CN111035654A - Preparation method of crospovidone-hydrogen peroxide complex - Google Patents

Preparation method of crospovidone-hydrogen peroxide complex Download PDF

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Publication number
CN111035654A
CN111035654A CN201911400071.XA CN201911400071A CN111035654A CN 111035654 A CN111035654 A CN 111035654A CN 201911400071 A CN201911400071 A CN 201911400071A CN 111035654 A CN111035654 A CN 111035654A
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China
Prior art keywords
hydrogen peroxide
crospovidone
complex
mixing
controlled
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CN201911400071.XA
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Chinese (zh)
Inventor
程跃光
吴璟
戴徽
汪菲
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Huangshan Bonsun Pharmaceuticals Co ltd
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Huangshan Bonsun Pharmaceuticals Co ltd
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Priority to CN201911400071.XA priority Critical patent/CN111035654A/en
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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
    • A61K9/70Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
    • A61K9/7007Drug-containing films, membranes or sheets
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/40Peroxides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/50Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
    • A61K47/51Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent
    • A61K47/56Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an organic macromolecular compound, e.g. an oligomeric, polymeric or dendrimeric molecule
    • A61K47/58Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an organic macromolecular compound, e.g. an oligomeric, polymeric or dendrimeric molecule obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. poly[meth]acrylate, polyacrylamide, polystyrene, polyvinylpyrrolidone, polyvinylalcohol or polystyrene sulfonic acid resin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/02Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents

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  • Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Public Health (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Engineering & Computer Science (AREA)
  • Epidemiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dermatology (AREA)
  • Communicable Diseases (AREA)
  • Oncology (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention provides a preparation method of a crospovidone hydrogen peroxide complex, which comprises the following steps: taking the crospovidone and the aqueous solution of hydrogen peroxide, placing the crospovidone and the aqueous solution of hydrogen peroxide in a mixing and stirring kettle, fully mixing and heating to prepare the wet particles of the crospovidone-hydrogen peroxide complex, and performing flash evaporation drying on the mixed complex for 2-12 hours to obtain the wet particles of the crospovidone-hydrogen peroxide complex, wherein the mixing temperature is controlled to be 45-95 ℃, the heating time is controlled to be 2-12 hours, the particle size of the crospovidone is 5-100 micrometers, and the flash evaporation drying temperature is controlled to be 90-. The cross-linked povidone is added into aqueous hydrogen peroxide solution for mixing reaction, and the cross-linked povidone hydrogen peroxide complex particles are obtained by flash evaporation and drying under the conditions of specific reaction time and temperature. When contacted with an excess of water, the hydrogen peroxide is slowly released, reducing irritation to the skin and mucous membranes.

Description

Preparation method of crospovidone-hydrogen peroxide complex
Technical Field
The invention belongs to the technical field of complex preparation, and particularly relates to a preparation method of a crospovidone hydrogen peroxide complex.
Background
The crospovidone-hydrogen peroxide complex is a hydrogen bond complex of a crosslinked vinylpyrrolidone-based polymer and hydrogen peroxide. Pyrrolidone is a five-membered lactam ring and carbonyl is a strong hydrogen bond acceptor. Since hydrogen peroxide is a strong hydrogen bond donor, it forms a stable complex with pyrrolidone, is insoluble in water and other solvents, however, it rapidly swells in the presence of water.
Disclosure of Invention
The invention provides a preparation method of a cross-linked povidone hydrogen peroxide complex, which is characterized in that cross-linked povidone is added into a hydrogen peroxide aqueous solution for mixing reaction, and under the conditions of specific reaction duration and temperature, the cross-linked povidone hydrogen peroxide complex particles are obtained by flash evaporation and drying. When contacted with an excess of water, the hydrogen peroxide is slowly released, reducing irritation to the skin and mucous membranes. .
To this end, the present invention provides a method for preparing a crospovidone hydrogen peroxide complex, comprising the steps of:
taking the crospovidone and the aqueous solution of hydrogen peroxide, placing the crospovidone and the aqueous solution of hydrogen peroxide in a mixing and stirring kettle for fully mixing and heating to prepare wet granules of the crospovidone-hydrogen peroxide complex, and performing flash evaporation drying on the mixed complex and packaging the mixed complex, wherein the mixing temperature is controlled to be 45-95 ℃, the heating time is 2-12 hours, the particle size of the crospovidone is 5-100 micrometers, and the flash evaporation drying temperature is controlled to be 90-140 ℃.
Preferably, the mixing reaction temperature is 65 to 70 ℃.
Preferably, the heating time is 4 to 8 hours.
Preferably, the heating time is 6 to 7 hours.
Preferably, the flash drying temperature is controlled at 100-120 ℃.
Preferably, the concentration of the aqueous hydrogen peroxide solution is 27% or 30% or 50%.
Preferably, the particle size of the crospovidone particles is 5 to 45 microns.
The invention has the beneficial effects that: the invention discloses a preparation method of a cross-linked povidone hydrogen peroxide complex, and the prepared povidone hydrogen peroxide complex is used for oral care, disinfection of mucous membranes or skin wounds and the like. When contacted with an excess of water, the hydrogen peroxide is slowly released, reducing irritation to the skin and mucous membranes.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. In the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a schematic diagram of the reaction scheme of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Example one
As shown in fig. 1: the preparation method of crospovidone hydrogen peroxide complex of this embodiment includes the following steps:
taking 500KG of crospovidone and 125KG of aqueous hydrogen peroxide, placing the crospovidone and the aqueous hydrogen peroxide into a mixing and stirring kettle, fully mixing and heating the mixture to prepare particles of a crospovidone-hydrogen peroxide complex, and performing flash evaporation drying on the mixed complex and packaging the mixed complex, wherein the mixing temperature is controlled to be 65 ℃, the heating time is 6 hours, the particle size of the crospovidone is 5 microns, the flash evaporation drying temperature is controlled to be 100 ℃, and the hydrogen peroxide content is 5.2%. Wherein the concentration of the aqueous hydrogen peroxide solution is 27%,
example two
Taking 500KG of crospovidone and 220KG of aqueous hydrogen peroxide, placing the crospovidone and the aqueous hydrogen peroxide into a mixing and stirring kettle, fully mixing and heating the mixture to prepare particles of a crospovidone-hydrogen peroxide complex, and carrying out flash evaporation drying on the mixed complex and then packaging the mixed complex, wherein the mixing temperature is controlled to be 70 ℃, the heating time is 7 hours, the particle size of the crospovidone is 45 micrometers, the flash evaporation drying temperature is controlled to be 120 ℃, and the hydrogen peroxide content is 9.5 percent. Wherein the concentration of the aqueous hydrogen peroxide solution is 30%.
EXAMPLE III
Taking 500KG of crospovidone and 300KG of aqueous hydrogen peroxide, placing the crospovidone and the aqueous hydrogen peroxide into a mixing and stirring kettle, fully mixing and heating the mixture to prepare particles of a crospovidone-hydrogen peroxide complex, and performing flash evaporation drying and packaging on the mixed complex, wherein the mixing temperature is controlled to be 65 ℃, the heating time is 7 hours, the particle size of the crospovidone is 30 micrometers, the flash evaporation drying temperature is controlled to be 120 ℃, and the content of hydrogen peroxide in the obtained crosslinked povidone-hydrogen peroxide complex is 18.3%, and the concentration of the aqueous hydrogen peroxide is 50%.
Example four
Taking 500KG of crospovidone and 430KG of aqueous hydrogen peroxide, placing the crospovidone and the aqueous hydrogen peroxide in a mixing and stirring kettle, fully mixing and heating the mixture to prepare particles of a crospovidone-hydrogen peroxide complex, and performing flash evaporation drying and packaging on the mixed complex, wherein the mixing temperature is controlled to be 65 ℃, the heating time is 7 hours, the particle size of the crospovidone is 30 micrometers, the flash evaporation drying temperature is controlled to be 120 ℃, and the content of hydrogen peroxide is 22.1%, wherein the concentration of the aqueous hydrogen peroxide is 50%.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.

Claims (8)

1. A method for preparing a crospovidone-hydrogen peroxide complex, comprising the steps of:
taking the crospovidone and the aqueous solution of hydrogen peroxide, placing the crospovidone and the aqueous solution of hydrogen peroxide in a mixing and stirring kettle, fully mixing and heating to prepare wet particles of the crospovidone and the hydrogen peroxide, and performing flash evaporation drying on the mixed complex for 2-12 hours at 45-95 ℃, wherein the particle size of the crospovidone is 5-100 microns, and the flash evaporation drying temperature is controlled at 90-140 ℃.
2. The method of claim 1, wherein the mixing temperature is 65-70 ℃.
3. The method of claim 2, wherein the heating time is 4-8 hours.
4. The method of claim 2, wherein the heating time is 6-7 hours.
5. The method for preparing crospovidone hydrogen peroxide as set forth in any one of claims 1 to 4, wherein the flash drying temperature is controlled to 100-120 ℃.
6. The method of claim 5, wherein the aqueous hydrogen peroxide solution has a concentration of 27% or 30% or 50%.
7. The method of claim 6, wherein the amount of the aqueous hydrogen peroxide solution minus water is 5-30% of the crospovidone.
8. The method of claim 6, wherein the particle size of the crospovidone particles is 5-45 microns.
CN201911400071.XA 2019-12-30 2019-12-30 Preparation method of crospovidone-hydrogen peroxide complex Pending CN111035654A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564609A (en) * 2021-06-09 2021-10-29 湖北中油优艺环保科技集团有限公司 Efficient scale remover for incineration system and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3376110A (en) * 1967-01-30 1968-04-02 Gen Aniline & Film Corp Solid stabilized hydrogen peroxide compositions
WO1993021931A1 (en) * 1992-04-30 1993-11-11 Isp Investments Inc. Strongly swellable, moderately crosslinked polyvinylpyrrolidone
US5312619A (en) * 1992-04-30 1994-05-17 Isp Investments Inc. Aqueous stable complex of a strongly swellable, moderately crosslinked polyvinylpyrrolidone and hydrogen peroxide
US6083408A (en) * 1993-12-17 2000-07-04 Basf Aktiengesellschaft And Schenk Filterbau Gmbh Depth-type filter for killing microorganisms and inactivating viruses which comprises a fibrous material and crospovidone-iodine and its use
CN110035736A (en) * 2016-12-06 2019-07-19 高露洁-棕榄公司 Oral care composition and application method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3376110A (en) * 1967-01-30 1968-04-02 Gen Aniline & Film Corp Solid stabilized hydrogen peroxide compositions
WO1993021931A1 (en) * 1992-04-30 1993-11-11 Isp Investments Inc. Strongly swellable, moderately crosslinked polyvinylpyrrolidone
US5312619A (en) * 1992-04-30 1994-05-17 Isp Investments Inc. Aqueous stable complex of a strongly swellable, moderately crosslinked polyvinylpyrrolidone and hydrogen peroxide
US6083408A (en) * 1993-12-17 2000-07-04 Basf Aktiengesellschaft And Schenk Filterbau Gmbh Depth-type filter for killing microorganisms and inactivating viruses which comprises a fibrous material and crospovidone-iodine and its use
CN110035736A (en) * 2016-12-06 2019-07-19 高露洁-棕榄公司 Oral care composition and application method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564609A (en) * 2021-06-09 2021-10-29 湖北中油优艺环保科技集团有限公司 Efficient scale remover for incineration system and preparation method thereof

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Application publication date: 20200421