CN106883333A - A kind of preparation method of big particle diameter PVPP - Google Patents
A kind of preparation method of big particle diameter PVPP Download PDFInfo
- Publication number
- CN106883333A CN106883333A CN201710235124.1A CN201710235124A CN106883333A CN 106883333 A CN106883333 A CN 106883333A CN 201710235124 A CN201710235124 A CN 201710235124A CN 106883333 A CN106883333 A CN 106883333A
- Authority
- CN
- China
- Prior art keywords
- pvpp
- particle diameter
- preparation
- big particle
- 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.)
- Granted
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 method of big particle diameter PVPP, in monomer NVP:The mass ratio of water is 9:Under conditions of 1,3.0% alkali metal hydroxide is added, be passed through nitrogen protection, being heated to 55 DEG C of initiations carries out Popcorn Polymerization, 60 revs/min of mixing speed；When temperature rises 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, particle diameter PVPP between 140~200 μm is finally given；Forming agent is generally at least one in TBHP, benzoyl peroxide, di-tert-butyl peroxide, azodiisobutyronitrile, peroxidized t-butyl perbenzoate.The present invention changes surface tension during grain forming by adding forming agent in the course of the polymerization process, it is suspended in the form of larger particles in water phase, part of the particle size between 140~200 μm is accounted for more than 80%.
Description
Technical field
The present invention relates to a kind of chemicals preparation method, more particularly to a kind of preparation method of big particle diameter PVPP,
Belong to pharmaceutic adjuvant technical field.
Background technology
PVPP（PVPP）, it is, by the PVP strand of line style, mutually to be handed over by physical method and chemical method
Connection, be a kind of high-crosslinking-degree, the product with good physiological inertia and adsorptivity, and PVPP has different in water
Swelling Capacity, the form for showing can be soft gel, white powder or porous granule.Itself water insoluble and various acid
Property, alkaline solution, with good physiological security.It is numerous that cross-linked pvp has been applied to wine brewing, beverage and medicine bioengineering etc.
Field.It can serve as the fining agent of plant type beverage, the disintegrant of medicine, the thickener and flocculant of dispersion, absorption
Agent etc..
The preparation of traditional PVPP, is by NVP（NVP）Copolymerization with self-crosslinking agent comes real
It is existing, NVP and appropriate crosslinking agent are carried out into precipitation polymerization in electrolyte aqueous solution, the product of generation by filtering, washing,
It is the NVP cross-linked polymers of porous and granular after drying.Highly cross-linked PVPP product is prepared, from Popcorn Polymerization
（Also known as proliferous polymerization）Mode is carried out.
But in traditional PVPP preparation technologies, the size tunable scope of PVPP is smaller, can only control substantially less than 150 μm
In the range of, PVPP is so significantly limit in wine brewing and beverage industry as fining agent, the application effect of stabilizer, together
When can reusable number of times it is less, cause the waste of resource.
The content of the invention
Part, of the invention by the way of addition forming agent in the course of the polymerization process in view of the shortcomings of the prior art, leads to
Surface tension when changing grain forming is crossed, it is suspended in the form of larger particles in water phase, make product PVPP
Part of the footpath between 140~200 μm accounts for more than 80%.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of big particle diameter PVPP, comprises the following steps：
S1, a certain amount of monomer NVP, water are mixed；
Alkali metal hydroxide is added in S2, the mixture to step S1, nitrogen protection is passed through；
S3, step S2 gained mixtures are stirred and are heated to 55 DEG C, trigger Popcorn Polymerization；
S4, when the mixture temperature of step S3 rises to 70 DEG C, stop heating, add forming agent, while reduce mixing speed；
S5, after after grain forming in the mixture of step S4, cool down stopped reaction, product is washed, is dried, obtain big grain
Footpath PVPP.
In order to the present invention is better achieved, in the step S1, the mass ratio of monomer NVP and water is 9:1.
Further, in the step S2, the alkali metal oxide 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 TBHP, benzoyl peroxide, di-t-butyl mistake
At least one in 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, with advantages below and beneficial effect：
The present invention, by changing surface tension during grain forming, makes it by way of adding forming agent in the course of the polymerization process
Can be suspended in the form of larger particles in water phase, part of the product PVPP particle diameters between 140~200 μm is accounted for 80%
More than.
Specific embodiment
The present invention is described in further detail with reference to embodiment, but embodiments of the present invention not limited to this.
Embodiment
NVP900 grams of monomer is taken, Agilent chromatograph is used, SE-54 capillary tube column analysis are as follows：NVP accounts for 99.70%, 2- pyrroles
Pyrrolidone accounts for 0.02%, adds 100 grams of water, is placed in there-necked flask；
60 revs/min of mixing speed, rushes nitrogen protection, and 55 DEG C are heated in water-bath, adds 27 grams of alkali metal hydroxides；
There-necked flask is removed into water-bath, is placed at room temperature, when there-necked flask temperature rises to 70 DEG C, add 0.5%~5.0% shaping
Agent, reduces speed of agitator to 20 revs/min；
When there-necked flask temperature reaches 90 DEG C, stopped reaction of lowering the temperature in cold bath is placed in, resulting polymers carry out washing three times, and dry
It is dry.
In sum, by the description of the present embodiment, those skilled in the art can be made preferably to implement this programme, but this
The implementation method of invention is not limited to the scope represented by embodiment.Embodiment is merely to illustrate the present invention, not for limit
The scope of the present invention processed.Additionally, after present disclosure is read, those skilled in the art can make various repairing to the present invention
Change, these equivalent variations equally fall within appended claims limited range of the present invention.
Claims (6)
1. a kind of preparation method of big particle diameter PVPP, it is characterised in that comprise the following steps：
S1, a certain amount of monomer NVP, water are mixed；
Alkali metal hydroxide is added in S2, the mixture to step S1, nitrogen protection is passed through；
S3, step S2 gained mixtures are stirred and are heated to 55 DEG C, trigger Popcorn Polymerization；
S4, when the mixture temperature of step S3 rises to 70 DEG C, stop heating, add forming agent, while reduce mixing speed；
S5, after after grain forming in the mixture of step S4, cool down stopped reaction, product is washed, is dried, obtain big grain
Footpath PVPP.
2. the preparation method of a kind of big particle diameter PVPP 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. the preparation method of a kind of big particle diameter PVPP according to claim 1, it is characterised in that：The step S2
In, the alkali metal oxide of addition is 3 with the mass ratio of monomer NVP:100.
4. the preparation method of a kind of big particle diameter PVPP according to claim 1, it is characterised in that：The step S3
In, mixing speed is 60 revs/min.
5. the preparation method of a kind of big particle diameter PVPP according to claim 1, it is characterised in that：The step S4
In, forming agent is TBHP, benzoyl peroxide, di-tert-butyl peroxide, azodiisobutyronitrile, benzylhydroperoxide
At least one in special butyl ester.
6. the preparation method of a kind of big particle diameter PVPP 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 true CN106883333A (en) | 2017-06-23 |
| CN106883333B 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) |
Cited By (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 |
| CN116515025A (en) * | 2023-05-11 | 2023-08-01 | 宇昂科技有限公司 | Crosslinked povidone and preparation method and application thereof |
| CN116574206A (en) * | 2023-05-11 | 2023-08-11 | 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 |
Cited By (5)
| 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 |
| CN116515025A (en) * | 2023-05-11 | 2023-08-01 | 宇昂科技有限公司 | Crosslinked povidone and preparation method and application thereof |
| CN116574206A (en) * | 2023-05-11 | 2023-08-11 | 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 |
| CN116574206B (en) * | 2023-05-11 | 2024-01-16 | 宇昂科技有限公司 | Crosslinked povidone and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106883333B (en) | 2018-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mahdavinia et al. | Modified chitosan 4. Superabsorbent hydrogels from poly (acrylic acid-co-acrylamide) grafted chitosan with salt-and pH-responsiveness properties | |
| CN106883333B (en) | A kind of preparation method of big grain size crospovidone | |
| CN107552008A (en) | A kind of method of corn cob fiber element based aquagel absorption heavy metal ion | |
| CN101935370A (en) | Method for preparing polyvinylpolypyrrolidone | |
| CN104672741B (en) | High solids content anionic self-emulsification aqueous epoxy resin emulsion and preparation method thereof | |
| CN101191003A (en) | High transparence MBS resin composition with excellent impact property | |
| CN103275450A (en) | Method for preparing super absorbent resin | |
| CN106008840B (en) | A kind of chitosan crosslinked modified resin and its preparation method and application | |
| CN113058661A (en) | Preparation method of macroporous acrylic acid weak acid cation exchange resin | |
| JPH03195713A (en) | Production of polymer having high water absorption | |
| CN104926974A (en) | Method for preparing styrene-acrylate copolymer | |
| CN103992435B (en) | A kind of synthetic method of Vltra tears graft acrylic acid methyl esters/vinyl acetate sand-fixation agent | |
| CN103360548A (en) | Preparation method for salt-tolerant super-absorbent resin | |
| CN103182255A (en) | Manufacturing method for polystyrene/polyvinylidene anion exchange alloy membrane | |
| CN106883359B (en) | A kind of high water absorption method for preparing microsphere with humidity resistance of size tunable | |
| CN105273117B (en) | A kind of styrene-acrylic emulsion and preparation method thereof of anti-flash rusting | |
| CN108946725A (en) | Spherical activated charcoal, the preparation method and use of loading cation surfactant | |
| CN109293950A (en) | High-hydroscopicity and preparation method thereof | |
| CN109851965B (en) | Nano composite high water absorption material and preparation method thereof | |
| CN103360549A (en) | Salt-tolerant super-absorbent resin | |
| CN108102019A (en) | The method that substep suspension polymerisation prepares the polymer beads for ion exchange resin | |
| CN101967208A (en) | Preparation method of superabsorbent acrylics | |
| CN111087558A (en) | Modified acrylic-based high-strength salt-resistant high-absorptivity resin and preparation method thereof | |
| CN101003599A (en) | Latex liquid of polymethacrylic resin, and preparation method | |
| CN103613696A (en) | Method for preparing super absorbent resin by using montmorillonite |
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 |