CN106074396A - A kind of method preparing potassium permanganate particles - Google Patents

A kind of method preparing potassium permanganate particles Download PDF

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CN106074396A
CN106074396A CN201610695409.9A CN201610695409A CN106074396A CN 106074396 A CN106074396 A CN 106074396A CN 201610695409 A CN201610695409 A CN 201610695409A CN 106074396 A CN106074396 A CN 106074396A
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potassium permanganate
particles
preparation
permanganate particles
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CN106074396B (en
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米金国
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Ji'nan Kangfusheng Pharmaceutical Co Ltd
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    • 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
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1617Organic compounds, e.g. phospholipids, fats
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/24Heavy metals; Compounds thereof
    • A61K33/32Manganese; Compounds thereof
    • 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
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • 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
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682Processes

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Abstract

The invention provides a kind of method preparing potassium permanganate particles, described method comprises the steps: S1: Feedstock treating: prepare saturated potassium permanganate solution, sucking filtration or filter with filter paper, takes filtrate;S2: be dried: decompression is distilled off moisture, obtains semiarid potassium permanganate;S3: add adjuvant, mix homogeneously under agitation;S4: making particle diameter is the 10~20 little granules of purpose, and magnesium stearate is uniformly sprinkled in comminutor during preparing this little granule;S5: preparation potassium permanganate particles;S6: be dried and sterilization treatment.The formed product rate of the potassium permanganate particles in the present invention is high, and the qualification rate of product has reached more than 99%, has extremely important industrial application value.

Description

A kind of method preparing potassium permanganate particles
Technical field
The present invention relates to field of medicaments, be specifically related to a kind of method preparing potassium permanganate particles.
Background technology
Widely, it has oxidisability in the application of potassium permanganate, is pharmaceutically being often used as preservative, disinfectant, is removing Smelly dose and antidote.Potassium permanganate has killing action to pathogenic microorganism such as various antibacterials, funguses, is usually used in acute dermatitis or urgency Property eczema soak, clean burst skin ulcer and hemorrhoid demibain, it is also possible to for the urinary tract infection etc. of women.
But the dosage form of potassium permanganate is based on tablet at present, and the moulding process of tablet is relatively complicated, and ratio of briquetting is low; Certainly, currently also there is a small amount of potassium permanganate particles, but the preparation technology of granule is traditional, simply raw material is mixed all with dressing Even directly carrying out pelletize, the ratio of briquetting causing finished particle is the most relatively low, and gained granule is easily broken and slight crack occurs, because of This, cause the application of potassium permanganate particles to be extremely limited.
Summary of the invention
The defect that the present invention is directed to prior art provides a kind of method preparing potassium permanganate particles.
It is an object of the invention to be achieved through the following technical solutions:
A kind of method preparing potassium permanganate particles, described method comprises the steps:
S1: Feedstock treating: potassium permanganate powder is dissolved in deionized water under agitation and obtains saturated permanganic acid Potassium solution, carries out saturated potassium permanganate solution sucking filtration or filters with filter paper, taking filtrate;
S2: be dried: the filtrate obtained in step S1 is distilled off moisture by decompression, until water content is 2%~8% Time till, then obtain semiarid potassium permanganate;
S3: add agitating device in the semiarid potassium permanganate obtained in step s 2, add auxiliary under agitation Material, described adjuvant is boric acid and hydroxypropyl cellulose, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 10~20 little granules of purpose, and in system During this little granule standby, magnesium stearate is uniformly sprinkled in comminutor;
S5: little granule prepared in step S4 is put into the potassium permanganate making required specification in the second comminutor Grain;
S6: the potassium permanganate particles prepared by step S5 is dried and sterilization treatment.
S7: pack, check, put in storage.
Further, the addition of described magnesium stearate is the 0.5~2.5% of potassium permanganate quality, more preferably 1.1~ 1.5%.
Further, the filtrate described in step S2 is distilled off moisture by decompression, until when water content is 6% being Only.
Further, the addition of the boric acid described in step S3 is the 0.5~1% of potassium permanganate quality, described hydroxypropyl The addition of base cellulose is the 0.3~0.8% of potassium permanganate quality.
Further, the adjuvant described in step S3 also includes fatty acid esters of sorbitan.
Further, the addition of described fatty acid esters of sorbitan is the 0.3~0.8% of potassium permanganate quality.
Further, the adjuvant described in step S3 also includes quick-dissolving agent.
Further, the addition of described quick-dissolving agent is the 0.3~0.5% of potassium permanganate quality.
The method have the advantages that
1. potassium permanganate was made saturated solution and is carried out filtration treatment, energy again before preparation potassium permanganate particles by the present invention Enough remove the most of impurity in the presence of potassium permanganate material powder, significantly improve the purity of potassium permanganate so that it is system The purity of the potassium permanganate particles become also improves, then effectively prevent impurity to the impact existing for potassium permanganate therapeutic effect;
2. the present invention first prepares little granule, less granule is made the potassium permanganate particles of required specification, the most greatly Improve the ratio of briquetting of granule and the qualification rate of product;And prepared particle stabilized, do not have any slight crack etc..
3. during preparing little granule, uniformly it is sprinkled into magnesium stearate, then substantially reduces each other during making to prepare granule Bind, further increase shaping speed and the ratio of briquetting of potassium permanganate particles;
4. after raw material and adjuvant are sufficiently mixed by the present invention, in certain water content, carry out short grained preparation, increase Add the adhesion of raw material and adjuvant, thus improved its ratio of briquetting, decreased broken granule or have slight crack granule;
5. the present invention improves the efficiency that potassium permanganate produces, and reduces the mill that machine brings because fragment repeats preparation Damage, extend machine service life, reduce production cost.
In a word, the production of potassium permanganate particles of the present invention can make formed product rate improve more than 20%, product qualified Rate has reached more than 99%, has extremely important industrial application value.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, specifically real below in conjunction with the present invention Execute example technical scheme is clearly and completely described, it is clear that described embodiment is that a part of the present invention is real Execute example rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation The every other embodiment obtained under property work premise, broadly falls into the scope of protection of the invention.
Embodiment 1
A kind of method preparing potassium permanganate particles described in the embodiment of the present invention, specifically comprises the following steps that
S1: Feedstock treating: at room temperature, is dissolved in deionized water under agitation by 10kg potassium permanganate powder, And the saturated potassium permanganate solution under prepared room temperature condition, saturated potassium permanganate solution is at room temperature used filter paper mistake Filter, removes and does not allows impurity, take filtrate;Above-mentioned stirring condition, for using motor stirrer stirring, so can stir more fully Mix uniformly;
S2: be dried: by the filtrate in step S1 by decompression distillation moisture removal, when water content is 4% till, then To semiarid potassium permanganate;
S3: add agitating device in the most semiarid potassium permanganate, add 0.06kg's under agitation Boric acid and the hydroxypropyl cellulose of 0.07kg, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 15 little granules of purpose, and should in preparation During little granule, 0.12kg magnesium stearate is uniformly sprinkled in comminutor, until completing pelletize;The addition of magnesium stearate makes Substantially reduce during preparing granule and bind each other, contribute to the molding of potassium permanganate particles;
S5: little granule prepared in step S4 is put in the second comminutor and makes potassium permanganate particles;
S6: the potassium permanganate particles prepared by step S5 is dried in the baking oven of 100 degrees Celsius, uses the most again Ultraviolet carries out sterilization treatment.
S7: pack, check, put in storage.
Embodiment 2
A kind of method preparing potassium permanganate particles described in the embodiment of the present invention, specifically comprises the following steps that
S1: Feedstock treating: at room temperature 10kg potassium permanganate powder is dissolved in deionized water under agitation, and Prepare the saturated potassium permanganate solution under room temperature condition, saturated potassium permanganate solution is at room temperature filtered with filter paper, removes Do not allow impurity, take filtrate;Above-mentioned stirring condition, for using motor stirrer stirring, so can stir more fully;
S2: be dried: by the filtrate in step S1 by decompression distillation moisture removal, when water content is 6% till, then To semiarid potassium permanganate;
S3: add agitating device in the most semiarid potassium permanganate, add the boron of 0.7kg under agitation Acid and the hydroxypropyl cellulose of 0.05kg, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 15 little granules of purpose, and should in preparation During little granule, 0.13kg magnesium stearate is uniformly sprinkled in comminutor, until completing pelletize;The addition of magnesium stearate makes Substantially reduce during preparing granule and bind each other, contribute to the molding of potassium permanganate particles;
S5: little granule prepared in step S4 is put into and makes potassium permanganate particles in the second comminutor, all Gao Meng In acid k particle, the content of potassium permanganate is 0.1g ± 7.5%;
S6: the potassium permanganate particles prepared by step S5 is dried in the baking oven of 100 degrees Celsius, uses the most again Ultraviolet carries out sterilization treatment.
S7: pack, check, put in storage.
Embodiment 3
A kind of method preparing potassium permanganate particles described in the embodiment of the present invention, specifically comprises the following steps that
S1: Feedstock treating: at room temperature 10kg potassium permanganate powder is dissolved in deionized water under agitation, and Prepare saturated potassium permanganate solution, saturated potassium permanganate solution is at room temperature carried out sucking filtration, remove and do not allow impurity, take filtrate; Above-mentioned stirring condition, for using motor stirrer stirring, so can stir more fully;
S2: be dried: by the filtrate in step S1 by decompression distillation moisture removal, when water content is 2% till, then To semiarid potassium permanganate;
S3: add agitating device in the most semiarid potassium permanganate, add 0.05kg's under agitation Boric acid, the hydroxypropyl cellulose of 0.08kg and 0.05kg fatty acid esters of sorbitan, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 10 little granules of purpose, and should in preparation During little granule, 0.15kg magnesium stearate is uniformly sprinkled in comminutor, until completing pelletize;
S5: little granule prepared in step S4 is put into and makes potassium permanganate particles in the second comminutor, all Gao Meng In acid k particle, the content of potassium permanganate is 0.1g ± 7.5%;
S6: the potassium permanganate particles prepared by step S5 is dried in the baking oven of 100 degrees Celsius, uses the most again Ultraviolet carries out sterilization treatment.
S7: pack, check, put in storage.
Embodiment 4
A kind of method preparing potassium permanganate particles described in the embodiment of the present invention, specifically comprises the following steps that
S1: Feedstock treating: at room temperature 10kg potassium permanganate powder is dissolved in deionized water under agitation, and Prepare saturated potassium permanganate solution, saturated potassium permanganate solution is at room temperature filtered with filter paper, removes and do not allow impurity, take filter Liquid;Above-mentioned stirring condition, for using motor stirrer stirring, so can stir more fully;
S2: be dried: by the filtrate in step S1 by decompression distillation moisture removal, when water content is 8% till, then To semiarid potassium permanganate;
S3: add agitating device in the most semiarid potassium permanganate, add the boron of 0.1kg under agitation Acid, the hydroxypropyl cellulose of 0.03kg, 0.07kg fatty acid esters of sorbitan and 0.045kg quick-dissolving agent, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 20 little granules of purpose, and should in preparation During little granule, 0.12kg magnesium stearate is uniformly sprinkled in comminutor, until completing pelletize;
S5: little granule prepared in step S4 is put into and makes potassium permanganate particles in the second comminutor, all Gao Meng In acid k particle, the content of potassium permanganate is 0.1g ± 7.5%;
S6: the potassium permanganate particles prepared by step S5 is dried in the baking oven of 100 degrees Celsius, uses the most again Ultraviolet carries out sterilization treatment.
S7: pack, check, put in storage.
Embodiment 5
A kind of method preparing potassium permanganate particles described in the embodiment of the present invention, specifically comprises the following steps that
S1: Feedstock treating: at room temperature 10kg potassium permanganate powder is dissolved in deionized water under agitation, and Preparing the saturated potassium permanganate solution under room temperature condition, saturated potassium permanganate solution at room temperature carries out sucking filtration, removing is not allowed Impurity, takes filtrate;Above-mentioned stirring condition, for using motor stirrer stirring, so can stir more fully;
S2: be dried: by the filtrate in step S1 by decompression distillation moisture removal, when water content is 8% till, then To semiarid potassium permanganate;
S3: add agitating device in the most semiarid potassium permanganate, add 0.08kg's under agitation Boric acid, the hydroxypropyl cellulose of 0.06kg and 0.035kg quick-dissolving agent, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 15 little granules of purpose, and should in preparation During little granule, 0.12kg magnesium stearate is uniformly sprinkled in comminutor, until completing pelletize;The addition of magnesium stearate makes Substantially reduce during preparing granule and bind each other, contribute to the molding of potassium permanganate particles;
S5: little granule prepared in step S4 is put into and makes potassium permanganate particles in the second comminutor, all Gao Meng In acid k particle, the content of potassium permanganate is 0.1g ± 7.5%;
S6: the potassium permanganate particles prepared by step S5 is dried in the baking oven of 100 degrees Celsius, uses the most again Ultraviolet carries out sterilization treatment.
S7: pack, check, put in storage.
In potassium permanganate particles in embodiment 1~5, the content of potassium permanganate can be 0.1g ± 7.5%, and specific size can Depending on practical situation.
Embodiment 6
Experimental project: the molding qualification rate of test potassium permanganate particles;
Experimental group: embodiment 1~5 is experimental group;
Matched group: to apply wider prior art as a control group at present, in matched group prepared by potassium permanganate particles Cheng Wei: weigh 10kg potassium permanganate raw material, and to weigh 0.08kg boric acid with 0.06kg hydroxypropyl cellulose be adjuvant, is sufficiently mixed Uniformly, then pelletize in comminutor, obtain finished product potassium permanganate particles, size is identical with experimental group.
Experimental technique: adding up the formed product qualification rate in experimental group and matched group, result is as shown in table 1.
Table 1 matched group and the formed product rate of potassium permanganate particles in experimental group
Compression molding rate (%)
Matched group 75.23
Embodiment 1 99.72
Embodiment 2 99.03
Embodiment 3 99.14
Embodiment 4 99.08
Embodiment 5 99.02
Conclusion: as shown in Table 1, the formed product rate of the potassium permanganate particles produced in embodiment of the present invention 1-5 all exists More than 99%, exceed more than 20% than matched group, therefore, present invention greatly enhances the ratio of briquetting of potassium permanganate particles, Save technique, reduce cost.
Embodiment 7
The dissolution velocity of test potassium permanganate particles.
Experimental group: embodiment 1~5 is experimental group;
Matched group: with the wider prior art of at present application to matched group, potassium permanganate particles preparation process in matched group For: weigh 10kg potassium permanganate raw material, and to weigh 0.08kg boric acid with 0.06kg hydroxypropyl cellulose be adjuvant, be sufficiently mixed all Even, then pelletize in comminutor, obtain finished product potassium permanganate particles, size is identical with experimental group.
Experimental technique: in experimental group and matched group, the dissolving method of potassium permanganate particles is: by a potassium permanganate Grain be placed on volume be 20mL, temperature be that in the deionized water of 40 degrees Celsius, the height of deionized water did not had potassium permanganate completely Grain.Record potassium permanganate particles is completely dissolved the required time, and the result of dissolution velocity is as shown in table 2.
Table 2 matched group and the dissolution velocity of potassium permanganate particles in experimental group
Dissolution velocity
Matched group 9 points 38 seconds
Embodiment 1 9 points 37 seconds
Embodiment 2 9 points 26 seconds
Embodiment 3 9 points 30 seconds
Embodiment 4 5 points 44 seconds
Embodiment 5 5 points 28 seconds
Conclusion: as shown in Table 2, after embodiment 4 and 5 adds a certain amount of quick-dissolving agent, the dissolving speed of potassium permanganate particles Rate is substantially accelerated, and decreases the time that user waits, reduces potassium permanganate particles ingress of air in course of dissolution simultaneously And there is the phenomenons such as oxidation.
It should be noted that all result of the tests are the meansigma methods repeating experiment 3 times in embodiment 6 and 7.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, Any those skilled in the art in the technical scope that the invention discloses, the change that can readily occur in or replacement, All should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Enclose and be as the criterion.

Claims (9)

1. the method preparing potassium permanganate particles, it is characterised in that described method comprises the steps:
S1: potassium permanganate powder is dissolved in deionized water under agitation and obtains saturated potassium permanganate solution, by saturated Saturated potassium permanganate solution carries out sucking filtration or filters with filter paper, takes filtrate;
S2: the filtrate obtained in step S1 is distilled off moisture by decompression, when water content is 2%~8% till, then Obtain semiarid potassium permanganate;
S3: add agitating device in the semiarid potassium permanganate obtained in step s 2, add adjuvant, institute under agitation Stating adjuvant is boric acid and hydroxypropyl cellulose, mix homogeneously;
S4: using the first comminutor to make particle diameter in step S3 after mix homogeneously is the 10~20 little granules of purpose, and should in preparation During little granule, magnesium stearate is uniformly sprinkled in comminutor;
S5: little granule prepared in step S4 is put into the potassium permanganate particles making required specification in the second comminutor;
S6: the potassium permanganate particles prepared by step S5 is dried and sterilization treatment.
The method of preparation potassium permanganate particles the most according to claim 1, it is characterised in that the tristearin described in step S4 Addition is potassium permanganate quality the 0.5~2.5% of acid magnesium.
The method of preparation potassium permanganate particles the most according to claim 2, it is characterised in that the addition of described magnesium stearate Amount is the 1.1~1.5% of potassium permanganate quality.
The method of preparation potassium permanganate particles the most according to claim 1, it is characterised in that the filtrate described in step S2 Moisture is distilled off by decompression, when water content is 6% till.
The method of preparation potassium permanganate particles the most according to claim 1, it is characterised in that the boric acid described in step S3 Addition is potassium permanganate quality 0.5~1%, the addition of described hydroxypropyl cellulose is the 0.3 of potassium permanganate quality ~0.8%.
The method of preparation potassium permanganate particles the most according to claim 1, it is characterised in that the adjuvant described in step S3 Also include fatty acid esters of sorbitan.
The method of preparation potassium permanganate particles the most according to claim 6, it is characterised in that described sorbitane fatty The addition of acid esters is the 0.3~0.8% of potassium permanganate quality.
The method of preparation potassium permanganate particles the most according to claim 1, it is characterised in that the adjuvant described in step S3 Also include quick-dissolving agent.
The method of preparation potassium permanganate particles the most according to claim 8, it is characterised in that the addition of described quick-dissolving agent For potassium permanganate quality 0.3~0.5%.
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CN116143176A (en) * 2022-11-22 2023-05-23 广西汇元锰业有限责任公司 Method for preparing manganous-manganic oxide

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