Mixed-dimension attapulgite clay-based multifunctional environment regulator for cultivation and preparation method of mixed-dimension attapulgite clay-based multifunctional environment regulator

Abstract

The invention discloses a mixed-dimension attapulgite clay-based multifunctional environment conditioning agent for cultivation and a preparation method thereof, and the preparation method comprises the following steps: putting chlorhexidine acetate or chlorhexidine gluconate modified mixed-dimension attapulgite clay, zeolite, vermiculite, calamine and a plant extract into a powder stirrer, and fully stirring in the process of fully mixing to obtain a mixed-dimension attapulgite clay-based multifunctional environment conditioning agent; the antibacterial liquid is sprayed to the surface of the mixture in a spraying mode, stirring continues to be conducted for 5-30 min, after grinding is conducted through a three-roller grinding machine, the mixed materials are dried, and the dried materials are screened through a 200-mesh sieve. The prepared environment conditioning agent for healthy breeding has the effects of drying, heat preservation, sterilization, disinfection, ammonia removal and deodorization, and can be widely applied to animal environment conditioning and newborn piglet talcum powder.

Description

Technical Field

[0001] The invention relates to an environmental regulator, in particular to a mixed-dimensional attapulgite clay-based multifunctional environmental regulator for breeding and a preparation method thereof, belonging to the technical field of animal breeding. Background Art

[0002] With the development of animal husbandry on a large scale and intensified, people are paying more and more attention to the impact of breeding environment on animals. A good breeding environment can improve the immunity of livestock and poultry and avoid or reduce the occurrence of epidemic diseases. A bad breeding environment will not only affect the health and welfare of animals, causing livestock and poultry to have poor resistance and be susceptible to diseases, and even cause the spread of diseases, but also reduce production efficiency and may have a negative impact on human health and the social environment.

[0003] The main factors affecting the breeding environment are temperature, humidity, air quality, pathogenic microorganisms, etc. During the breeding process, it is necessary to adjust the appropriate temperature and humidity according to the different types of animals to ensure the comfort and health of the animals, ensure good ventilation, and reduce the accumulation of harmful gases (such as ammonia, carbon dioxide) and dust. People often pay more attention to temperature control and ignore the harm caused by humidity. Excessive humidity in the environment can easily cause the reproduction of pathogenic microorganisms, cause parasitic diseases, animal respiratory system and conjunctivitis and other diseases, and cause a significant decrease in the daily weight gain and feed utilization rate of animals; especially young livestock and poultry, whose immune systems are not fully developed, are more sensitive to the impact of the breeding environment.

[0004] Aquaculture environment regulators are healthy aquaculture products that improve production efficiency by improving the aquaculture environment. They can keep the breeding environment dry, improve the sanitation of the pens, especially the delivery room, delivery bed and incubator, inhibit the growth and reproduction of pathogenic microorganisms, and reduce the incidence of diseases. At the same time, they can wipe the whole body of newborn young animals to keep their body surface dry and comfortable. At present, the aquaculture environment regulators used in the domestic market mainly include Misto from OLMIX of France, Baijingbao and Matsong from the United States, Ox from Germany, and Meiko from the Netherlands. Most products are mainly composed of montmorillonite, focusing on the water absorption of the product, ignoring the heat preservation and anti-inflammatory effects on animals and the adsorption of harmful gases such as ammonia. Therefore, it is urgent to develop new mineral functional environment regulators through functional modification and structural regulation to meet market demand.

[0005] Attapulgite is a natural one-dimensional nano-hydrated magnesium-aluminum silicate clay mineral with nanorod-like crystal structure, nanopores and surface active groups. The large pore structure and large specific surface area give it better adsorption performance. It has been included in the feed product catalog and is added to feed to adsorb toxic and harmful substances such as intestinal pathogens, heavy metals, mycotoxins, etc., to protect animal intestinal health and improve animal production performance. At the same time, it has the ability to selectively adsorb polar small molecules such as NH3 and H2O, which can effectively reduce the concentration of ammonia and moisture in the breeding environment.

[0006] Mixed-dimensional attapulgite clay is a special attapulgite clay mineral material. In addition to attapulgite, the main mineral components are also accompanied by illite, chlorite, kaolinite and illite-montmorillonite mixed-layer minerals, etc., showing a structural morphology of nanorods and nanosheets interwoven. The unique rod-sheet interwoven structure and the rich surface silanol active groups make it not only have the characteristics of attapulgite, but also show better multifunctionality. However, the mixed-dimensional attapulgite clay ore is not smooth enough due to its alkalinity (pH is 8-10) and high sand content, and the direct use as an environmental regulator is not effective. To this end, the present invention prepares an environmental regulator with excellent performance by modifying the mixed-dimensional attapulgite clay, assembling antibacterial factors and regulating surface properties. Summary of the invention

[0007] The purpose of the present invention is to address the defects of existing environmental regulators for aquaculture. By assembling antibacterial factors, regulating surface properties and integrating technologies for mixed-dimensional attapulgite clay, a healthy aquaculture environmental regulator with multiple functions such as drying properties, antibacterial and anti-inflammatory properties, and ammonia nitrogen adsorption is provided to provide technical and product support for safe aquaculture.

[0008] The mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture provided by the present invention is prepared by placing modified mixed-dimensional attapulgite clay, zeolite, vermiculite, calamine and plant extract in a powder mixer, spraying an antibacterial liquid on the surface of the mixture in a spraying form during the thorough mixing process, continuing to stir for 5 to 30 minutes, grinding with a three-roll grinder, drying the mixed material, and passing through a 200-mesh sieve to obtain the obtained product; The raw materials are mixed in the following proportions by weight: 70-85 parts of modified mixed-dimensional attapulgite clay, 1-5 parts of zeolite, 3-5 parts of vermiculite, 3-5 parts of plant extract, 3-15 parts of calamine, and 3-10 parts of antibacterial liquid.

[0009] The modified mixed-dimensional attapulgite clay is a modified mixed-dimensional attapulgite clay powder with a mesh size of 200 or more, a water content of ≤10%, and a sand content of ≤2%; the modification method is as follows: 1) Purification of mixed-dimensional attapulgite clay: The crushed mixed-dimensional attapulgite clay is evenly dispersed in an acidic aqueous solution with a pH value of 3-4 and activated for more than 4 hours, and then subjected to hydrocyclone treatment, solid-liquid separation and drying treatment in sequence; 2) Modification of mixed-dimensional attapulgite clay: first dissolve chlorhexidine acetate or chlorhexidine gluconate in an aqueous solution, then add the purified mixed-dimensional attapulgite clay to react at room temperature for 2-4 hours, filter, dry, crush, and pass through a 200-mesh sieve to obtain a clay mineral modified with chlorhexidine acetate or chlorhexidine gluconate.

[0010] The added amount of the chlorhexidine acetate or chlorhexidine gluconate is 3% to 15% of the mass of the mixed-dimensional attapulgite clay.

[0011] The zeolite and vermiculite are both powder materials with a mesh size of 200 or more, a water content of ≤10%, and a sand content of ≤2%.

[0012] The plant extract is mainly one or more of purslane extract, bletilla striata extract, liquorice extract, isatis root extract, codonopsis pilosula extract, astragalus extract, honeysuckle extract and wild chrysanthemum extract.

[0013] The antibacterial liquid is obtained by fully stirring 0.5-2 wt% of organic acid, 4-6 wt% of emulsifier and 1-3 wt% of vegetable oil in hot water at 60-90°C.

[0014] Among them, the organic acid is mainly one or more of benzoic acid, gallic acid, citric acid, and salicylic acid; the emulsifier is mainly one or more of monocaprin, monocaprylin, monolaurin, monomyristic glyceryl, coconut glucoside, glyceryl stearate, monolactic acid glyceryl, and Tween 80; the vegetable oil is mainly one or more of peanut oil, corn oil, sunflower oil, and blended oil.

[0015] The present invention organically combines modified mixed-dimensional attapulgite clay, zeolite, vermiculite, calamine powder, plant extracts, and antibacterial liquid, and develops an environmental regulator for healthy breeding with multiple functions such as drying and smoothing, antibacterial and anti-inflammatory, and ammonia nitrogen adsorption under the synergistic effect of multiple functions. By purifying and modifying the mixed-dimensional attapulgite clay, the adsorption and antibacterial properties of the mixed-dimensional attapulgite clay are improved; the addition of zeolite and vermiculite not only improves the adsorption performance of ammonia, but also plays a good thermal insulation role; the addition of plant extracts can soothe the skin and make animals feel comfortable; at the same time, under the action of mechanical force and chemistry, the natural antibacterial factors of plant extracts are efficiently immobilized and directional adsorbed on the surface in the pores of mixed-dimensional attapulgite clay through physical adsorption and surface chemical bonding; spraying antibacterial liquid on the surface of the mixed mixture will effectively adjust the surface hydrophilicity and hydrophobicity under the action of mechanical force and chemistry, giving the material better smoothness and antibacterial properties; through technical integration, the product can achieve multiple functions such as drying and smoothness, antibacterial and anti-inflammatory, and adsorption of ammonia nitrogen.

[0016] In summary, the environmental conditioner for healthy breeding prepared by the present invention has the functions of drying, heat preservation, sterilization, disinfection, ammonia removal and deodorization, and can be widely used in animal environment regulation and newborn piglet talcum powder. When applied to livestock and poultry pens, the breeding environment can be kept dry and comfortable. When applied to piglet delivery, the skin surface can be quickly dried, the body temperature can be maintained, and the environmental adaptability of newborn piglets can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The water-retention diagram of the environmental conditioning agent prepared in Examples 1-5 of the present invention; Figure 2 The angle of repose diagram of the environmental conditioning agent prepared in Examples 1-5 of the present invention; Figure 3 The adsorption diagram of ammonia gas by the environmental conditioner prepared in Examples 1-5 of the present invention; Figure 4 is the MIC (mg / mL) of the environmental regulator in Examples 1-5 of the present invention against Escherichia coli.

[0018] Figure 5 is the MIC (mg / mL) of the environmental regulator in Examples 1-5 of the present invention against Staphylococcus aureus. DETAILED DESCRIPTION

[0019] The mixed-dimensional attapulgite clay-based aquaculture environmental regulator described in the present invention is further explained below in conjunction with specific embodiments.

[0020] The preparation process of the mixed-dimensional attapulgite clay purified powder used in the following examples is as follows: the crushed mixed-dimensional attapulgite clay is uniformly dispersed in a sulfuric acid aqueous solution with a pH value of 3-4 and activated for 4 hours, and then subjected to hydrocyclone treatment, solid-liquid separation, and drying treatment in sequence and passed through a 200-mesh sieve to obtain.

[0021] Example 1 (1) Modification of mixed-dimensional attapulgite clay: Weigh 4 g of chlorhexidine acetate and dissolve it in 250 mL of water. Add 100 g of purified mixed-dimensional attapulgite clay under stirring and react at room temperature for 4 h. Filter, dry, crush, and pass through a 200-mesh sieve to obtain chlorhexidine acetate-modified mixed-dimensional attapulgite clay.

[0022] (2) Preparation of antibacterial liquid: Add 0.75 wt% benzoic acid, 2 wt% coco-glucoside, 4 wt% lauric acid monoglyceride, and 1 wt% corn oil into 35 wt% hot water at 80 °C and stir well.

[0023] (3) Preparation of environmental regulator: Weigh 70 parts of modified mixed-dimensional attapulgite clay, 5 parts of zeolite, 3 parts of vermiculite, 1 part of purslane extract, 3 parts of licorice extract, and 8 parts of calamine, and place them in a powder mixer. During the thorough mixing process, spray 10 parts of antibacterial liquid on the surface of the mixture in the form of a spray. Continue stirring for 15 minutes. After grinding with a three-roll mill, the mixed materials are dried to remove moisture therein, and the environmental regulator is obtained after passing through a 200-mesh sieve.

[0024] Example 2 (1) Modification of mixed-dimensional attapulgite clay: 3.5 g of chlorhexidine acetate was weighed and dissolved in 250 mL of water. 100 g of purified mixed-dimensional attapulgite clay was added under stirring and reacted at room temperature for 4 h. The mixture was filtered, dried, crushed, and passed through a 200-mesh sieve to obtain chlorhexidine acetate-modified mixed-dimensional attapulgite clay.

[0025] (2) Preparation of antibacterial solution: Add 2 wt% citric acid, 2 wt% Tween 80, 4 wt% monomyristyl glyceride, and 2 wt% peanut oil into 45 wt% hot water at 75°C until fully stirred.

[0026] (3) Preparation of environmental regulator: Weigh 80 parts of modified mixed-dimensional attapulgite clay, 3 parts of zeolite, 5 parts of vermiculite, 2 parts of Bletilla striata extract, 2 parts of Isatis indigotica extract, and 3 parts of calamine, and place them in a powder mixer. During the thorough mixing process, spray 5 parts of antibacterial liquid on the surface of the mixture in the form of a spray. Continue stirring for 10 minutes. After grinding with a three-roll mill, the mixed materials are dried to remove moisture therein, and the environmental regulator is obtained after passing through a 200-mesh sieve.

[0027] Example 3 (1) Modification of mixed-dimensional attapulgite clay: 20 mL of 20 wt% chlorhexidine gluconate was dispersed in 250 ml of water, and 75 g of purified mixed-dimensional attapulgite clay was added under stirring. The mixture was reacted at room temperature for 2 h, filtered, dried, crushed, and passed through a 200-mesh sieve to obtain chlorhexidine gluconate-modified mixed-dimensional attapulgite clay.

[0028] (2) Preparation of antibacterial liquid: Add 1 wt% citric acid, 2 wt% glyceryl stearate, 4 wt% lauric acid monoglyceride, and 3 wt% blending oil into 40 wt% 80°C hot water until fully stirred.

[0029] (3) Preparation of environmental regulator: Weigh 70 parts of modified mixed-dimensional attapulgite clay, 2 parts of zeolite, 3 parts of vermiculite, 3 parts of Portulaca oleracea extract, 2 parts of Chrysanthemum indica extract, and 10 parts of calamine, and place them in a powder mixer. During the thorough mixing process, spray 10 parts of antibacterial liquid on the surface of the mixture in the form of a spray, continue stirring for 10 minutes, grind with a three-roll mill, dry the mixed materials to remove moisture, and pass through a 200-mesh sieve to obtain an environmental regulator.

[0030] Example 4 (1) Modification of mixed-dimensional attapulgite clay: 50 mL of 20 wt% chlorhexidine gluconate was dispersed in 200 ml of water, and 100 g of purified mixed-dimensional attapulgite clay was added under stirring. The mixture was reacted at room temperature for 2 h, filtered, dried, crushed, and passed through a 200-mesh sieve to obtain chlorhexidine gluconate-modified mixed-dimensional attapulgite clay.

[0031] (2) Preparation of antibacterial liquid: Add 1 wt% citric acid, 2 wt% Tween 80, 3 wt% lauric acid monoglyceride, and 2 wt% blending oil into 35 wt% 85°C hot water until fully stirred.

[0032] (3) Preparation of environmental regulator: Weigh 75 parts of modified mixed-dimensional attapulgite clay, 2 parts of zeolite, 3 parts of vermiculite, 1 part of honeysuckle extract, 1 part of wild chrysanthemum extract, 1 part of Codonopsis pilosula extract, 1 part of Astragalus membranaceus extract, and 10 parts of calamine, and place them in a powder mixer. During the thorough mixing process, spray 6 parts of antibacterial liquid on the surface of the mixture in the form of a spray. Continue stirring for 15 minutes. After grinding with a three-roll mill, the mixed materials are dried to remove moisture therein, and passed through a 200-mesh sieve to obtain an environmental regulator.

[0033] Example 5 (1) Modification of mixed-dimensional attapulgite clay: 50 mL of 20 wt% chlorhexidine gluconate was dispersed in 200 ml of water, and 100 g of purified mixed-dimensional attapulgite clay was added under stirring. The mixture was reacted at room temperature for 2 h, filtered, dried, crushed, and passed through a 200-mesh sieve to obtain chlorhexidine gluconate-modified mixed-dimensional attapulgite clay.

[0034] (2) Preparation of antibacterial liquid: Add 0.5 wt% benzoic acid, 2 wt% Tween 80, 3 wt% glyceryl monolactic acid, and 2 wt% blending oil into 35 wt% hot water at 70°C until fully stirred.

[0035] (3) Preparation of environmental regulator: Weigh 70 parts of modified mixed-dimensional attapulgite clay, 2 parts of zeolite, 2 parts of vermiculite, 1 part of honeysuckle extract, 1 part of wild chrysanthemum extract, 1 part of astragalus extract, and 15 parts of calamine, and place them in a powder mixer. During the thorough mixing process, spray 8 parts of antibacterial liquid on the surface of the mixture in the form of a spray. Continue stirring for 30 minutes. After grinding with a three-roll mill, the mixed materials are dried to remove moisture therein, and passed through a 200-mesh sieve to obtain an environmental regulator.

[0036] Performance evaluation of products prepared in Examples 1-5 (wherein CK is a mixed-dimensional attapulgite clay purified powder): (1) Water-holding capacity: Mainly evaluates the control of environmental conditioners on environmental humidity. Test method: Select a 9cm diameter funnel, fold a 18cm diameter filter paper, place it against the wall of the funnel, and place the funnel on a 50mL measuring cylinder. Weigh 10g of each sample and pour it into a funnel covered with filter paper. Slowly add 30mL of distilled water to the product, allowing the water to slowly pass through the sample and filter paper. Each product lasts for about 30 minutes. The main thing is to ensure that after all the water is added, no water drops drip from under the filter paper for 3 consecutive minutes. The water-holding capacity of various products can be calculated from the amount of water after filtration. The results are as follows: Figure 1 The greater the water-binding capacity, the stronger the hygroscopicity.

[0037] Depend on Figure 1 It can be seen that the hygroscopicity of Examples 1 and 2 is basically equivalent to that of CK, but Examples 3, 4, and 5 have better hygroscopicity than the control, which can effectively reduce the humidity in the livestock house and absorb the mucus on the surface of newborn piglets.

[0038] (2) Angle of repose: In a static equilibrium state, the acute angle between the free surface of the accumulated powder and the horizontal plane is called the angle of repose. Take 50g of sample and put it on a 20-mesh sieve. Use the intelligent powder property tester (BT-1001) to measure the angle of repose. The oscillation rate is 7 gears, the time is 180s, and the measurement is repeated three times. The results are averaged. The data is shown in Figure 2 The angle of repose directly reflects the fluidity of the powder. The smaller the angle of repose, the better the fluidity of the powder.

[0039] Depend on Figure 2 It can be seen that the product of the embodiment has better fluidity than CK, indicating better smoothness, is not easy to stick to the animal's body, and can fall off the animal's body quickly.

[0040] (3) Ammonia vapor adsorption: Add excess saturated ammonia water under the partition of the glass desiccator and place the sample bottle on the partition of the glass desiccator. Weigh 100 mg of sample and pour it into the sample bottle of the desiccator. Cover the desiccator lid to seal it. Take out the sample bottle and weigh it at regular intervals. Record the weighing time and sample mass and calculate the adsorption percentage. The result is as follows: Figure 3 shown.

[0041] Depend on Figure 3 It can be seen that the example product has a higher ammonia adsorption capacity than CK, which can effectively eliminate and control harmful gases in animal pens, protect the pen environment, and ensure animal health.

[0042] (4) Evaluation of antibacterial performance: The minimum inhibitory concentration (MIC) was tested by agar dilution method. The test steps were as follows: the sterilized sample was dispersed into agar medium at 40-50°C according to different concentrations, and the sample plate was obtained after cooling; 1-2 μL of 10 4 CFU / mL of fresh bacterial suspension was inoculated at 3 different positions on the sample plate, and positive control and negative control plates were prepared at the same time. Then the inoculated plates were cultured in a 37°C incubator for 18-24 hours. If there was no colony growth on the sample plate after the culture was completed, the bacteria were considered to be completely inhibited, and the minimum sample concentration that completely inhibited bacterial growth was the MIC.

[0043] Taking Escherichia coli and Staphylococcus aureus as examples, the experimental results are as follows Figure 4 and 5 As shown by Figure 4 and 5 It can be seen that the products in the examples have certain antibacterial properties. The MIC of Example 2 against Escherichia coli and Staphylococcus aureus is 20 mg / ml, and the MIC of the products in the other examples against both bacteria can reach 10 mg / ml.

Claims

1. A method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture, characterized in that: The modified mixed-dimensional attapulgite clay, zeolite, vermiculite, calamine and plant extract are placed in a powder mixer, and during the thorough mixing process, an antibacterial liquid is sprayed on the surface of the mixture, and the mixture is continuously stirred for 5 to 30 minutes, and then ground with a three-roll mill, dried and passed through a 200-mesh sieve to obtain the mixture; The raw materials are mixed in the following proportions by weight: 70-85 parts of modified mixed-dimensional attapulgite clay, 1-5 parts of zeolite, 3-5 parts of vermiculite, 3-5 parts of plant extract, 3-15 parts of calamine, and 3-10 parts of antibacterial liquid.

2. The method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture according to claim 1, characterized in that: The modified mixed-dimensional attapulgite clay is mixed-dimensional attapulgite clay powder with a mesh size of 200 or more, a water content of ≤10%, and a sand content of ≤2%. The modification method is as follows: 1) Purification of mixed-dimensional attapulgite clay: The crushed mixed-dimensional attapulgite clay is evenly dispersed in an acid solution with a pH value of 3-4 and activated for more than 4 hours, and then subjected to hydrocyclone treatment, solid-liquid separation and drying treatment in sequence; 2) Modification of mixed-dimensional attapulgite clay: first dissolve chlorhexidine acetate or chlorhexidine gluconate in an aqueous solution, then add the purified mixed-dimensional attapulgite clay to react at room temperature for 2-4 hours, filter, dry, crush, and pass through a 200-mesh sieve to obtain a clay mineral modified with chlorhexidine acetate or chlorhexidine gluconate.

3. The method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture as claimed in claim 2, characterized in that: The added amount of the chlorhexidine acetate or chlorhexidine gluconate is 3% to 15% of the mass of the mixed-dimensional attapulgite clay.

4. The method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture according to claim 1, characterized in that: The zeolite and vermiculite are both powder materials with a mesh size of 200 or more, a water content of ≤10%, and a sand content of ≤2%.

5. The method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture according to claim 1, characterized in that: The plant extract is mainly one or more of purslane extract, bletilla striata extract, liquorice extract, isatis root extract, codonopsis pilosula extract, astragalus extract, honeysuckle extract and wild chrysanthemum extract.

6. The method for preparing a mixed-dimensional attapulgite clay-based multifunctional environmental conditioner for aquaculture according to claim 1, characterized in that: The antibacterial liquid is obtained by fully stirring 0.5-2 wt% organic acid, 4-6 wt% emulsifier, and 1-3 wt% vegetable oil in hot water at 60-90°C; Among them, the organic acid is mainly one or more of benzoic acid, gallic acid, citric acid, and salicylic acid; the emulsifier is mainly one or more of monocaprin, monocaprylin, monolaurin, monomyristic glyceryl, coconut glucoside, glyceryl stearate, monolactic acid glyceryl, and Tween 80; the vegetable oil is mainly one or more of peanut oil, corn oil, sunflower oil, and blended oil.

7. A mixed-dimensional attapulgite clay-based multifunctional environmental regulator for aquaculture prepared by the method as claimed in claim 1.

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