CN104448083A - Preparation method of medical-grade polyvinylpyrrolidone K90 - Google Patents
Preparation method of medical-grade polyvinylpyrrolidone K90 Download PDFInfo
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- CN104448083A CN104448083A CN201410799267.1A CN201410799267A CN104448083A CN 104448083 A CN104448083 A CN 104448083A CN 201410799267 A CN201410799267 A CN 201410799267A CN 104448083 A CN104448083 A CN 104448083A
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- polyvinylpyrrolidone
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920006316 polyvinylpyrrolidine Polymers 0.000 title abstract 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920003081 Povidone K 30 Polymers 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 abstract description 5
- 239000003999 initiator Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
- UYMKPFRHYYNDTL-UHFFFAOYSA-N ethenamine Chemical compound NC=C UYMKPFRHYYNDTL-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract 2
- 231100000419 toxicity Toxicity 0.000 abstract 2
- 239000002861 polymer material Substances 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920003082 Povidone K 90 Polymers 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a polyvinylpyrrolidone, namely PVP for short. The polyvinylpyrrolidone is a nonionic polymeric compound, and is the most characteristic fine chemical variety which is researched the deepest and the most widely in N-vinyl amide polymers. The polyvinylpyrrolidone belongs to the technical field of polymerization of high polymer materials, and particularly relates to a preparation method of medical-grade polyvinylpyrrolidone K90. The problems that an initiator polymerized by the existing polyvinylpyrrolidone K90 has toxicity, and is not suitable for production of the medical-grade polyvinylpyrrolidone K90 are solved. By adopting the initiator which is free of toxicity on a human body, the preparation method is simple in production process, convenient for post-treatment, nontoxic and harmless; the cost of the product is greatly reduced; and the preparation method is suitable for the production of the medical-grade polyvinylpyrrolidone K90.
Description
Technical field
The invention belongs to the polymerization technique field of macromolecular material, be specifically related to the preparation method of a kind of medicinal polyvinylpyrrolidonewith K90.
Background technology
Polyvinylpyrrolidone (polyvinyl pyrrolidone) is called for short PVP, is a kind of non-ionic macromolecule compound, is most characteristic in N-vinylamide polymer, and be studied the most deeply, fine chemicals kind widely.Nonionic, positively charged ion, the large class of negatively charged ion 3 are developed into, technical grade, pharmaceutical grade, food grade 3 kinds of specifications, relative molecular mass from thousands of to more than 1,000,000 homopolymer, multipolymer and crosslinking series of polymers product, and obtain widespread use with its excellent unique performance.
PVP has excellent physiological inertia, does not participate in human metabolism, has again excellent biocompatibility, does not form any stimulation to skin, mucous membrane, eye etc.From biological viewpoint, the molecular structure characteristic of PVP is similar to that structure with simple protein model, even it water-soluble to some micromolecular mating capability and can by the precipitation agent ammonium sulfate of some protein, trichoroacetic acid(TCA), tannic acid and phenols the characteristic such as to precipitate and also mix with protein.So that make PVP be widely used as the auxiliary material of pharmaceutical preparation.
PVP is divided into level Four by its molecular-weight average size, often traditionally represents with K value, and different K values represents corresponding PVP average molecular weight range respectively.Compare in the market common are K15, K30, K50, K90 wherein PVP K30 included by Chinese Pharmacopoeia in 2010 years.
Because K90 molecular weight is comparatively large, polyreaction generally adopts azo-compound as initiator, and azo-compound is generally poisonous to human body, can not use in medicine, and this just greatly limit the purposes of K90 in medicine on existing market.
Summary of the invention
Utilize V-Pyrol RC to prepare a method for medicinal 30 POVIDONE K 30 BP/USP 90, it is characterized in that:
Raw material mass mixture ratio is:
V-Pyrol RC massfraction is 100 parts;
Deionized water quality mark 100 parts;
The massfraction of hydrogen peroxide: when concentration is 26%-32%, 1.4-1.8 part;
Ammoniacal liquor massfraction: when concentration is 24%-28%, 0.3-0.7 part;
Preparation technology:
Deionized water 100 mass fraction is added in polymerization reaction kettle, be warming up to 50 DEG C, the V-Pyrol RC stirring velocity adding mass fraction 100 is again per minute 120-150 turns, when temperature is raised to 70 DEG C, add the ammoniacal liquor of 0.3-0.7 part when concentration is 24%-28%, then add the hydrogen peroxide initiation reaction of 1.4-1.8 part when concentration is 26%-32%.Keep 70 DEG C to react 4 hours, polymeric solution is spray-dried obtains powdery K90.
Advantage of the present invention have employed the hydrogen peroxide that very easily removes as initiator, and production process is simple, and convenient post-treatment, greatly reduces the cost of product, and nontoxic, is applicable to the production of pharmaceutical grade medicine auxiliary material.Product of the present invention meets the requirement of the pharmacopeia such as Europe, the U.S..
embodiment:
Deionized water 100kg is added in polymerization reaction kettle, be warming up to 50 DEG C, the V-Pyrol RC adding 100 kg again stirs, stirring velocity is per minute 120-150 turns, when temperature is raised to 70 DEG C, add the ammoniacal liquor of 0.3-0.7 kg when concentration is 24%-28%, then add the hydrogen peroxide initiation reaction of 1.4-1.8 kg when concentration is 26%-32%.Keep 70 DEG C to react 4 hours, polymeric solution is spray-dried obtains powdery K90.
Below the assay of PVP K90 five embodiments:
| Sequence number | Level of residual monomers | Aldehyde | K value | Solid content (calculating with nitrogen content) |
| 1 | 0.0002% | 0.02% | 89.7 | 12.3% |
| 2 | 0.0003% | 0.03% | 90.5 | 12.4% |
| 3 | 0.0002% | 0.02% | 91.3 | 11.9% |
| 4 | 0.0001% | 0.02% | 90.5 | 12.1% |
| 5 | 0.0003% | 0.03% | 90.7 | 12.0% |
| Standard is limited the quantity | Be not more than 0.001% | Be not more than 0.05% | 87-93 | 11.5%-12.8% |
Obviously, the above embodiment of the present invention is only and clearly demonstrates example of the present invention, and not limits enforcement of the present invention.For those of ordinary skill in the field, other different changes can also be made on the basis of the above description, cannot give all embodiments exhaustive at this.Everyly belong to the apparent change that technical scheme of the present invention amplifies and be still within scope.
Claims (1)
1. utilize V-Pyrol RC to prepare a method for medicinal 30 POVIDONE K 30 BP/USP 90, it is characterized in that:
Raw material mass mixture ratio is:
V-Pyrol RC massfraction is 100 parts;
Deionized water quality mark 100 parts;
The massfraction of hydrogen peroxide: when concentration is 26%-32%, 1.4-1.8 part;
Ammoniacal liquor massfraction: when concentration is 24%-28%, 0.3-0.7 part;
Preparation technology:
Deionized water 100 mass fraction is added in polymerization reaction kettle, be warming up to 50 DEG C, the V-Pyrol RC adding mass fraction 100 again stirs, stirring velocity is per minute 120-150 turns, when temperature is raised to 70 DEG C, add the ammoniacal liquor of 0.3-0.7 part when concentration is 24%-28%, then add the hydrogen peroxide initiation reaction of 1.4-1.8 part when concentration is 26%-32%, keep 70 DEG C to react 4 hours, polymeric solution is spray-dried obtains powdery K90.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410799267.1A CN104448083A (en) | 2014-12-22 | 2014-12-22 | Preparation method of medical-grade polyvinylpyrrolidone K90 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410799267.1A CN104448083A (en) | 2014-12-22 | 2014-12-22 | Preparation method of medical-grade polyvinylpyrrolidone K90 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104448083A true CN104448083A (en) | 2015-03-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410799267.1A Pending CN104448083A (en) | 2014-12-22 | 2014-12-22 | Preparation method of medical-grade polyvinylpyrrolidone K90 |
Country Status (1)
| Country | Link |
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| CN (1) | CN104448083A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906768A (en) * | 2016-04-20 | 2016-08-31 | 贵州省欣紫鸿药用辅料有限公司 | Synthesis method of crospovidone |
| CN106543361A (en) * | 2015-09-23 | 2017-03-29 | 南京紫鸿生物科技有限公司 | A kind of method for preparing pharmaceutic adjuvant polyvinylpolypyrrolidone |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4786699A (en) * | 1985-09-13 | 1988-11-22 | Basf Aktiengesellschaft | Preparation of polyvinylpyrrolidone |
-
2014
- 2014-12-22 CN CN201410799267.1A patent/CN104448083A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4786699A (en) * | 1985-09-13 | 1988-11-22 | Basf Aktiengesellschaft | Preparation of polyvinylpyrrolidone |
Non-Patent Citations (1)
| Title |
|---|
| 严瑞瑄主编: "《水溶性高分子》", 31 July 2010, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543361A (en) * | 2015-09-23 | 2017-03-29 | 南京紫鸿生物科技有限公司 | A kind of method for preparing pharmaceutic adjuvant polyvinylpolypyrrolidone |
| CN105906768A (en) * | 2016-04-20 | 2016-08-31 | 贵州省欣紫鸿药用辅料有限公司 | Synthesis method of crospovidone |
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Application publication date: 20150325 |
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