CN106883333B - A kind of preparation method of big grain size crospovidone - Google Patents
A kind of preparation method of big grain size crospovidone Download PDFInfo
- Publication number
- CN106883333B CN106883333B CN201710235124.1A CN201710235124A CN106883333B CN 106883333 B CN106883333 B CN 106883333B CN 201710235124 A CN201710235124 A CN 201710235124A CN 106883333 B CN106883333 B CN 106883333B
- Authority
- CN
- China
- Prior art keywords
- crospovidone
- grain size
- preparation
- big grain
- mixing speed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F126/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F126/06—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
- C08F126/10—N-Vinyl-pyrrolidone
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation methods of big grain size crospovidone, in monomer NVP:The mass ratio of water is 9:Under conditions of 1,3.0% alkali metal hydroxide is added, is passed through nitrogen protection, is heated to 55 DEG C and causes progress Popcorn Polymerization, 60 revs/min of mixing speed；When temperature rise is to 70 DEG C, 0.5%~5.0% forming agent is added, while reducing mixing speed to 20 revs/min；After grain forming, by washing drying, grain size crospovidone between 140~200 μm is finally obtained；Forming agent is generally at least one of tert-butyl hydroperoxide, benzoyl peroxide, di-tert-butyl peroxide, azodiisobutyronitrile, peroxidized t-butyl perbenzoate.The present invention is changed surface tension when grain forming, so that it is suspended in the form of larger particles in water phase, part of the particle size between 140~200 μm is made to account for 80% or more by adding forming agent in the course of the polymerization process.
Description
Technical field
The present invention relates to a kind of chemicals preparation method, more particularly to a kind of preparation method of big grain size crospovidone,
Belong to pharmaceutic adjuvant technical field.
Background technology
Crospovidone（PVPP）, it is the povidone strand by line style, is mutually handed over by physical method and chemical method
It is a kind of high-crosslinking-degree made of connection, the product with good physiological inertia and adsorptivity, PVPP has different in water
Swelling Capacity, the form showed can be soft gel, white powder or porous granule.Itself not soluble in water and various acid
Property, alkaline solution, have good physiological security.It is numerous that cross-linked pvp has been applied to wine brewing, beverage and medicine bioengineering etc.
Field.It may be used as the fining agent of plant type beverage, the disintegrant of drug, the thickener and flocculant of dispersion, absorption
Agent etc..
The preparation of traditional crospovidone is to pass through n-vinyl pyrrolidone（NVP）Copolymerization with self-crosslinking agent comes real
It is existing, NVP and suitable crosslinking agent are subjected to precipitation polymerization in electrolyte aqueous solution, the product of generation is filtered, washed,
It is the NVP cross-linked polymers of porous and granular after drying.Highly cross-linked crospovidone product is prepared, Popcorn Polymerization is selected
（Also known as proliferous polymerization）Mode carries out.
But in traditional PVPP preparation processes, the size tunable range of PVPP is smaller, can only be controlled substantially less than 150 μm
In the range of, PVPP is significantly limited in this way and is being made wine and the application effect as fining agent, stabilizer in beverage industry, together
When the number that can reuse it is less, cause the waste of resource.
Invention content
Place in view of the shortcomings of the prior art, the present invention are led to by the way of adding forming agent in the course of the polymerization process
Surface tension when changing grain forming is crossed, makes it that can suspend in the form of larger particles in water phase, makes product PVPP
Part of the diameter between 140~200 μm accounts for 80% or more.
The purpose of the invention is achieved by the following technical solution：
A kind of preparation method of big grain size crospovidone, includes the following steps：
S1, a certain amount of monomer NVP, water are mixed；
S2, alkali metal hydroxide is added into the mixture of step S1, is passed through nitrogen protection；
S3, mixture obtained by step S2 is stirred and is heated to 55 DEG C, initiation Popcorn Polymerization；
S4, when the mixture temperature of step S3 rises to 70 DEG C, stop heating, be added forming agent, while reduce stirring speed
Degree；
S5, after grain forming in the mixture of step S4, cooling stopped reaction is washed product, is dried, obtained
Big grain size crospovidone.
In order to be better achieved the present invention, in the step S1, the mass ratio of monomer NVP and water is 9:1.
Further, in the step S2, the alkali metal hydroxide of addition is 3 with the mass ratio of monomer NVP:100.
Further, in the step S3, mixing speed is 60 revs/min.
Preferably, in the step S4, forming agent is tert-butyl hydroperoxide, benzoyl peroxide, di-t-butyl mistake
At least one of oxide, azodiisobutyronitrile, peroxidized t-butyl perbenzoate.
Preferably, in the step S4, mixing speed is 20 revs/min.
The present invention compared with the prior art, has the following advantages and advantageous effect：
The present invention by way of adding forming agent in the course of the polymerization process, by changing surface tension when grain forming,
Make it that can suspend in the form of larger particles in water phase, part of the product PVPP grain sizes between 140~200 μm is made to account for
80% or more.
Specific implementation mode
The present invention is described in further detail with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment
NVP900 grams of monomer is taken, with Agilent chromatograph, SE-54 capillary tube column analysis is as follows：NVP accounts for 99.70%, 2- pyrroles
Pyrrolidone accounts for 0.02%, and 100 grams of water are added, are placed in there-necked flask；
60 revs/min of mixing speed, rushes nitrogen protection, and 55 DEG C are heated in water-bath, and 27 grams of alkali metal hydroxides are added；
There-necked flask is removed into water-bath, is placed at room temperature, when there-necked flask temperature rises to 70 DEG C, be added 0.5%~5.0% at
Type agent reduces speed of agitator to 20 revs/min；
When there-necked flask temperature reaches 90 DEG C, the stopped reaction that cools down is placed in cold bath, resulting polymers are washed three times,
And it dries.
In conclusion description through this embodiment, can make those skilled in the art preferably implement this programme, but this
The embodiment of invention is not limited to the range represented by embodiment.Embodiment is merely to illustrate the present invention, not for limit
The scope of the present invention processed.In addition, after reading present disclosure, those skilled in the art can make the present invention various repair
Change, these equivalent variations equally fall within the appended claims limited range of the present invention.
Claims (5)
1. a kind of preparation method of big grain size crospovidone, it is characterised in that include the following steps：
S1, a certain amount of monomer NVP, water are mixed；
S2, alkali metal hydroxide is added into the mixture of step S1, is passed through nitrogen protection；
S3, mixture obtained by step S2 is stirred and is heated to 55 DEG C, initiation Popcorn Polymerization；
S4, when the mixture temperature of step S3 rises to 70 DEG C, stop heating, forming agent be added, while reducing mixing speed；
S5, after grain forming in the mixture of step S4, cooling stopped reaction is washed product, is dried, obtains big grain
Diameter crospovidone；
Wherein, in the step S4, forming agent is tert-butyl hydroperoxide, benzoyl peroxide, di-tert-butyl peroxide, idol
At least one of nitrogen bis-isobutyronitrile, tertiary butyl perbenzoate.
2. a kind of preparation method of big grain size crospovidone according to claim 1, it is characterised in that：The step S1
In, the mass ratio of monomer NVP and water is 9:1.
3. a kind of preparation method of big grain size crospovidone according to claim 1, it is characterised in that：The step S2
In, the alkali metal hydroxide of addition is 3 with the mass ratio of monomer NVP:100.
4. a kind of preparation method of big grain size crospovidone according to claim 1, it is characterised in that：The step S3
In, mixing speed is 60 revs/min.
5. a kind of preparation method of big grain size crospovidone according to claim 1, it is characterised in that：The step S4
In, mixing speed is 20 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710235124.1A CN106883333B (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of big grain size crospovidone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710235124.1A CN106883333B (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of big grain size crospovidone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106883333A CN106883333A (en) | 2017-06-23 |
| CN106883333B true CN106883333B (en) | 2018-10-23 |
Family
ID=59183523
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710235124.1A Active CN106883333B (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of big grain size crospovidone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106883333B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485771A (en) * | 2018-10-30 | 2019-03-19 | 焦作中维特品药业股份有限公司 | A kind of preparation method of crospovidone |
| CN116574206B (en) * | 2023-05-11 | 2024-01-16 | 宇昂科技有限公司 | Crosslinked povidone and preparation method and application thereof |
| CN116515025B (en) * | 2023-05-11 | 2024-01-16 | 宇昂科技有限公司 | Crosslinked povidone and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935370A (en) * | 2010-08-06 | 2011-01-05 | 安徽山河药用辅料股份有限公司 | Method for preparing 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 |
| 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 |
-
2017
- 2017-04-12 CN CN201710235124.1A patent/CN106883333B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935370A (en) * | 2010-08-06 | 2011-01-05 | 安徽山河药用辅料股份有限公司 | Method for preparing polyvinylpolypyrrolidone |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106883333A (en) | 2017-06-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106883333B (en) | A kind of preparation method of big grain size crospovidone | |
| Mahdavinia et al. | Modified chitosan 4. Superabsorbent hydrogels from poly (acrylic acid-co-acrylamide) grafted chitosan with salt-and pH-responsiveness properties | |
| Kiatkamjornwong et al. | Influence of reaction parameters on water absorption of neutralized poly (acrylic acid‐co‐acrylamide) synthesized by inverse suspension polymerization | |
| JP6874223B2 (en) | Thermally expandable microspheres prepared from biomonomers | |
| CN101880354B (en) | High molecular emulsion polymer and preparation method thereof | |
| AU3979100A (en) | Process for the preparation of monodisperse polymer particles | |
| CN101935370A (en) | Method for preparing polyvinylpolypyrrolidone | |
| CN109456506A (en) | The heat-expandable microsphere and preparation method thereof of low residual monomer content | |
| CN104672741B (en) | High solids content anionic self-emulsification aqueous epoxy resin emulsion and preparation method thereof | |
| CN106008840B (en) | A kind of chitosan crosslinked modified resin and its preparation method and application | |
| CN103304724A (en) | Vinyl chloride-acrylic acid ester-vinyl acetate-acrylic acid copolymerized emulsion | |
| JPH03195713A (en) | Production of polymer having high water absorption | |
| CN105218731A (en) | A kind of shock resistance type chloroethylene copolymer resin and preparation method thereof | |
| AU689621B2 (en) | Suspending agent for suspension polymerization of vinyl compound | |
| CN108070060B (en) | Microsphere powder of micron-level high-crosslinked polymer and preparation method and application thereof | |
| JP4210566B2 (en) | Method for producing hollow resin fine particles and hollow resin fine particles | |
| CN101389803B (en) | Process for production of composite fiber | |
| JPH09227605A (en) | Production of acrylic-base polymer bead | |
| Yang et al. | One-pot polyvinyl chloride preparation utilizing polyacrylate latex with tertiary amine groups for improved thermal stability, toughness, and reduced reactor scaling | |
| CN106967269A (en) | A kind of preparation method of food grade polyacrylamide | |
| JP2745703B2 (en) | Method for producing water-absorbing polymer | |
| CN103601842A (en) | Preparation method of polyacrylic acid large-particle size bead-like water-absorbent resin | |
| JP2722695B2 (en) | Method for producing water-absorbing polymer | |
| CN109851965B (en) | Nano composite high water absorption material and preparation method thereof | |
| JPWO2021162085A5 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |