CN115254019A - Silicate functional mycotoxin adsorbent and preparation method thereof - Google Patents
Silicate functional mycotoxin adsorbent and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
Abstract
The invention belongs to the technical field of mycotoxin, and discloses a silicate functional mycotoxin adsorbent and a preparation method thereof, wherein the silicate functional mycotoxin adsorbent consists of 20-25 parts of modified zeolite, 20-25 parts of nano zinc oxide, 10-15 parts of modified attapulgite, 10-15 parts of modified bentonite, 10-15 parts of active carbon, 10-15 parts of a honeysuckle extract, 10-15 parts of a konjak extract and 5-8 parts of a camellia extract in parts by mass. According to the invention, through mutual cooperation of various natural substances of the modified zeolite, the nano zinc oxide, the modified attapulgite, the modified bentonite, the activated carbon, the honeysuckle extract, the konjak extract and the camellia extract, the adsorption of various mycotoxins can be efficiently carried out, and meanwhile, the adsorbed toxins can be wrapped in adsorption particles and discharged out of a body, so that the safety is high, and the environment is not polluted.
Description
Technical Field
The invention belongs to the technical field of mycotoxin, and particularly relates to a silicate functional mycotoxin adsorbent and a preparation method thereof.
Background
Currently, mycotoxins are secondary metabolites generated in the growth and reproduction process of mold fungi, and among more than 20 of currently known mycotoxins, more than 20 of the currently known mycotoxins can cause damage to animal growth, particularly aflatoxin B1 (AFB 1), zearalenone (ZEN) and vomitoxin, which can cause serious consequences such as reduction of animal growth performance, clinical disease initiation, even death and the like.
Due to the current global climate abnormality, the mold contamination of feed raw materials is increased. Since 11 months in 2014, zearalenone and vomitoxin in corn byproducts and fermented feed samples are seriously polluted, and vomitoxin in wheat and wheat bran is seriously polluted. A CLS test sample result established in 8 months in 2015 shows that the concentration of zearalenone in the fermented feed exceeds 4000ug/kg (the national standard limit is 500 ug/kg), the concentrations of complete materials and zearalenone in corn exceed 300ug/kg, and the situation of feed safety is very severe. The mycotoxin adsorbent is an effective means for reducing the harm of mycotoxin and improving the production performance of animals by adding the mycotoxin adsorbent into the feed, so that the development and popularization of mycotoxin adsorbent products are significant.
However, the conventional mycotoxin adsorbents have poor adsorption effects, cannot adsorb various mycotoxins, and are not safe enough.
Through the above analysis, the problems and defects of the prior art are as follows: the existing mycotoxin adsorbents are poor in adsorption effect, incapable of adsorbing various mycotoxins and insufficient in safety.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a silicate functional mycotoxin adsorbent and a preparation method thereof.
The invention is realized in such a way that the silicate functional mycotoxin adsorbent is composed of, by mass, 20-25 parts of modified zeolite, 20-25 parts of nano zinc oxide, 10-15 parts of modified attapulgite, 10-15 parts of modified bentonite, 10-15 parts of activated carbon, 10-15 parts of a honeysuckle extract, 10-15 parts of a konjak extract and 5-8 parts of a camellia extract.
Another object of the present invention is to provide a method for preparing a silicate-based functional mycotoxin adsorbent, such as the silicate-based functional mycotoxin adsorbent, the method for preparing the silicate-based functional mycotoxin adsorbent comprising:
step one, obtaining native zeolite, and cleaning, crushing and modifying the obtained native zeolite to obtain modified zeolite;
step two, obtaining attapulgite, and roasting, crushing and modifying the attapulgite to obtain modified attapulgite; obtaining bentonite, and preparing modified bentonite by roasting and acidic activation treatment on the bentonite;
step three, obtaining the konjak, and carrying out crushing, enzymolysis, extraction and drying treatment on the obtained konjak to obtain a konjak extract; respectively preparing honeysuckle extract and camellia extract;
step four, weighing the prepared modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, honeysuckle extract, konjak extract and camellia extract in proportion;
step five, uniformly mixing the weighed modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, honeysuckle extract, konjak extract and camellia extract by using a stirrer to obtain the silicate functional mycotoxin adsorbent.
Further, in the step one, the step of washing, crushing and modifying the obtained native zeolite to obtain the modified zeolite comprises the following steps:
(1) Removing surface impurities from the weighed primary zeolite, cleaning the primary zeolite by using clear water, and drying the primary zeolite by using a dryer;
(2) Crushing and crushing the dried primary zeolite by using a crusher, and sieving to obtain zeolite powder;
(3) Adding a certain amount of sodium hypochlorite solution into the obtained zeolite powder, uniformly stirring, and soaking for a period of time at normal temperature;
(4) Centrifuging and filtering the uniformly mixed solution to remove supernatant, and drying by using a drying device;
(5) And washing the dried object with deionized water for 2-3 minutes, then roasting the object with a muffle furnace, grinding with a grinding device, and sieving with a 80-100-mesh sieve to obtain the modified zeolite.
Further, in the step (2), the sieving comprises: sieving with 90-100 mesh sieve.
Further, in the step (4), the drying includes: drying at 120-130 deg.C for 1 hr;
in the step (5), the roasting includes: calcining at 200-300 deg.C for 1 hr.
Further, in the second step, the modified attapulgite is obtained by roasting, crushing and modifying the attapulgite, and comprises:
firstly, obtaining attapulgite, washing the obtained attapulgite by using deionized water, and naturally drying the attapulgite;
secondly, placing the air-dried attapulgite in a muffle furnace for roasting treatment, and naturally cooling the roasted attapulgite to room temperature;
thirdly, crushing the cooled attapulgite by using a crusher to obtain attapulgite powder;
then, adding a certain amount of glucose solution into the obtained attapulgite powder, uniformly stirring, and heating the mixed liquid of the attapulgite powder and the glucose solution in a water bath;
and finally, carrying out freeze drying treatment on the mixed liquid to obtain the modified attapulgite.
Further, in the second step, the acidic activation treatment of bentonite includes: soaking the roasted bentonite in 15% hydrochloric acid solution at normal temperature for 2-6 hr.
Further, in the third step, the konjac is obtained, and the obtained konjac is subjected to crushing, enzymolysis, extraction and drying to obtain a konjac extract, wherein the konjac extract comprises:
(1) Cleaning the konjak by using clean water, drying by using a drying device, and powdering the dried konjak by using a pulverizer to obtain konjak powder;
(2) Adding cellulase into the obtained konjac flour, hydrolyzing under the assistance of ultrasonic waves, centrifuging, filtering and drying to obtain an enzymolysis product;
(3) Adding the obtained enzymolysis product into a Soxhlet extraction device, extracting for the second time in the presence of an extracting solution, filtering, and keeping a precipitate;
(4) And cleaning the obtained precipitate with absolute ethyl alcohol, and drying in vacuum to obtain the konjak extract.
Further, the (2) performing hydrolysis with the aid of ultrasonic waves includes: hydrolyzing at 45-55 deg.C under ultrasonic power of 260W for 20-25 min.
Further, in the step (3), the extracting solution is obtained by mixing absolute ethyl alcohol and propylene glycol according to a mass ratio of 2.
In combination with the above technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
according to the invention, through the mutual cooperation of various natural substances of the modified zeolite, the nano-zinc oxide, the modified attapulgite, the modified bentonite, the activated carbon, the honeysuckle extract, the konjak extract and the camellia extract, the adsorption of various mycotoxins can be efficiently carried out, and meanwhile, the adsorbed toxins can be wrapped in adsorption particles and discharged out of a body, so that the safety is high, and the environment is not polluted.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the silicate functional mycotoxin adsorbent can adjust the micro-ecological environment of the animal digestive tract, keep flora balance in the intestinal tract, activate an immune system, improve the immunity of the organism, enhance the functions of detoxifying and expelling toxins of the liver, protect and repair the body harm caused by infection of germs, mycotoxins and the like, and realize multiple effects of detoxifying, repairing and promoting growth.
Drawings
FIG. 1 is a flow chart of a method for preparing silicate-based functional mycotoxin adsorbents according to embodiments of the present invention;
FIG. 2 is a flow chart of a method for obtaining modified zeolite by washing, crushing and modifying the obtained native zeolite according to an embodiment of the present invention;
FIG. 3 is a flow chart of the method for obtaining attapulgite, roasting, crushing and modifying the attapulgite to obtain modified attapulgite according to the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
1. The embodiments are explained. This section is an illustrative example developed to explain the claims in order to enable those skilled in the art to fully understand how to implement the present invention.
The silicate functional mycotoxin adsorbent provided by the embodiment of the invention comprises, by mass, 20-25 parts of modified zeolite, 20-25 parts of nano zinc oxide, 10-15 parts of modified attapulgite, 10-15 parts of modified bentonite, 10-15 parts of activated carbon, 10-15 parts of honeysuckle extract, 10-15 parts of konjak extract and 5-8 parts of camellia extract.
As shown in fig. 1, a method for preparing a silicate-based functional mycotoxin adsorbent according to an embodiment of the present invention includes:
s101, obtaining native zeolite, and cleaning, crushing and modifying the obtained native zeolite to obtain modified zeolite;
s102, obtaining attapulgite, and roasting, crushing and modifying the attapulgite to obtain modified attapulgite; obtaining bentonite, and preparing modified bentonite by roasting and acid activation treatment on the bentonite;
s103, obtaining the konjak, and performing crushing, enzymolysis, extraction and drying treatment on the obtained konjak to obtain a konjak extract; respectively preparing honeysuckle extract and camellia extract;
s104, weighing the prepared modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, a honeysuckle extract, a konjak extract and a camellia extract in proportion;
s105, uniformly mixing the weighed modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, honeysuckle extract, konjak extract and camellia extract by using a stirrer to obtain the silicate functional mycotoxin adsorbent.
As shown in fig. 2, in step S101, the step of washing, crushing and modifying the obtained native zeolite to obtain the modified zeolite includes:
s201, removing surface impurities from the weighed primary zeolite, cleaning the primary zeolite with clear water, and drying the primary zeolite with a dryer;
s202, crushing and crushing the dried primary zeolite by using a crusher, and sieving by using a sieve with 90-100 meshes to obtain zeolite powder;
s203, adding a certain amount of sodium hypochlorite solution into the obtained zeolite powder, uniformly stirring, and soaking for a period of time at normal temperature;
s204, centrifuging and filtering the uniformly mixed solution to remove supernatant, and drying for 1 hour at 120-130 ℃ by using a drying device;
s205, washing the dried object with deionized water for 2-3 minutes, roasting the object for 1 hour at 200-300 ℃ by using a muffle furnace, grinding by using a grinding device, and sieving by using a sieve of 80-100 meshes to obtain the modified zeolite.
As shown in fig. 3, in step S102, obtaining the attapulgite, and performing roasting, crushing, and modifying treatment to obtain the modified attapulgite according to the embodiment of the present invention includes:
s301, obtaining attapulgite, washing the obtained attapulgite by using deionized water, and naturally drying the attapulgite;
s302, placing the air-dried attapulgite in a muffle furnace for roasting treatment, and naturally cooling the roasted attapulgite to room temperature;
s303, crushing the cooled attapulgite by using a crusher to obtain attapulgite powder;
s304, adding a certain amount of glucose solution into the obtained attapulgite powder, uniformly stirring, and heating the mixed liquid of the attapulgite powder and the glucose solution in a water bath;
s305, carrying out freeze drying treatment on the mixed liquid to obtain the modified attapulgite.
In step S102, the performing of the acid activation treatment on the bentonite provided by the embodiment of the present invention includes: soaking the roasted bentonite in 15% hydrochloric acid solution at normal temperature for 2-6 hr.
In step S103, the steps of obtaining the konjac, and performing pulverization, enzymolysis, extraction, and drying on the obtained konjac to obtain the konjac extract include:
(1) Cleaning the konjak by using clean water, drying by using a drying device, and powdering the dried konjak by using a pulverizer to obtain konjak powder;
(2) Adding cellulase into the obtained rhizoma Amorphophalli powder, hydrolyzing at 45-55 deg.C under ultrasonic power of 260W for 20-25 min, centrifuging, filtering, and drying to obtain enzymolysis product;
(3) Adding the obtained enzymolysis product into a Soxhlet extraction device, carrying out secondary extraction under the participation of an extracting solution, filtering, and keeping a precipitate;
(4) And cleaning the obtained precipitate with absolute ethyl alcohol, and vacuum drying to obtain the konjak extract.
(3) In the method, the extracting solution provided by the embodiment of the invention is obtained by mixing absolute ethyl alcohol and propylene glycol according to the mass ratio of 2.
2. Application examples. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is an application example of the technical scheme of the claims to a specific product or related technology.
The silicate functional mycotoxin adsorbent provided by the embodiment of the invention is added into animal feed according to the proportion of 3% -6%, so that adsorption of various mycotoxins can be effectively carried out.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The silicate functional mycotoxin adsorbent is characterized by comprising, by mass, 20-25 parts of modified zeolite, 20-25 parts of nano zinc oxide, 10-15 parts of modified attapulgite, 10-15 parts of modified bentonite, 10-15 parts of activated carbon, 10-15 parts of a honeysuckle extract, 10-15 parts of a konjak extract and 5-8 parts of a camellia extract.
2. A method of preparing a silicate functional mycotoxin adsorbent as defined in claim 1, wherein the method comprises:
step one, obtaining native zeolite, and cleaning, crushing and modifying the obtained native zeolite to obtain modified zeolite;
step two, obtaining attapulgite, and roasting, crushing and modifying the attapulgite to obtain modified attapulgite; obtaining bentonite, and preparing modified bentonite by roasting and acid activation treatment on the bentonite;
step three, obtaining the konjak, and carrying out crushing, enzymolysis, extraction and drying treatment on the obtained konjak to obtain a konjak extract; respectively preparing honeysuckle extract and camellia extract;
step four, weighing the prepared modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, honeysuckle extract, konjak extract and camellia extract in proportion;
step five, uniformly mixing the weighed modified zeolite, nano zinc oxide, modified attapulgite, modified bentonite, activated carbon, honeysuckle extract, konjak extract and camellia extract by using a stirrer to obtain the silicate functional mycotoxin adsorbent.
3. The method for preparing silicate-based functional mycotoxin adsorbent of claim 2, wherein the first step of washing, pulverizing and modifying the obtained native zeolite to obtain modified zeolite comprises:
(1) Removing surface impurities from the weighed primary zeolite, cleaning the primary zeolite by using clear water, and drying the primary zeolite by using a dryer;
(2) Crushing and crushing the dried protozeolite by using a crusher, and sieving to obtain zeolite powder;
(3) Adding a certain amount of sodium hypochlorite solution into the obtained zeolite powder, uniformly stirring, and soaking for a period of time at normal temperature;
(4) Centrifuging and filtering the uniformly mixed solution to remove supernatant, and drying by using a drying device;
(5) And washing the dried object with deionized water for 2-3 minutes, then roasting the object with a muffle furnace, grinding with a grinding device, and sieving with a 80-100-mesh sieve to obtain the modified zeolite.
4. The method for preparing silicate-based functional mycotoxin adsorbent of claim 3, wherein the sieving in step (2) comprises: sieving with 90-100 mesh sieve.
5. The method for preparing silicate-based functional mycotoxin adsorbent of claim 3, wherein the drying step (4) comprises: drying at 120-130 deg.C for 1 hr;
in the step (5), the firing includes: calcining at 200-300 deg.C for 1 hr.
6. The method for preparing the silicate-based functional mycotoxin adsorbent of claim 2, wherein in the second step, the modified attapulgite is obtained by roasting, crushing and modifying the attapulgite, and the modified attapulgite comprises the following components:
firstly, obtaining attapulgite, washing the obtained attapulgite by using deionized water, and naturally drying the attapulgite;
secondly, placing the air-dried attapulgite in a muffle furnace for roasting treatment, and naturally cooling the roasted attapulgite to room temperature;
thirdly, crushing the cooled attapulgite by using a crusher to obtain attapulgite powder;
then, adding a certain amount of glucose solution into the obtained attapulgite powder, uniformly stirring, and heating the mixed liquid of the attapulgite powder and the glucose solution in a water bath;
and finally, carrying out freeze drying treatment on the mixed liquid to obtain the modified attapulgite.
7. The method for preparing silicate-based functional mycotoxin adsorbent of claim 2, wherein in the second step, the acid activation treatment of bentonite comprises: soaking the roasted bentonite in 15% hydrochloric acid solution at normal temperature for 2-6 hr.
8. The method for preparing the silicate-based functional mycotoxin adsorbent of claim 2, wherein the step three of obtaining the konjac, and pulverizing, performing enzymatic hydrolysis, extracting, and drying the obtained konjac to obtain the konjac extract comprises:
(1) Cleaning the konjak by using clean water, drying by using a drying device, and powdering the dried konjak by using a pulverizer to obtain konjak powder;
(2) Adding cellulase into the obtained konjac flour, hydrolyzing under the assistance of ultrasonic waves, centrifuging, filtering, and drying to obtain an enzymolysis product;
(3) Adding the obtained enzymolysis product into a Soxhlet extraction device, extracting for the second time in the presence of an extracting solution, filtering, and keeping a precipitate;
(4) And cleaning the obtained precipitate with absolute ethyl alcohol, and vacuum drying to obtain the konjak extract.
9. The method according to claim 8, wherein the hydrolysis under the assistance of ultrasonic waves in step (2) comprises: hydrolyzing at 45-55 deg.C under the power of ultrasonic wave of 260W for 20-25 min.
10. The method for preparing the silicate-based functional mycotoxin adsorbent of claim 2, wherein in the step (3), the extract is obtained by mixing absolute ethyl alcohol and propylene glycol in a mass ratio of 2.
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2022
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