CN105456287A - Selenium sulfide ultrafine powder and preparing method thereof - Google Patents

Selenium sulfide ultrafine powder and preparing method thereof Download PDF

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Publication number
CN105456287A
CN105456287A CN201510880617.1A CN201510880617A CN105456287A CN 105456287 A CN105456287 A CN 105456287A CN 201510880617 A CN201510880617 A CN 201510880617A CN 105456287 A CN105456287 A CN 105456287A
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Prior art keywords
selenium sulfide
ultrafine powder
powder
sulfide ultrafine
selenium
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CN201510880617.1A
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CN105456287B (en
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张志昂
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Zhang Zhiang
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Dayou Pharmaceutical Yangzhou Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/04Sulfur, selenium or tellurium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/23Sulfur; Selenium; Tellurium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0014Skin, i.e. galenical aspects of topical compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/143Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/145Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

Abstract

The invention discloses a selenium sulfide ultrafine powder and a preparing method thereof, and belongs to the field of washing products. The selenium sulfide ultrafine powder and the preparing method solve the problem that the production time of selenium sulfide ultrafine powder which is prepared through medium ball milling micronization and serves as a lotion is long, and the quality problems that selenium sulfide is large in particle, uneven in dispersion and instable. The particle size of the selenium sulfide ultrafine powder is 1-50 microns. The method includes the following steps that 1, dry selenium sulfide powder, purified water, medicine-level titanium dioxide and medicine-level glycerin are mixed to be even, and then citric acid is added to adjust the pH value to range from 3.5 to 4.5; 2, the mixture is arranged in a grinding-type ultrafine grinder to be ground and smashed, and the selenium sulfide ultrafine powder is obtained. The selenium sulfide ultrafine powder can be applied to daily chemical products such as lotions, liquid shampoo and hair conditioners.

Description

Selenium sulfide ultrafine powder and preparation method thereof
Technical field
The invention belongs to articles for washing field; Be specifically related to selenium sulfide ultrafine powder and preparation method thereof.
Background technology
Selenium sulfide is that bright orange is to red-brown powder; With faint hydrogen sulfide odor, water insoluble, be slightly soluble in chloroform, be atomicly dissolved in ether, be substantially insoluble to other organic solvents.Under daylight, high temperature or alkali condition, easy Oxidative inactivation blackening; The necessary lucifuge of product, is stored in cool place, hermetic container.
Selenium sulfide is used for dandruff dispelling, seborrhea, dandruff dermatitis, tinea versicolor etc.Be usually used in external, to put scalp on the skin outside 1% or 2.5% lotion, weekly 1 ~ 2 time to every 4 weeks 1 time as required.
A kind of new technique that micronization technology is the later development for adaptation modern high technology of 20 century 70s and derives from, usually adopt medium ball grinding method, the drug particle obtained is at 50 ~ 200 μm; Nowadays, the selenium sulfide medicated powder micronization produced in selenium sulfide lotion adopts this technology.Its shortcoming: first, medium micronization must be placed, production cycle is long, complex process, powder body (selenium sulfide medicated powder) granule is large, uneven, thus affect the dispersion inhomogeneities of selenium sulfide in lotion base, medicated powder granule suspension unstability, finally affect the unstability of product quality; The second, the production time long (a ball milling cycle needs 5-6 hour), loss is large, and production efficiency is low.
Summary of the invention
The invention solves medium ball milling micronization to prepare selenium sulfide ultrafine powder to there is selenium sulfide granule as lotion large, disperse uneven, instable quality problems, shorten the production time simultaneously, and provide selenium sulfide ultrafine powder and preparation method thereof.
In the present invention, the particle diameter of selenium sulfide ultrafine powder is (1 ~ 50) μm.
In the present invention, the preparation method of selenium sulfide ultrafine powder is carried out in the steps below:
Step one, by selenium sulfide dry powder, purified water, pharmaceutical grade titanium dioxide (i.e. pharmaceutical grade titanium dioxide) and pharmaceutical grade glycerol mix homogeneously, then add citric acid adjust ph between 3.5 ~ 4.5;
Step 2, be then placed in grinding type super micron mill pulverizing of milling, namely obtain selenium sulfide ultrafine powder.
In step one, the mass ratio of selenium sulfide dry powder, purified water, pharmaceutical grade titanium dioxide (i.e. pharmaceutical grade titanium dioxide) and pharmaceutical grade glycerol is 1:1:2:3.
Carry out at power 1.5kW, the speed of mainshaft 1500r/min pulverizing of milling in step 2.
Grinding time of milling in step 2 is 30min ~ 60min.
The ultrafine powder granular size of selenium sulfide of the present invention controls 1 ~ 50 μm of scope.As fruit granule all reaches nanoscale, so selenium sulfide medicated powder toxicology, biology and pharmacodynamics etc. aspect need safety evaluation again.In other words, nanoscale selenium sulfide medicated powder, its lotion product needs again to carry out research by new drug registration and declares, and increases cost.The granular size of product of the present invention, in the middle of medium ball abrasive particle and nano-scale particle, is namely less than medium ball milling micro powder granule about 100 times, is greater than between nano-scale particle 1000; Both solved selenium sulfide in lotion large because of ball milling micro powder granule, disperse homogeneity and the instable quality problems that suspend, meanwhile, it also avoid because of after selenium sulfide nano powder, the risk that new drug registration is evaluated pressed again by its preparation lotion.
Selenium sulfide medicated powder changes through micronization processes rear surface character, and specific surface area increases greatly, according to Noyes-Whitney equation, due to particle diameter reduce, specific surface area increases, thus adds the homogeneity of selenium sulfide medicated powder in lotion and stability; In addition, reduction due to selenium sulfide medicated powder particle diameter can also increase the adhesion of medicated powder and skin mucosa, thus increases the contact area of medicine and skin, extends contact time, medicine can be made fully effectively to play pharmacological effect, indirectly improve the drug effect of selenium sulfide lotion.
The granule of the inventive method selenium sulfide medicated powder 1 ~ 50 μm, granule 50 ~ 200 μm of particle diameters utilizing ultra micro powdering techniques to prepare of selenium sulfide medicated powder prepared by traditional ball grinding technique micronization are little, have multiple advantage:
(1) due to its special chemical property of selenium sulfide, preparation process adds a small amount of stabilizing agent, adopts wet milling process, reaches ultra micro efflorescence object; Its ultra micro powdering techniques is different from liposome, solid dispersion etc. not containing host material, is only made up of medicine, and containing appropriate stabilizing agent, ensure that main drug effectiveness, it also avoid the use of carrier, reduce costs, decrease the incidence rate of toxic and side effects.
(2) particle diameter is little, increases the adhesion of medicine and skin, prolong drug pathogen skin holdup time and improve the bioavailability of medicine.
(3) medicine stability is improved; Particle diameter reduces, and specific surface area increases, and surface energy also increases, and surface charge is large, and the mutual repulsive force of particle band identical charges increases, and reduces particle accumulation, increases stability.
Invention applies micronizer tool, carry out pulverizing without the ultra micro efflorescence of medium to selenium sulfide medicated powder, make selenium sulfide granule and reach 1 ~ 50 μm of ultrafine powder, can directly add in the substrate of selenium sulfide lotion, shampoo and hair conditioner, reach simplification production technology, shorten the requirement of production time and raising product internal control quality standard.
The present invention by the Grain size controlling of selenium sulfide at 1 ~ 50 μm, this not only simplifies and shortens the production technology of selenium sulfide lotion, the more important thing is and substantially increase the dispersion homogeneity of selenium sulfide in lotion base and the stability of suspension, directly enhance the product quality of selenium sulfide lotion.
Compared with the technique of the selenium sulfide prepared with traditional ball grinding technique micronization, granule reduces about 100 times, and the dispersion homogeneity in lotion base, stability are better than ball milling powder body; Simplify technique, shorten the production time, improve production efficiency, also reduce production cost, be easily applied to industrialization.
The route of the inventive method is simple, and process conditions are gentle, morphology microstructure, steady quality: super micron mill setting different technical parameters, can obtain the homogeneous powder body of different microgranule, production technology collimation is good, and products therefrom homogeneity is good, steady quality.
Outstanding advantage of the present invention is to utilize single or multiple equipment to combine, and carries out continuous prodution, and the technological process that can produce with pharmaceutical industriesization easily realizes seamless connection, and this technical characterstic is that other conventional arts are unrivaled.
Selenium sulfide ultrafine powder of the present invention can be applicable to the daily chemical products such as lotion, shampoo, hair conditioner.
Accompanying drawing explanation
Fig. 1 is the grain size distribution grinding powder body after 30min in detailed description of the invention six.
Detailed description of the invention
Detailed description of the invention one: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 1 μm.
Detailed description of the invention two: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 30 μm.
Detailed description of the invention three: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 50 μm.
Detailed description of the invention four: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 5 μm.
Detailed description of the invention five: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 20 μm.
Detailed description of the invention six: in present embodiment, the particle diameter of selenium sulfide ultrafine powder is 10 μm, and its preparation method carries out in the steps below:
Step one, by selenium sulfide dry powder, purified water, pharmaceutical grade titanium dioxide and pharmaceutical grade glycerol mix homogeneously, then add citric acid adjust ph between 3.5 ~ 4.5;
Step 2, be then placed in grinding type super micron mill, carry out milling at power 1.5kW, speed of mainshaft 1500r/min and pulverize 30min (see Fig. 1), sieve, namely obtain selenium sulfide ultrafine powder; Wherein in step one, the mass ratio of selenium sulfide dry powder, purified water, pharmaceutical grade titanium dioxide and pharmaceutical grade glycerol is 1:1:2:3.
Present embodiment makes the dispersion homogeneity of selenium sulfide ultrafine powder, the theoretical foundation of stability: investigate test through 6 months product quality accelerations, the quality of product is stability, meets target level of product quality.

Claims (7)

1. selenium sulfide ultrafine powder, is characterized in that the particle diameter of selenium sulfide ultrafine powder is for (1 ~ 50) μm.
2. selenium sulfide ultrafine powder according to claim 1, is characterized in that the particle diameter of selenium sulfide ultrafine powder is for (5 ~ 30) μm.
3. selenium sulfide ultrafine powder according to claim 1, is characterized in that the particle diameter of selenium sulfide ultrafine powder is 10 μm.
4. the preparation method of selenium sulfide ultrafine powder as claimed in claim 1, is characterized in that the preparation method of selenium sulfide ultrafine powder is carried out in the steps below:
Step one, by selenium sulfide dry powder, purified water, pharmaceutical grade titanium dioxide and pharmaceutical grade glycerol mix homogeneously, then add citric acid adjust ph between 3.5 ~ 4.5;
Step 2, be then placed in grinding type super micron mill pulverizing of milling, namely obtain selenium sulfide composite superfine powder body.
5. the preparation method of selenium sulfide ultrafine powder according to claim 4, is characterized in that the mass ratio of selenium sulfide dry powder in step one, purified water, pharmaceutical grade titanium dioxide and pharmaceutical grade glycerol is 1:1:2:3.
6. the preparation method of selenium sulfide ultrafine powder according to claim 4, is characterized in that carrying out at power 1.5kW, the speed of mainshaft 1500r/min pulverizing of milling in step 2.
7. the preparation method of selenium sulfide composite superfine powder body according to claim 4, the grinding time that it is characterized in that milling in step 2 is 30min ~ 60min.
CN201510880617.1A 2015-12-03 2015-12-03 Selenium disulfide ultrafine powder and preparation method thereof Active CN105456287B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109310665A (en) * 2016-04-14 2019-02-05 阿祖拉眼科有限公司 For treating the selenium disulfide composition of meibomian gland dysfunction
CN113620258A (en) * 2021-07-14 2021-11-09 郑小青 Selenium sulfide composite powder for hair washing
CN114010514A (en) * 2021-10-08 2022-02-08 大有药业扬州有限公司 Micronized selenium disulfide active antifungal lotion
CN114788788A (en) * 2022-05-09 2022-07-26 无锡知妍生物科技有限公司 Selenium sulfide wrapping technology and selenium sulfide shampoo
US11517586B2 (en) 2020-01-10 2022-12-06 Azura Ophthalmics Ltd. Instructions for composition and sensitivity
US11633410B2 (en) 2014-10-19 2023-04-25 Azura Ophthalmics Ltd Compositions and methods for the treatment of meibomian gland dysfunction

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CN102060277A (en) * 2010-11-25 2011-05-18 广东先导稀有材料股份有限公司 Production method of selenium sulfide

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CN102060277A (en) * 2010-11-25 2011-05-18 广东先导稀有材料股份有限公司 Production method of selenium sulfide

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11633410B2 (en) 2014-10-19 2023-04-25 Azura Ophthalmics Ltd Compositions and methods for the treatment of meibomian gland dysfunction
CN109310665A (en) * 2016-04-14 2019-02-05 阿祖拉眼科有限公司 For treating the selenium disulfide composition of meibomian gland dysfunction
US11040062B2 (en) 2016-04-14 2021-06-22 Azura Ophthalmics Ltd. Selenium disulfide compositions for use in treating meibomian gland dysfunction
US11517586B2 (en) 2020-01-10 2022-12-06 Azura Ophthalmics Ltd. Instructions for composition and sensitivity
CN113620258A (en) * 2021-07-14 2021-11-09 郑小青 Selenium sulfide composite powder for hair washing
CN114010514A (en) * 2021-10-08 2022-02-08 大有药业扬州有限公司 Micronized selenium disulfide active antifungal lotion
CN114010514B (en) * 2021-10-08 2022-10-14 张志昂 Antifungal selenium disulfide lotion composition
WO2023056732A1 (en) 2021-10-08 2023-04-13 张志昂 Product for treating skin fungi and micronized preparation method therefor
CN114788788A (en) * 2022-05-09 2022-07-26 无锡知妍生物科技有限公司 Selenium sulfide wrapping technology and selenium sulfide shampoo

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