CN111972408A - Special antibacterial mildew inhibitor for casein and preparation method thereof - Google Patents

Special antibacterial mildew inhibitor for casein and preparation method thereof Download PDF

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Publication number
CN111972408A
CN111972408A CN202010842028.5A CN202010842028A CN111972408A CN 111972408 A CN111972408 A CN 111972408A CN 202010842028 A CN202010842028 A CN 202010842028A CN 111972408 A CN111972408 A CN 111972408A
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China
Prior art keywords
casein
antibacterial
mixing
agent
precursor
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Pending
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CN202010842028.5A
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Chinese (zh)
Inventor
孔维峰
郑晓平
于海阔
李佼佼
韦海翔
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Nanjing Tiansland Biotechnology Co ltd
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Nanjing Tiansland Biotechnology Co ltd
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Priority to CN202010842028.5A priority Critical patent/CN111972408A/en
Publication of CN111972408A publication Critical patent/CN111972408A/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2

Abstract

The invention discloses a special antibacterial mildew preventive for casein and a preparation method thereof, wherein the special antibacterial mildew preventive for casein comprises zinc pyrithione, thiazole antibacterial agents, emulsifying agents, thickening agents, chloroform, phosphate buffer solutions and casein, and zinc pyrithione is weighed and ground to obtain a dispersed semi-finished product; and then emulsifying the weighed antibacterial agent, magnetically stirring and mixing the antibacterial agent and the dispersed semi-finished product, mixing and dissolving the obtained precursor with chloroform under a shading condition, evaporating, drying, grinding and filtering, and then mixing, diffusing and ultrasonically treating the obtained liposome and casein ultrasonically dispersed in phosphate buffer solution to obtain the antibacterial mildew preventive wrapped by the casein, so that the antibacterial mildew preventive effect is improved, the casein is used for wrapping, the service time of the antibacterial mildew preventive is prolonged, and the utilization rate is improved.

Description

Special antibacterial mildew inhibitor for casein and preparation method thereof
Technical Field
The invention relates to the technical field of antibacterial mildew inhibitors, and particularly relates to a special antibacterial mildew inhibitor for casein and a preparation method thereof.
Background
At present, inorganic antibacterial agents, organic antibacterial agents, composite antibacterial agents and the like which are commonly existing in the market have ideal antibacterial effect when in use, but the use time is short, so that the utilization rate is reduced.
Disclosure of Invention
The invention aims to provide the special antibacterial mildew inhibitor for casein and the preparation method thereof, so that the service time is prolonged, and the utilization rate is improved.
In order to achieve the above object, in a first aspect, the present invention provides a preparation method of an antimicrobial and antifungal agent specially used for casein, including:
weighing zinc pyrithione and grinding to obtain a dispersed semi-finished product;
emulsifying the weighed antibacterial agent, and mixing the weighed antibacterial agent with the dispersed semi-finished product to obtain a precursor;
dissolving the precursor and a water phase medium, and performing ultrasonic filtration to obtain a liposome;
and mixing and stirring the liposome and casein, and performing ultrasonic treatment to obtain the antibacterial mildew preventive coated by the casein.
Wherein, emulsifying the weighed antibacterial agent and mixing the weighed antibacterial agent with the dispersed semi-finished product to obtain a precursor, comprising the following steps:
weighing an antibacterial agent and an emulsifier according to a specified amount in proportion, mixing, adding distilled water and a thickening agent, mixing and stirring for 10-20min, adding the dispersion finished product into the stirred mixture, and performing magnetic stirring for 15-30min to obtain a precursor, wherein the specified amount of the antibacterial agent is 5-8 parts.
Dissolving the precursor and a water phase medium, and performing ultrasonic filtration to obtain the liposome, wherein the method comprises the following steps:
and weighing the precursor and chloroform according to the mixing ratio under the shading condition, mixing and dissolving, and evaporating and drying the dissolved liquid at 30 ℃ for 24 hours in sequence.
Wherein, dissolving the precursor and a water phase medium, and carrying out ultrasonic filtration to obtain the liposome, and the method also comprises the following steps:
and (3) carrying out hydration ultrasonic treatment on the dried block by using a phosphate buffer solution for 5h, then crushing the mixed solution for 30-40min by using a crusher according to an intermittent working mode, and centrifuging and filtering the crushed liquid to obtain the liposome.
Mixing, stirring and ultrasonically treating the liposome and casein to obtain the antibacterial mildew preventive coated by the casein, wherein the antibacterial mildew preventive comprises the following components:
and ultrasonically dispersing weighed casein in the phosphate buffer removing solution, adding the liposome, and mixing, diffusing and ultrasonically treating to obtain the antibacterial and mildewproof agent wrapped by the casein.
In a second aspect, the invention provides a special antibacterial and antifungal agent for casein, which comprises zinc pyrithione, thiazole antibacterial agents, an emulsifier, a thickening agent, chloroform, a phosphate buffer solution and casein.
The invention relates to a special antibacterial mildew preventive for casein and a preparation method thereof, wherein the special antibacterial mildew preventive for casein comprises zinc pyrithione, thiazole antibacterial agents, emulsifying agents, thickening agents, chloroform, phosphate buffer solutions and casein, and zinc pyrithione is weighed and ground to obtain a dispersed semi-finished product; and then emulsifying the weighed antibacterial agent, magnetically stirring and mixing the antibacterial agent and the dispersed semi-finished product, mixing and dissolving the obtained precursor with chloroform under a shading condition, evaporating, drying, grinding and filtering, and then mixing, diffusing and ultrasonically treating the obtained liposome and casein ultrasonically dispersed in phosphate buffer solution to obtain the antibacterial mildew preventive wrapped by the casein, so that the antibacterial mildew preventive effect is improved, the casein is used for wrapping, the service time of the antibacterial mildew preventive is prolonged, and the utilization rate is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic step diagram of a preparation method of the antimicrobial and antifungal agent specially used for casein provided by the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, the present invention provides a method for preparing an antibacterial and antifungal agent specially used for casein, including:
s101, weighing zinc pyrithione and grinding to obtain a dispersed semi-finished product.
Specifically, zinc pyrithione is weighed according to the proportion of 1:5.5, and is dispersed in distilled water, and is ground for about 2 minutes by a grinder for 2 times respectively to form a stable dispersion semi-finished product, wherein, during the dispersion, a dispersing agent can be added to increase the dispersion effect and speed, and the dispersing agent can be one or more of lignosulfonate, alkyl naphthalene sulfonate, a bis (alkyl) naphthalene sulfonate formaldehyde condensate, a naphthalene sulfonate formaldehyde condensate sodium salt, an alkyl or aralkyl naphthalene sulfonate formaldehyde condensate sodium salt, cresol sulfonic acid, a naphthol sulfonate formaldehyde condensate sodium salt, petroleum sodium sulfonate, an alkylbenzene sulfonic acid calcium salt and other salts, an ethylene oxide-propylene oxide block copolymer, an alkylphenol polyoxyethylene ether formaldehyde condensate and alkylphenol polyoxyethylene polyoxypropylene ether; the zinc pyrithione is also called bis (2-thio-1-pyridine oxide) zinc, abbreviated as ZPT, is an environment-friendly antibacterial mildew inhibitor, has good inhibition effect on bacteria and fungi, and is dissolved by using distilled water as a solvent, so that other chemical components are prevented from being introduced, and the product is more environment-friendly.
S102, emulsifying the weighed antibacterial agent, and mixing the antibacterial agent with the dispersed semi-finished product to obtain a precursor.
Specifically, an antibacterial agent and an emulsifier are respectively weighed according to a ratio of 25:1, wherein the specified amount of the antibacterial agent is 5-8 parts, namely 0.2 part of the emulsifier; emulsifying the antibacterial agent into an oil phase by using an emulsifier, adding distilled water and a thickening agent, mixing and stirring for 10-20min, and simultaneously adding the dispersion finished product into the stirred mixture, and magnetically stirring for 15-30min to obtain a precursor, wherein the antibacterial agent is a thiazole antibacterial agent and can be one or more of OIT, OIT and BBIT, DCOIT is named 4, 5-dichloro-2-n-octyl-4-isothiazoline-3-ketone in Chinese nomenclature, a broad-spectrum antibacterial and antifungal agent, and a latest slow release technology provides lasting protection, achieves the effect even exceeding TBTO (tributyltin compound), does not contain heavy metals, is released into the environment, and rapidly permeates into precipitates to be decomposed without accumulation; the OIT, the Chinese name of which is 2-n-octyl-4-isothiazoline-3-ketone, has broad-spectrum sterilization, is mildew-proof and algae-resistant, does not contain mercury and lead, is green and environment-friendly, has low solubility in water and long pesticide effect time, and particularly has excellent control capability on mildew; the BBIT, the Chinese name of which is 2-butyl-1, 2-benzisothiazolin-3-one, is a new generation of BIT alkyl derivative, solves the problems existing in the prior BIT in use, such as low efficiency, large dosage, poor effect on mildew and algae, lack of microbial action spectrum and the like, has obtained American EPA authentication, is environment-friendly and safe; the antibacterial agent can be selected from n-butyl-1, 2-benzisothiazolin-3-one (BBIT), and the emulsifier is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium butyl naphthalene sulfonate, condensate of fatty alcohol and ethylene oxide, naphthalene sulfonic acid formaldehyde condensate, alkyl naphthalene sulfonate, castor oil, silicones, azone and thiaketone; the thickening agent is selected from one or more of polysaccharide, carbomer, poloxamer and modified cellulose, a defoaming agent is added in the process of magnetic stirring to eliminate bubbles generated in the stirring process and ensure the mixing effect, and the precursor is compounded by zinc pyrithione and thiazole antibacterial agents, so that the precursor has the effects of resisting bacteria and preventing mildew and has a strong sterilization function.
S103, dissolving the precursor and a water phase medium, and performing ultrasonic filtration to obtain the liposome.
Specifically, firstly, an aqueous medium is a phosphate buffer solution prepared according to a pharmacopeia standard edition, the pH value is 6.5-7.4, 7.2 is selected, the precursor and chloroform are weighed according to a mixing ratio to be mixed and dissolved under a shading condition, and the chloroform is decomposed under a lighting condition to generate toxic phosgene, so that the process is carried out under the shading condition, and the safety of a product and the normal production are ensured; evaporating the dissolved liquid in an evaporator at 30 ℃ until the water is evaporated to dryness, forming a smooth film on the inner wall of a flask or a test tube containing the liquid, and then putting the test tube or the flask in a vacuum drying oven for drying for 24 hours, wherein the drying temperature is mainly ensured not to cause further chemical reaction of the product in the process of drying the liquid, so as to generate other required products or substances harmful to the required products.
And then, hydrating the dried block by using a phosphate buffer solution, wherein the hydration ultrasonic power is 100W, the ultrasonic time is 5h, and the ultrasonic treatment is carried out for a long time, so that the thorough hydration can be ensured, the hydration completeness of the product is improved, and the utilization rate of the product is further improved. According to an intermittent working mode, a pulverizer is utilized to pulverize the mixed liquid for 30-40min, specifically, the hydrated liquid is put into a cell ultramicro pulverizer to be pulverized in a working mode of working for 10s at a power of 360W and then stopping working for 10s, a test tube or a flask in the pulverizer can be vibrated in the process of stopping pulverizing, the pulverized mixed liquid at the previous moment is vibrated and mixed, the uniform density of each layer in the mixed liquid is ensured when the pulverized liquid at the next moment is pulverized, and the mixing effect is effectively ensured; and centrifuging the crushed liquid at the rotating speed of 4000rpm for 20 minutes, preparing centrifuged upper-layer liquid, and filtering by using a filter membrane with the required diameter to obtain the liposome.
S104, mixing and stirring the liposome and casein, and performing ultrasonic treatment to obtain the antibacterial mildew preventive coated by the casein.
Specifically, a certain amount of casein is weighed and ultrasonically dispersed in a Brij-35 phosphate buffer solution to form a casein-Brij-35 phosphate buffer solution, the ultrasonic power can be 100W, the ultrasonic time is 2 hours, then the casein-Brij-35 phosphate buffer solution is added into the liposome for stirring and mixing, and vibration diffusion is carried out for 20 minutes under the ultrasonic condition to ensure the uniformity of the density of the mixed liquid after diffusion, then the mixed liquid is frozen to be in an ice block shape and slowly melted at normal temperature, finally ultrasonic treatment is carried out for 2 hours under the ultrasonic power of 50W to close the liposome, the obtained solution is the antibacterial and antifungal agent wrapped by the casein, and the precursor prepared by zinc pyrithione and thiazole antibacterial agent is wrapped in the casein liposome to reduce the volatilization rate of the precursor in the using process, the service life is prolonged, and the utilization rate is improved.
The invention provides a special antibacterial mildew preventive for casein, which comprises zinc pyrithione, thiazole antibacterial agents, emulsifying agents, thickening agents, chloroform, phosphate buffer solutions and casein.
In the embodiment, the zinc pyrithione is also called bis (2-thio-1-pyridine oxide) zinc, abbreviated as ZPT, is an environment-friendly antibacterial and antifungal agent, has good inhibition effect on bacteria and fungi, and is dissolved by using distilled water as a solvent, so that other chemical components are prevented from being introduced, and the product is more environment-friendly; the antibacterial agent is thiazole antibacterial agent, and can be one or more of OIT, OIT and BBIT; the antibacterial agent can be selected from n-butyl-1, 2-benzisothiazolin-3-one (BBIT), and the emulsifier is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, butyl naphthalene sulfonic acid sodium salt, condensate of fatty alcohol and ethylene oxide, naphthalene sulfonic acid formaldehyde condensate, alkyl naphthalene sulfonate, castor oil, organosilicon, azone and thiaketone; the thickening agent is selected from one or more of polysaccharide, carbomer, poloxamer and modified cellulose, chloroform is easy to volatilize, the influence on a produced finished product is small, after the precursor is compounded by zinc pyrithione and thiazole antibacterial agents, the precursor can play a role in resisting bacteria and preventing mildew, and has a strong sterilization function, and the precursor prepared from the zinc pyrithione and the thiazole antibacterial agents is wrapped in casein liposome, so that the volatilization rate of the precursor in the using process can be reduced, the using time is prolonged, and the using utilization rate is improved.
The invention relates to a special antibacterial mildew preventive for casein and a preparation method thereof, wherein the special antibacterial mildew preventive for casein comprises zinc pyrithione, thiazole antibacterial agents, emulsifying agents, thickening agents, chloroform, phosphate buffer solutions and casein, and zinc pyrithione is weighed and ground to obtain a dispersed semi-finished product; and then emulsifying the weighed antibacterial agent, magnetically stirring and mixing the antibacterial agent and the dispersed semi-finished product, mixing and dissolving the obtained precursor with chloroform under a shading condition, evaporating, drying, grinding and filtering, and then mixing, diffusing and ultrasonically treating the obtained liposome and casein ultrasonically dispersed in phosphate buffer solution to obtain the antibacterial mildew preventive wrapped by the casein, so that the antibacterial mildew preventive effect is improved, the casein is used for wrapping, the service time of the antibacterial mildew preventive is prolonged, and the utilization rate is improved.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A preparation method of the special antibacterial mildew preventive for casein is characterized by comprising the following steps:
weighing zinc pyrithione and grinding to obtain a dispersed semi-finished product;
emulsifying the weighed antibacterial agent, and mixing the weighed antibacterial agent with the dispersed semi-finished product to obtain a precursor;
dissolving the precursor and a water phase medium, and performing ultrasonic filtration to obtain a liposome;
and mixing and stirring the liposome and casein, and performing ultrasonic treatment to obtain the antibacterial mildew preventive coated by the casein.
2. The method for preparing the antibacterial and antifungal agent specially used for casein according to claim 1, wherein the weighed antibacterial agent is emulsified and mixed with the dispersion semi-finished product to obtain a precursor, comprising:
weighing an antibacterial agent and an emulsifier according to a specified amount in proportion, mixing, adding distilled water and a thickening agent, mixing and stirring for 10-20min, adding the dispersion finished product into the stirred mixture, and performing magnetic stirring for 15-30min to obtain a precursor, wherein the specified amount of the antibacterial agent is 5-8 parts.
3. The method for preparing the antibacterial and antifungal agent specially used for casein according to claim 2, wherein the precursor is dissolved with an aqueous medium, and the liposome is obtained by ultrasonic filtration, comprising the following steps:
and weighing the precursor and chloroform according to the mixing ratio under the shading condition, mixing and dissolving, and evaporating and drying the dissolved liquid at 30 ℃ for 24 hours in sequence.
4. The method for preparing the antibacterial and antifungal agent specially used for casein according to claim 3, wherein the precursor is dissolved with an aqueous medium, and the liposome is obtained by ultrasonic filtration, further comprising:
and (3) carrying out hydration ultrasonic treatment on the dried block by using a phosphate buffer solution for 5h, then crushing the mixed solution for 30-40min by using a crusher according to an intermittent working mode, and centrifuging and filtering the crushed liquid to obtain the liposome.
5. The method for preparing the antibacterial and mildewcide special for casein according to claim 4, wherein the antibacterial and mildewcide coated by the casein is obtained by mixing, stirring and ultrasonically treating the liposome and the casein, and comprises the following steps of:
and ultrasonically dispersing weighed casein in the phosphate buffer removing solution, adding the liposome, and mixing, diffusing and ultrasonically treating to obtain the antibacterial and mildewproof agent wrapped by the casein.
6. An antibacterial mildew preventive special for casein, which is characterized in that,
the special antibacterial and mildewproof agent for casein comprises zinc pyrithione, thiazole antibacterial agents, emulsifying agents, thickening agents, chloroform, phosphate buffer solutions and casein.
CN202010842028.5A 2020-08-20 2020-08-20 Special antibacterial mildew inhibitor for casein and preparation method thereof Pending CN111972408A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB244150A (en) * 1924-09-03 1925-12-03 Latex Developments Ltd Improvements in or relating to waterproof paints
TWI248554B (en) * 1999-07-13 2006-02-01 Inctec Inc Casein solution
CN102783693A (en) * 2012-07-18 2012-11-21 华南理工大学 Preparation method of edible antibacterial nanometer particles
CN106038327A (en) * 2016-07-04 2016-10-26 江苏大学 Preparation method and application of casein-cinnamon essential oil lipidosome antibacterial agent
CN109485994A (en) * 2018-09-18 2019-03-19 青岛国恩科技股份有限公司 A kind of antibacterial antimildew polyacrylic and preparation method thereof for outer drum for drum washing machine
CN111248209A (en) * 2020-03-10 2020-06-09 上海毕特生物科技有限公司 Environment-friendly mildew-proof antibacterial agent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB244150A (en) * 1924-09-03 1925-12-03 Latex Developments Ltd Improvements in or relating to waterproof paints
TWI248554B (en) * 1999-07-13 2006-02-01 Inctec Inc Casein solution
CN102783693A (en) * 2012-07-18 2012-11-21 华南理工大学 Preparation method of edible antibacterial nanometer particles
CN106038327A (en) * 2016-07-04 2016-10-26 江苏大学 Preparation method and application of casein-cinnamon essential oil lipidosome antibacterial agent
CN109485994A (en) * 2018-09-18 2019-03-19 青岛国恩科技股份有限公司 A kind of antibacterial antimildew polyacrylic and preparation method thereof for outer drum for drum washing machine
CN111248209A (en) * 2020-03-10 2020-06-09 上海毕特生物科技有限公司 Environment-friendly mildew-proof antibacterial agent

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Application publication date: 20201124