention effect on piglet diarrhea.
(3) Therapeutic effect test method: 300 weaned piglets were inoculated with Escherichia coli and fed with common feed. After 48 hours, 260 piglets with diarrhea symptoms were selected and divided into 13 groups. One group is a blank control group, three groups are comparative groups, and the rest groups are experimental groups. The control group was fed with common feed, while the comparative group was fed with
0.5% chitosan, 0.5% copper-loaded montmorillonite and 0.5% chitosan-montmorillonite powder composite, while the experimental group was fed with 0.5% chitosan-copper-loaded montmorillonite powder intercalation composite granular feed additives with different mass ratios. The feeding methods were free drinking and eating, and the treatment conditions were recorded for 120 hours.
(4) Test results: The test groups, feed types and test results are shown in Table 2. In comparative proportion 1, only chitosan was added, but copper-loaded montmorillonite powder was not added. Comparative proportion 2 is that only copper-loaded montmorillonite powder is added, and chitosan is not added; comparative proportion 3 is the addition of chitosan-montmorillonite powder composite prepared in Example 10; in the test group, the chitosan-montmorillonite intercalated composite prepared in different mass ratios of Examples 1-9 was added as an additive, and the chitosan-montmorillonite intercalated composite additive was added.
Table 2 LU502824 Diarrhea rate Group Feed Feed additive (%) C ti mes Commonfood | em | 80 proportion 1 C ti C -loaded compara ve Common feed OPDer oa © 45 proportion 2 montmorillonite powder C ti E le 10 it ompara 1Ve Common feed Xample compost Cc 45 proportion 3 material Example 1 composite Test group 1 Common feed ; 40 material Example 2 composite Test group 2 Common feed ; 40 material Example 3 composite Test group 3 Common feed ; 35 material Example 4 composite Test group 4 Common feed ; 25 material Example 5 composite material Example 6 composite material Example 7 composite material Example 8 composite material Example 9 composite material From the above results, it can be seen that the compound feed additive of the present invention has obvious effect on treating piglet diarrhea, and the diarrhea rate of piglets added with the compound feed additive is reduced by at least 55% compared with the blank control group.
Compared with chitosan, copper-loaded montmorillonite powder or chitosan-montmorillonite powder composite, adding compound feed additive has more obvious therapeutic effect on preventing piglet diarrhea.
When the mass ratio of chitosan to montmorillonite powder is 4:1, the granular feed additive has the most obvious therapeutic effect on piglet diarrhea, and the effect of using copper-loaded montmorillonite powder is obviously better than montmorillonite powder.
The above results show that the components in the compound feed additive of the inventidit/502824 have synergistic effect, and the therapeutic effect is better than that of adding chitosan, copper- loaded montmorillonite powder or chitosan-montmorillonite powder composite material alone. Moreover, the compound feed additive made of chitosan and copper-loaded montmorillonite with the mass ratio of 4:1 has the best effect, and the most obvious therapeutic effect on piglet diarrhea.
2. Application in adult pigs (1) Except that the test object is adult pigs and the proportion of dietary additives is reduced to 0.15%, other test methods are the same as the test method of preventive effect of weaned piglets. (2) The test results are shown in Table 3: Table 3 Comparative | Comme | Commonfeod | om | ow proportion 1 C ti C -loaded compara ve Common feed OPDer oa © 45 proportion 2 montmorillonite powder C ti E le 10 it ompara 1Ve Common feed Xample compost © 45 proportion 3 material E le 1 it material E le 2 it material E le 3 ite material Example 4 composite material Example 5 composite material Example 6 composite material Example 7 composite material Example 8 composite Test group 8 Common feed ; 30 material Example 9 composite Test group 9 Common feed ; 35 material
From the above results, it can be seen that the compound feed additive of the present inventid#/502824 has an obvious effect on preventing diarrhea of adult pigs, and the diarrhea rate of piglets added with the compound feed additive is reduced by at least 35% compared with the common control group. Compared with chitosan, copper-loaded montmorillonite powder or chitosan- montmorillonite powder composite, the effect of adding compound feed additives on preventing diarrhea in adult pigs is more obvious. When the mass ratio of chitosan to copper-loaded montmorillonite is 4:1, the granular feed additive has the most obvious preventive effect on diarrhea in adult pigs, and the effect of using copper-loaded montmorillonite powder is obviously better than that of montmorillonite powder. The above results show that the components in the compound feed additive of the present invention have synergistic effect, which is better than the prevention effect of adding chitosan or copper-loaded montmorillonite powder alone. Moreover, the granular feed additive made of chitosan and copper-loaded montmorillonite powder with the mass ratio of 1:4 has the best effect and the most obvious prevention effect on diarrhea of adult pigs.
(3) Except that the test object is adult pigs and the proportion of dietary additives is reduced to 0.2%, other test methods are the same as those of weaned piglets.
(4) The test results are shown in Table 4:
Table 4 LU502824 Diarrh t Group Feed Feed additive tarrhea tale (%) Comparative i ; Common feed Chitosan 70 proportion 1 Comparative Copper-loaded ; Common feed 4 45 proportion 2 montmorillonite powder Comparative Example 10 composite ; Common feed . 45 proportion 3 material Example 1 composite Test group 1 Common feed ; 35 material Example 2 composite Test group 2 Common feed ; 35 material Example 3 composite Test group 3 Common feed ; 30 material Example 4 composite Test group 4 Common feed ; 25 material E le 5 it Test group 5 Common feed ample compost © 20 material E le 6 it material E le 7 it material E le 8 it material E le 9 it material From the above results, it can be seen that the compound feed additive of the present invention has obvious effect on treating diarrhea of adult pigs, and the diarrhea rate of adult pigs added with the compound feed additive is reduced by at least 55% compared with the blank control group.
Compared with chitosan, copper-loaded montmorillonite powder or chitosan-montmorillonite powder composite, the effect of adding compound feed additives on diarrhea in adult pigs is more obvious.
When the mass ratio of chitosan to montmorillonite powder is 4:1, the granular feed additive has the most obvious therapeutic effect on diarrhea in adult pigs, and the effect of using copper-loaded montmorillonite powder is obviously better than that of montmorillonite powder.
The above results show that the components in the compound feed additive of the inventidit)502824 have synergistic effect, and the therapeutic effect is better than that of adding chitosan, copper- loaded montmorillonite powder or chitosan-montmorillonite powder composite material alone. Moreover, the compound feed additive made of chitosan and copper-loaded montmorillonite with the mass ratio of 4:1 has the best therapeutic effect, and the most obvious therapeutic effect on diarrhea of adult pigs.
Obviously, the above-mentioned embodiments of the present invention are only examples to clearly illustrate the present invention, and are not limitations on the embodiments of the present invention. For those of ordinary skill in the art, other changes or variations can be made on the basis of the above description. It is not necessary and impossible to exhaust all the embodiments here. Any modification, equivalent substitution and improvement made within the spirit and principle of the present invention shall be included in the scope of protection of the claims of the present invention.
Claims (9)
1. A chitosan-copper-loaded montmorillonite intercalation composite material, characterized in that the intercalation composite material uses copper-loaded montmorillonite dispersion as the main material of intercalation, and chitosan is used for intercalation compounding.
2. The chitosan-copper-loaded montmorillonite intercalation composite material according to claim 1, characterized in that the copper content of the copper-loaded montmorillonite powder is
0.5%-5%, and the molecular weight of the chitosan is 10-50 kDa.
3. The chitosan-copper-loaded montmorillonite intercalation composite material according to claim 2, characterized in that the pore diameter of the intercalated composite material is 5-100 pm, the expansion index is 60-95%, and the bulk density is 0.3-1 g/cm’.
4. A preparation method of chitosan-copper-loaded montmorillonite intercalation composite material according to any one of claims 1 to 3, characterized by comprising the following steps: dispersing montmorillonite into Cu”’-containing solution, adjusting pH value to acidity, heating, stirring, centrifuging, precipitating, drying, and grinding to obtain copper-loaded montmorillonite powder, and preparing the copper-loaded montmorillonite powder into suspension; adding chitosan solution with pH value of 4-6, heating, stirring, filtering and drying to obtain chitosan-copper-loaded montmorillonite intercalation composite material.
5. The preparation method of chitosan-copper-loaded montmorillonite intercalation composite material according to claim 4, characterized in that the mass ratio of the copper-loaded montmorillonite powder to chitosan is (1-4):(1-4), the concentration of copper-loaded montmorillonite suspension is 2-6%, and the concentration of chitosan solution is 1-5%.
6. The preparation method of chitosan-copper-loaded montmorillonite intercalation composite according to claim 4, characterized in that the concentration of the Cu” solution is
0.005-0.05 mol/L; the temperature of heating and stirring is 60-65 °C and the time is 6 h; the rotating speed of centrifugation 1s 3000 rpm and the time is 20 minutes; the adding speed of the chitosan solution is 20-60 drops/min.
7. The preparation method of chitosan-copper-loaded montmorillonite intercalation composite according to claim 6, characterized in that the mass-volume ratio of montmorillonite to Cu”* solution is 10 g:200 mL.
8. An application of chitosan-copper-loaded montmorillonite intercalation composite material/502824 according to any one of claims 1 to 3 in feed additive for preventing or treating porcine inflammatory bowel disease.
9. A pig feed, characterized by containing the chitosan-copper-loaded montmorillonite intercalation composite material according to any one of claims 1 to 3.
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