CN115812850A - Preparation method of calcium propionate powder with composite gel coating layer and corresponding powder - Google Patents
Preparation method of calcium propionate powder with composite gel coating layer and corresponding powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 152
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 title claims abstract description 123
- 235000010331 calcium propionate Nutrition 0.000 title claims abstract description 123
- 239000004330 calcium propionate Substances 0.000 title claims abstract description 123
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
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- 239000011240 wet gel Substances 0.000 claims abstract description 104
- 239000002243 precursor Substances 0.000 claims abstract description 81
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- 235000017897 Cymbopogon citratus Nutrition 0.000 claims abstract description 67
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- 238000002156 mixing Methods 0.000 claims abstract description 36
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- 240000002262 Litsea cubeba Species 0.000 claims abstract description 31
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- 238000000034 method Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 11
- 244000166675 Cymbopogon nardus Species 0.000 claims abstract description 10
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 235000013399 edible fruits Nutrition 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 244000245109 Lindera glauca Species 0.000 claims description 10
- 235000001577 Lindera glauca Nutrition 0.000 claims description 10
- 235000002566 Capsicum Nutrition 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006002 Pepper Substances 0.000 claims description 7
- 235000016761 Piper aduncum Nutrition 0.000 claims description 7
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- 239000005708 Sodium hypochlorite Substances 0.000 claims description 7
- 239000000287 crude extract Substances 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 229920001144 Hydroxy alpha sanshool Polymers 0.000 claims description 3
- PSKIOIDCXFHNJA-UHFFFAOYSA-N Sanshool Natural products CC=CC=CC=CCCC=CC=CC(=O)NC(C)C PSKIOIDCXFHNJA-UHFFFAOYSA-N 0.000 claims description 3
- SBXYHCVXUCYYJT-UEOYEZOQSA-N alpha-Sanshool Chemical compound C\C=C\C=C\C=C/CC\C=C\C(=O)NCC(C)C SBXYHCVXUCYYJT-UEOYEZOQSA-N 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 3
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims description 2
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- AZJQQNWSSLCLJN-UHFFFAOYSA-N 2-ethoxyquinoline Chemical compound C1=CC=CC2=NC(OCC)=CC=C21 AZJQQNWSSLCLJN-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to the technical field of feed storage, and provides a preparation method of calcium propionate powder with a composite gel coating layer and corresponding powder, wherein the method comprises the following steps: preparing the extracted citronella grass root cellulose powder into citronella grass root cellulose wet gel precursor solution; preparing the obtained extract of the litsea cubeba into wet gel precursor solution of the litsea cubeba extract; mixing the lemongrass rhizome cellulose wet gel precursor solution and the sanshou pricklyash peel extract wet gel precursor solution according to the proportion, stirring and standing to obtain a composite wet gel intermediate, and performing supercritical purification to obtain a composite gel; fully mixing the calcium propionate powder with the composite gel according to the proportion, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, and carrying out heat treatment in a protective atmosphere to obtain the calcium propionate powder with a composite gel coating layer. The invention can improve the stability and quality-keeping effect of the natural feed quality-keeping additive without increasing the cost.
Description
Technical Field
The invention relates to the technical field of feed storage, in particular to a preparation method of calcium propionate powder with a composite gel coating layer and corresponding powder.
Background
Under the influence of the external environment, particularly the temperature and the humidity, the feed has the advantages that the components of the feed are changed, nutrient substances are gradually lost, and the feed is easy to mildew and oxidize when being transported or stored for a long time, so that various toxins are produced, the quality of the feed is reduced, and the feed is harmful to the fed animals. In order to reduce the economic loss caused by the mildew and oxidation of the feed, the feed mildew preventive and the antioxidant become important components of the feed as important feed additives. In practical application, the traditional mildew preventive and antioxidant can effectively delay the mildew and oxidation of the feed, but the effect is at the cost of sacrificing the whole nutrition level and palatability of the feed, and the additive with better mildew-proof and antioxidant effects has higher corrosivity, so that the taste and safety of the meat quality of animals can be reduced.
The Chinese acre is wide in breadth, rich in Chinese herbal medicine plant resources, and along with the continuous improvement of safety consciousness of people in recent years, the application of Chinese herbal medicine as a quality guaranteeing agent in feed becomes an important research direction and content. However, the poor stability of the Chinese herbal medicine and the high cost of raw materials and processes restrict the use of the Chinese herbal medicine as a feed quality guaranteeing agent.
Therefore, how to improve the stability of the Chinese herbal medicine feed quality-guaranteeing additive while reducing the cost becomes a technical problem to be solved urgently.
Disclosure of Invention
In view of this, in order to overcome the defects of the prior art, the invention provides a preparation method of calcium propionate powder with a composite gel coating layer and corresponding powder.
In one aspect, the invention provides a preparation method of calcium propionate powder with a composite gel coating layer, comprising the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Preprocessing the lemongrass roots into lemongrass root powder, extracting cellulose of the lemongrass roots, and preparing the extracted cellulose powder of the lemongrass roots into a wet cellulose gel precursor solution of the lemongrass roots;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Heating the sanchi fruit in a water bath, condensing, refluxing, filtering, drying and sterilizing to obtain a sanchi fruit extract, and preparing the obtained sanchi fruit extract into a sanchi fruit extract wet gel precursor solution;
step three, preparing composite gel
Mixing the lemongrass rhizome cellulose wet gel precursor solution prepared in the step one with the sanshool extract wet gel precursor solution prepared in the step two according to the ratio, stirring and standing the obtained mixed precursor solution to obtain a composite wet gel intermediate, and performing supercritical purification on the composite wet gel intermediate to obtain composite gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing the calcium propionate powder with the composite gel prepared in the third step according to the ratio, and coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And D, carrying out heat treatment on the composite gel coated calcium propionate powder obtained in the fourth step in a protective atmosphere to obtain the calcium propionate powder with the composite gel coating layer.
Further, the first step of the preparation method of the calcium propionate powder with the composite gel coating layer comprises the following steps:
pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass rhizome powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-liquid ratio of 1;
preparing a lemongrass rhizome cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring for 40min at the temperature of 2 ℃, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment for 30min at the temperature of-10 ℃ to obtain the lemongrass rhizome cellulose wet gel precursor solution.
Further, the second step of the preparation method of the calcium propionate powder with the composite gel coating layer comprises the following steps:
preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1:12, heating in water bath at 100 deg.C, condensing and refluxing at 80 deg.C for 120min, filtering, drying at 121 deg.C, and sterilizing for 20s to obtain fructus Zanthoxyli Spinifolii extract;
preparing a wet gel precursor solution of the lindera glauca fruit extract: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain the wet gel precursor solution of the litsea cubeba extract.
Further, the third step of the preparation method of the calcium propionate powder with the composite gel coating layer comprises:
mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain the composite wet gel.
Further, the fourth step of the preparation method of the calcium propionate powder with the composite gel coating layer comprises: and (3) fully mixing 100 parts by weight of calcium propionate powder with 10-50 parts by weight of the composite gel prepared in the third step, and coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment to obtain the composite gel-coated calcium propionate powder.
Furthermore, in the fourth step of the preparation method of the calcium propionate powder with the composite gel coating layer, the granularity of the calcium propionate powder is 200-300 μm, the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min.
Further, the fifth step of the preparation method of the calcium propionate powder with the composite gel coating layer comprises: and (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
In another aspect, the invention provides a calcium propionate powder with a composite gel coating layer, which is prepared by the method.
The preparation method of the calcium propionate powder with the composite gel coating layer and the corresponding powder have the following beneficial effects:
1. the lemongrass roots and the litsea cubeba are selected as main raw materials, the extraction process is simple and convenient, the raw material sources are rich, and the cost is low.
2. The compound gel is prepared by preparing the citronella grass root cellulose wet gel precursor solution and the sanshou pepper fruit extract wet gel precursor solution, and the stability of the citronella grass root cellulose and the sanshou pepper fruit extract is improved while compounding.
3. The prepared composite gel is coated on the surface of the calcium propionate powder to obtain the composite gel coated calcium propionate powder, so that the carrier is provided for the lemongrass rhizome cellulose and the litsea cubeba fruit extract, the mildew-proof effect of the calcium propionate is fully exerted, and the compounding and quality guarantee of the calcium propionate are realized.
4. The compound gel coated calcium propionate powder is subjected to heat treatment to obtain the calcium propionate powder with a compound gel coating layer, and the lemongrass rhizome cellulose and the litsea cubeba extract are coated on the outer side of the calcium propionate in a stable coating layer form to form the long-acting slow-release mildew-proof antioxidant compound powder.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a flowchart illustrating a method for preparing calcium propionate powder with a composite gel coating layer according to an exemplary first embodiment of the present invention.
Fig. 2 is a graph comparing the peroxide values of calcium propionate powders with composite gel coating layers prepared according to the second to sixth embodiments of the present invention and a control group.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
It should be noted that, in the case of no conflict, the features in the following embodiments and examples may be combined with each other; moreover, all other embodiments that can be derived by one of ordinary skill in the art from the embodiments disclosed herein without making any creative effort fall within the scope of the present disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the appended claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the disclosure, one skilled in the art should appreciate that one aspect described herein may be implemented independently of any other aspects and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. Additionally, such an apparatus may be implemented and/or such a method may be practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
Fig. 1 is a flowchart illustrating a method for preparing calcium propionate powder with a composite gel coating layer according to an exemplary first embodiment of the present invention, as shown in fig. 1, the method of this embodiment includes:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Preprocessing lemongrass roots into lemongrass root powder, extracting cellulose of the lemongrass roots, and preparing the extracted lemongrass root cellulose powder into a lemongrass root cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Heating the sanchi fruit in a water bath, condensing, refluxing, filtering, drying and sterilizing to obtain a sanchi fruit extract, and preparing the obtained sanchi fruit extract into a sanchi fruit extract wet gel precursor solution;
step three, preparing composite gel
Mixing the lemongrass rhizome cellulose wet gel precursor solution prepared in the step one with the sanshool extract wet gel precursor solution prepared in the step two according to the ratio, stirring and standing the obtained mixed precursor solution to obtain a composite wet gel intermediate, and performing supercritical purification on the composite wet gel intermediate to obtain composite gel;
step four, preparation of composite gel coated calcium propionate powder
Fully mixing the calcium propionate powder with the composite gel prepared in the third step according to the ratio, and coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And D, carrying out heat treatment on the composite gel coated calcium propionate powder obtained in the fourth step in a protective atmosphere to obtain the calcium propionate powder with the composite gel coating layer.
The invention provides a preparation method of calcium propionate powder with a composite gel coating layer, which is implemented by the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass root cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring at the temperature of 2 ℃ for 40min, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment at the temperature of-10 ℃ for 30min to obtain a lemongrass rhizome cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1;
preparing a shanji pepper fruit extract wet gel precursor solution: mixing 100 parts by weight of the sanshou fruit extract and 350 parts by weight of deionized water, stirring at 2 ℃ for 15min, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment at-5 ℃ for 30min to obtain a wet gel precursor solution of the sanshou fruit extract;
step three, preparing composite gel
Mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain composite wet gel;
step four, preparation of composite gel coated calcium propionate powder
Fully mixing 100 parts by weight of calcium propionate powder with the granularity of 300 mu m and 10 parts by weight of the composite gel prepared in the third step, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, wherein the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
The third embodiment of the present invention provides a method for preparing calcium propionate powder with a composite gel coating layer, where the method of this embodiment is implemented by the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass root cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring at the temperature of 2 ℃ for 40min, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment at the temperature of-10 ℃ for 30min to obtain a lemongrass rhizome cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1:12, heating in water bath at 100 deg.C, condensing and refluxing at 80 deg.C for 120min, filtering, drying at 121 deg.C, and sterilizing for 20s to obtain fructus Zanthoxyli Spinifolii extract;
preparing a shanji pepper fruit extract wet gel precursor solution: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain a wet gel precursor solution of the extract of the litsea cubeba;
step three, preparing composite gel
Mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain composite wet gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing 100 parts by weight of calcium propionate powder with the granularity of 280 mu m and 20 parts by weight of the composite gel prepared in the third step, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, wherein the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
The invention provides a preparation method of calcium propionate powder with a composite gel coating layer, which is implemented according to the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass rhizome cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring at the temperature of 2 ℃ for 40min, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment at the temperature of-10 ℃ for 30min to obtain a lemongrass rhizome cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1;
preparing a shanji pepper fruit extract wet gel precursor solution: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain a wet gel precursor solution of the extract of the litsea cubeba;
step three, preparing composite gel
Mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain composite wet gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing 100 parts by weight of calcium propionate powder with the granularity of 250 mu m and 30 parts by weight of the composite gel prepared in the third step, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, wherein the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
The fifth embodiment of the present invention provides a method for preparing calcium propionate powder with a composite gel coating layer, where the method of this embodiment is implemented by the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass root cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring at the temperature of 2 ℃ for 40min, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment at the temperature of-10 ℃ for 30min to obtain a lemongrass rhizome cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1;
preparing a wet gel precursor solution of the lindera glauca fruit extract: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain a wet gel precursor solution of the extract of the litsea cubeba;
step three, preparing composite gel
Mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain composite wet gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing 100 parts by weight of calcium propionate powder with the granularity of 230 mu m and 40 parts by weight of the composite gel prepared in the third step, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, wherein the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
The invention provides a preparation method of calcium propionate powder with a composite gel coating layer, which is implemented by the following steps:
step one, preparation of a lemongrass rhizome cellulose wet gel precursor solution
Pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass root cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring at the temperature of 2 ℃ for 40min, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment at the temperature of-10 ℃ for 30min to obtain a lemongrass rhizome cellulose wet gel precursor solution;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1;
preparing a shanji pepper fruit extract wet gel precursor solution: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain a wet gel precursor solution of the extract of the litsea cubeba;
step three, preparing composite gel
Mixing 100 parts by weight of a lemongrass rhizome cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring at-10 ℃ for 60min, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain composite wet gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing 100 parts by weight of calcium propionate powder with the particle size of 200 mu m and 50 parts by weight of the composite gel prepared in the third step, coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment, wherein the ultrasonic dispersion frequency is 20KHZ, and the ultrasonic dispersion time is 10min to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
Seventh example of the invention calcium propionate powders with composite gel coating layers prepared in examples two to six were tested. Specifically, the calcium propionate powders with composite gel coating layers prepared in the second to sixth embodiments are grouped and numbered; the average particle size of the calcium propionate powder with the composite gel coating layer is measured according to ASTM E2980-2014 Standard test method for evaluating the average particle size of powder by air permeability; the results are shown in Table 1.
TABLE 1
| Examples | Sample number | Average particle size of calcium propionate powder with composite gel coating layer |
| Example two | S1 | 312μm |
| EXAMPLE III | S2 | 298μm |
| Example four | S3 | 265μm |
| EXAMPLE five | S4 | 255μm |
| EXAMPLE six | S5 | 262μm |
As shown in table 1, the average particle size of the calcium propionate powder with composite gel coating layer prepared in examples two to six is not larger than 312 μm.
The technical principle concept of the invention is as follows:
preparing a lemongrass rhizome cellulose wet gel precursor solution and a lindera glauca fruit extract wet gel precursor solution to prepare a composite gel, coating the prepared composite gel on the surface of calcium propionate powder to obtain composite gel-coated calcium propionate powder, and performing heat treatment on the composite gel-coated calcium propionate powder to obtain the calcium propionate powder with a composite gel coating layer.
The eighth example of the present invention performs a mildew-proof effect test on the calcium propionate powder having the composite gel coating layer prepared in the second to sixth examples. Specifically, the calcium propionate powder with the composite gel coating layer prepared in examples two to six is premixed in a piglet feed, the sample components are respectively numbered as T1, T2, T3, T4 and T5, the mold quantity is detected according to GB13092 "determination of total number of molds in feed" after natural mold growth for 15d, and the inhibition rate of the calcium propionate powder with the composite gel coating layer is calculated, the inhibition rate (%) = (mold content of control sample-mold content of test sample)/mold content of control sample × 100%, and the test results are shown in table 2.
As shown in table 2, the bacteriostatic rate of the calcium propionate powder with the composite gel coating layer prepared in the second to sixth embodiments is not less than 44%.
TABLE 2
| Examples | Sample number | Rate of inhibition of bacteria |
| Example two | T1 | 58％ |
| EXAMPLE III | T2 | 55％ |
| Example four | T3 | 62％ |
| EXAMPLE five | T4 | 49％ |
| Example six | T5 | 44％ |
The calcium propionate powder with the composite gel coating layer prepared in the second to sixth embodiments of the application is added into piglet feed, and the sample groups are respectively numbered as Y1, Y2, Y3, Y4 and Y5; ethoxyquinoline (EMQ) was added to the piglet feed to form control group D1; piglet feed without antioxidant as control group D2; the addition ratio of each sample group was 0.35kg/t. The peroxide values of the respective sample groups were measured in accordance with GB 5009.227-2016 (national food safety Standard for determination of peroxide values in food), and the results of the measurements are shown in Table 3 and FIG. 2.
TABLE 3
As can be seen from Table 3 and FIG. 2, the peroxide values of all the sample groups showed an increasing trend from day 7 to day 14. The peroxide values of control D1 and test samples B1, B2, B3, B4 and B5 were significantly lower than the peroxide value of control D2 during days 21 and 28. On days 35-49, peroxide values increased and then decreased in all control groups; whereas the peroxide values of the sample groups Y1, Y2, Y3, Y4 and Y5 fluctuated less and were significantly lower than those of the contemporary control groups D1 and D2. On day 56, the peroxide values of all control and test groups dropped to a lower level. The peroxide values of the test groups were lower than the peroxide values of all the control groups during the entire test period.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A preparation method of calcium propionate powder with a composite gel coating layer is characterized by comprising the following steps:
step one, preparing a lemongrass rhizome cellulose wet gel precursor solution
Preprocessing the lemongrass roots into lemongrass root powder, extracting cellulose of the lemongrass roots, and preparing the extracted cellulose powder of the lemongrass roots into a wet cellulose gel precursor solution of the lemongrass roots;
step two, preparation of a wet gel precursor solution of the litsea cubeba extract
Heating the Zanthoxylum bungeanum Maxim fruit in water bath, condensing, refluxing, filtering, drying and sterilizing to obtain Zanthoxylum bungeanum Maxim fruit extract, and preparing the obtained Zanthoxylum bungeanum Maxim fruit extract into a Zanthoxylum bungeanum Maxim fruit extract wet gel precursor liquid;
step three, preparing composite gel
Mixing the lemongrass rhizome cellulose wet gel precursor solution prepared in the step one with the sanshool extract wet gel precursor solution prepared in the step two according to the ratio, stirring and standing the obtained mixed precursor solution to obtain a composite wet gel intermediate, and performing supercritical purification on the composite wet gel intermediate to obtain composite gel;
step four, preparing composite gel coated calcium propionate powder
Fully mixing the calcium propionate powder with the composite gel prepared in the third step according to the ratio, and coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment to obtain the composite gel coated calcium propionate powder;
step five, preparing calcium propionate powder with composite gel coating layer
And D, carrying out heat treatment on the composite gel coated calcium propionate powder obtained in the fourth step in a protective atmosphere to obtain the calcium propionate powder with the composite gel coating layer.
2. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein the first step of the method comprises:
pretreatment: cutting rhizoma Imperatae into segments, adding into 60 deg.C distilled water, heating at constant temperature for 80min, drying, pulverizing, and sieving to obtain 40 μm rhizoma Imperatae powder;
extracting the cellulose of the lemongrass roots: adding the lemongrass root powder into 0.15mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1; adding the crude extract powder into 0.1mol/L sodium hypochlorite solution according to a solid-to-liquid ratio of 1;
preparing a lemongrass rhizome cellulose wet gel precursor solution: mixing 100 parts by weight of lemongrass rhizome cellulose and 500 parts by weight of deionized water, stirring for 40min at the temperature of 2 ℃, adding 30 parts by weight of 0.2mol/L sodium hydroxide solution, and carrying out ultrasonic treatment for 30min at the temperature of-10 ℃ to obtain the lemongrass rhizome cellulose wet gel precursor solution.
3. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein the second step of the method comprises:
preparing a litsea cubeba extract: adding fructus Zanthoxyli Spinifolii into distilled water at a solid-to-liquid ratio of 1;
preparing a shanji pepper fruit extract wet gel precursor solution: mixing 100 parts by weight of the extract of the litsea cubeba with 350 parts by weight of deionized water, stirring for 15min at the temperature of 2 ℃, adding 29 parts by weight of 0.1mol/L citric acid solution, and carrying out ultrasonic treatment for 30min at the temperature of-5 ℃ to obtain the wet gel precursor solution of the litsea cubeba extract.
4. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein the third step of the method comprises:
mixing 100 parts by weight of a citronella grass root cellulose wet gel precursor solution and 135 parts by weight of a lindera glauca fruit extract wet gel precursor solution according to the weight part ratio, stirring for 60min at-10 ℃, standing for 24h to obtain a composite wet gel intermediate, and performing supercritical purification treatment on the composite wet gel intermediate by using a supercritical purifier, wherein the temperature in the supercritical purifier is-5 ℃, the pressure in the supercritical purifier is 8.5MPa, and the purified fluid is absolute ethyl alcohol to obtain the composite wet gel.
5. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein the fourth step of the method comprises: and (3) fully mixing 100 parts by weight of calcium propionate powder with 10-50 parts by weight of the composite gel prepared in the third step, and coating the composite gel on the surface of the calcium propionate powder through ultrasonic dispersion treatment to obtain the composite gel-coated calcium propionate powder.
6. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein in the fourth step of the method, the particle size of the calcium propionate powder is 200-300 μm, the frequency of ultrasonic dispersion is 20KHZ, and the time of ultrasonic dispersion is 10min.
7. The method for preparing calcium propionate powder with composite gel coating layer according to claim 1, wherein the fifth step of the method comprises: and (3) placing the composite gel coated calcium propionate powder obtained in the fourth step in a hydrogen protective atmosphere, heating to 280 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 120min to obtain the calcium propionate powder with the composite gel coating layer.
8. Calcium propionate powder with a composite gel coating layer, characterized in that the calcium propionate powder with a composite gel coating layer is prepared by the method of any one of claims 1 to 7.
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