CN101757880A - Preparation method of mono-dispersion microballoon resin - Google Patents
Preparation method of mono-dispersion microballoon resin Download PDFInfo
- Publication number
- CN101757880A CN101757880A CN201010301044A CN201010301044A CN101757880A CN 101757880 A CN101757880 A CN 101757880A CN 201010301044 A CN201010301044 A CN 201010301044A CN 201010301044 A CN201010301044 A CN 201010301044A CN 101757880 A CN101757880 A CN 101757880A
- Authority
- CN
- China
- Prior art keywords
- preparation
- microballoon resin
- mono
- dispersion
- microballoon
- 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.)
- Pending
Links
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to a preparation method of mono-dispersion microballoon resin, comprising the following steps: (1) pretreatment: monoenes monomers and cross-linking agents carry out alkali washing and rinsing respectively, dispersing agents are placed into water and are completely dissolved after being fully mixed; (2) preparation: the monoenes monomers, the cross-linking agents and pore-making agents are fully mixed, and then the mixture is added in dispersing agent aqueous solution, the mixture is stirred and two times of the temperature-rising reaction are carried out; (3) impurity removal: mother solution is discarded, the microballoon resin is collected, and then acetone is used for elution, ultra-violet analysis is carried out to the elution reagent, when impurity peak is lower to 10ppm, the microballoon resin finished product is obtained; the preparation method in the invention is simple, the grain size of the prepared microballoon resin is uniform and can be adjusted within a 5mum-70mum range, the surface is smooth, the grain size distribution is narrow with about plus/minus 5mum, and the method has good characteristics and brings great convenience to users.
Description
Technical field
The present invention relates to microballoon resin, especially a kind of preparation method of mono-dispersion microballoon resin.
Background technology
The monodispersity microballoon resin is meant the comparatively polymer microsphere resin of homogeneous of particle size, in standard metering, biomedicine, information, analytical chemistry, colloid science and chromatographic isolation field, be widely used, the method of the synthetic polymer microballoon of having reported mainly comprises emulsion polymerization synthesizing submicron monodisperse polymer particles, but anion or non-ionic surface active agent constantly are deposited on the polymer and are embedded in the polymer beads, thereby have limited the validity of this method.The single dispersion of dispersin polymerization and suspension polymerisation energy synthesizing micron-grade and the polymer beads of wide dispersion, but stabilizing agent and dispersant have limited the application of microballoon attached to the surface of microballoon.
According to the retrieval, find two pieces of patents related to the present invention, wherein the patent disclosure of CN1631913 a kind of mono-dispersed nano/micron polymer microballoon resin and preparation method thereof, its polymer microballoon is the copolymer microsphere of the crosslinked gel-type polyenoid class monomer homopolymers of 20-100% or polyenoid class monomer and other functional monoene class monomer, its particle diameter is in 100 nanometers-10 micron, the decentralization of particle diameter is 1.017-1.037, and the functional group content scope is 0.1-3.0mmol/g.Patent CN85100884 disclose a kind of about anionic agglomeration microsphere resin preparation and as the characteristic and the using method of high-performance ion chromatography column filler, with the single dispersion quaternary ammoniated crosslinked polystyrene latex of granularity less than 0.5 μ m, on the surface of granularity, can be made into the anionic agglomeration microsphere resin of low ion exchange capacity with the Coulomb force agglomeration greater than the crosslinked polystyrene microsphere of 5 μ m.Above-mentioned two patents all exist the reaction time long, and complex steps is difficult for the deficiency of industrialization.
Summary of the invention
The present invention seeks to overcome the deficiencies in the prior art part, the preparation method of mono-dispersion microballoon resin of a kind of generated time weak point, narrow diameter distribution, output capacity height, easy large-scale production is provided.
The present invention realizes that the technical scheme of purpose is:
A kind of preparation method of mono-dispersion microballoon resin is characterized in that: the step of preparation is:
(1) preliminary treatment: respectively with alkali cleaning and washing, the degree of cross linking of control monoene class monomer and crosslinking agent is 8%-55% with monoene class monomer, crosslinking agent; Dispersant is put into water dissolve fully, guarantee that the aqueous dispersant final concentration is 1-5g/L;
(2) preparation: monoene class monomer, crosslinking agent, perforating agent are fully mixed, join in the aqueous dispersant after the mixing, stir 100-500 rev/min, reacted 1-2 hour, and slowly be warming up to the 75-85 degree in the course of reaction, the reaction back is incubated 1.5-2.5 hour when 80 spend, in 0.5-1.5 hour, slowly be warming up to the 90-100 degree again, kept this thermotonus again 1.5-2.5 hour, reaction finishes, and makes the reactant liquor that contains microballoon resin;
(3) removal of impurities: the reactant liquor that will contain microballoon resin discards mother liquor, collects microballoon resin, and microballoon resin is washed with water, uses the acetone wash-out then, and elution reagent is carried out ultra-violet analysis, when its assorted peak is low to moderate 10ppm, is the microballoon resin finished product.
And described dispersant is the mixture of polyvinylpyrrolidone, lauryl sodium sulfate and polysorbate60.
And the weight ratio of described polyvinylpyrrolidone, lauryl sodium sulfate and polysorbate60 is: 20-80: 2-20: 1-10.
And described monoene class monomer is styrene, methyl acrylate, acrylic acid, acrylonitrile methyl methacrylate or a kind of in the chlorine methylene-benzene ethene.
And described crosslinking agent is two acrylic acid glycol esters or divinylbenzene.
And described perforating agent is toluene or saturated alkane.
And described saturated alkane is octane or decane.
Advantage of the present invention and beneficial effect are:
1, the preparation method of microballoon resin provided by the invention adopts the mixture of big macromolecule water-solubility polyethylene of dispersing agent pyrrolidones, lauryl sodium sulfate and polysorbate60, and this dispersant can effectively shorten generated time, makes the raising production efficiency of products
2, the preparation method who the present invention relates to is simple, and the microballoon resin particle diameter of preparing is even, and is adjustable in the 5um-70um scope, smooth surface, and narrow diameter distribution, scope be ± 5um about, have excellent characteristic, bring great convenience to the user.
3, the method reaction condition gentleness that the present invention relates to, each step is simple to operate, and does not have exclusive equipment, brings convenience to production.
The specific embodiment
The utility model is described in further detail below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection domain of the present utility model with this.
Embodiment 1
A kind of preparation method of mono-dispersion microballoon resin, step is:
(1) preliminary treatment: styrene 100ml, divinylbenzene (DVB) 10ml are used 10% NaOH aqueous solution alkali cleaning respectively three times, water is given a baby a bath on the third day after its birth time then, dispersant (polyvinylpyrrolidone 3g, lauryl sodium sulfate 0.5g, polysorbate60 0.3g) is put into 3000ml water be fully mixed to dissolving fully.
The degree of cross linking of crosslinking agent divinylbenzene is that 8%-55% all can.
Styrene is monoene class monomer, also can adopt methyl acrylate, acrylic acid, acrylonitrile methyl methacrylate, to replacements such as chlorine methylene-benzene ethene.
Divinylbenzene (DVB) is a crosslinking agent, also available pair of replacement such as acrylic acid glycol ester.
Dispersant is: the mixture of polyvinylpyrrolidone, 12 sodium alkyl sulfates and polysorbate60, mixed weight is than being 20-80: 2-20: 1-10.
(2) preparation: styrene 100ml, divinylbenzene 10ml, toluene 15ml are fully mixed, join after the mixing in the aqueous solution of dispersant, stir 400 rev/mins, reacted 1.5 hours, slowly be warming up to 80 degree in the course of reaction, the reaction back is incubated 2 hours when 80 spend; The reaction environment temperature slowly was warming up to 95 degree again in 1 hour, kept this thermotonus again 2 hours, reaction finishes, and makes the reactant liquor that contains microballoon resin.
Toluene is perforating agent, can also use replacements such as saturated alkane such as octane, decane.
(3) removal of impurities: the above-mentioned reactant liquor that contains microballoon resin is discarded mother liquor, collect microballoon resin, the microballoon resin water is given a baby a bath on the third day after its birth time, flush away residue water soluble dispersing agent is used the acetone wash-out three times again, and elution reagent is carried out ultra-violet analysis, when its assorted peak is low to moderate 10ppm, be the microballoon resin finished product.
The microballoon resin finished product grain size of this prepared in reaction is adjustable in the 5um-70um scope, narrow diameter distribution, particle size distribution range be ± 5um about, the transparent no bubble of this microballoon resin.
Embodiment 2
A kind of preparation method of mono-dispersion microballoon resin, step is:
(1) preliminary treatment: styrene 100ml, divinylbenzene 20ml are used 10% NaOH aqueous solution alkali cleaning respectively three times, water is given a baby a bath on the third day after its birth time then, dispersant (polyvinylpyrrolidone 5g, lauryl sodium sulfate 0.7g, polysorbate60 0.3g) is put into 4000ml water be fully mixed to dissolving fully;
(2) preparation: set degree of cross linking 8%-55%, styrene 100ml, divinylbenzene 20ml, decane 25ml are fully mixed, join after the mixing in the aqueous solution of dispersant, stir 300 rev/mins, reacted 2 hours, slowly be warming up to 80 degree in the course of reaction, the reaction back is incubated 2 hours when 80 spend; The reaction environment temperature slowly was warming up to 95 degree again in 1 hour, kept this thermotonus again 2 hours, reaction finishes.
(3) removal of impurities: above-mentioned reactant liquor is discarded mother liquor, collect microballoon resin, microballoon resin is washed with water 3 times, flush away residue water soluble dispersing agent is used the acetone wash-out three times again, and elution reagent is carried out ultra-violet analysis, when its assorted peak is low to moderate 10ppm, be the microballoon resin finished product.
The microballoon resin finished product grain size of this prepared in reaction is adjustable in the 5um-70um scope, narrow diameter distribution, particle size distribution range be ± 5um about, the transparent no bubble of this microballoon resin.
Claims (7)
1. preparation method of mono-dispersion microballoon resin, it is characterized in that: the step of preparation is:
(1) preliminary treatment: respectively with alkali cleaning and washing, the degree of cross linking of control monoene class monomer and crosslinking agent is 8%-55% with monoene class monomer, crosslinking agent; Dispersant is put into water dissolve fully, guarantee that the aqueous dispersant final concentration is 1-5g/L;
(2) preparation: monoene class monomer, crosslinking agent, perforating agent are fully mixed, join in the aqueous dispersant after the mixing, stir 100-500 rev/min, reacted 1-2 hour, and slowly be warming up to the 75-85 degree in the course of reaction, the reaction back is incubated 1.5-2.5 hour when 80 spend, in 0.5-1.5 hour, slowly be warming up to the 90-100 degree again, kept this thermotonus again 1.5-2.5 hour, reaction finishes, and makes the reactant liquor that contains microballoon resin;
(3) removal of impurities: the reactant liquor that will contain microballoon resin discards mother liquor, collects microballoon resin, and microballoon resin is washed with water, uses the acetone wash-out then, and elution reagent is carried out ultra-violet analysis, when its assorted peak is low to moderate 10ppm, is the microballoon resin finished product.
2. a kind of preparation method of mono-dispersion microballoon resin according to claim 1 is characterized in that: described dispersant is the mixture of polyvinylpyrrolidone, lauryl sodium sulfate and polysorbate60.
3. a kind of preparation method of mono-dispersion microballoon resin according to claim 2 is characterized in that: the weight ratio of described polyvinylpyrrolidone, lauryl sodium sulfate and polysorbate60 is: 20-80: 2-20: 1-10.
4. a kind of preparation method of mono-dispersion microballoon resin according to claim 1 is characterized in that: described monoene class monomer is styrene, methyl acrylate, acrylic acid, acrylonitrile methyl methacrylate or a kind of in the chlorine methylene-benzene ethene.
5. a kind of preparation method of mono-dispersion microballoon resin according to claim 1 is characterized in that: described crosslinking agent is two acrylic acid glycol esters or divinylbenzene.
6. a kind of preparation method of mono-dispersion microballoon resin according to claim 1 is characterized in that: described perforating agent is toluene or saturated alkane.
7. a kind of preparation method of mono-dispersion microballoon resin according to claim 6 is characterized in that: described saturated alkane is octane or decane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010301044A CN101757880A (en) | 2010-02-02 | 2010-02-02 | Preparation method of mono-dispersion microballoon resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010301044A CN101757880A (en) | 2010-02-02 | 2010-02-02 | Preparation method of mono-dispersion microballoon resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101757880A true CN101757880A (en) | 2010-06-30 |
Family
ID=42489359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010301044A Pending CN101757880A (en) | 2010-02-02 | 2010-02-02 | Preparation method of mono-dispersion microballoon resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101757880A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928365A (en) * | 2010-09-27 | 2010-12-29 | 天津市富集科技有限公司 | Method for preparing amphiphilic monodisperse microspherical resin |
| CN102382226A (en) * | 2011-08-12 | 2012-03-21 | 天津博纳艾杰尔科技有限公司 | Preparation method of poly-N-vinylpyrrodidone-divinylbenzene microsphere |
| CN102731701A (en) * | 2012-04-23 | 2012-10-17 | 苏州异导光电材料科技有限公司 | Method for preparing mono-disperse polymer functional microspheres with photochemical method |
| CN104004131A (en) * | 2014-02-25 | 2014-08-27 | 江苏海普功能材料有限公司 | High specific surface area amphoteric adsorption resin containing pyrrolidone bases and preparation method thereof |
| CN105037630A (en) * | 2015-09-21 | 2015-11-11 | 南京大学 | Hydrophilic polymer microsphere and simple preparing method thereof |
-
2010
- 2010-02-02 CN CN201010301044A patent/CN101757880A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928365A (en) * | 2010-09-27 | 2010-12-29 | 天津市富集科技有限公司 | Method for preparing amphiphilic monodisperse microspherical resin |
| CN102382226A (en) * | 2011-08-12 | 2012-03-21 | 天津博纳艾杰尔科技有限公司 | Preparation method of poly-N-vinylpyrrodidone-divinylbenzene microsphere |
| CN102382226B (en) * | 2011-08-12 | 2014-03-19 | 天津博纳艾杰尔科技有限公司 | Preparation method of poly-N-vinylpyrrodidone-divinylbenzene microsphere |
| CN102731701A (en) * | 2012-04-23 | 2012-10-17 | 苏州异导光电材料科技有限公司 | Method for preparing mono-disperse polymer functional microspheres with photochemical method |
| CN104004131A (en) * | 2014-02-25 | 2014-08-27 | 江苏海普功能材料有限公司 | High specific surface area amphoteric adsorption resin containing pyrrolidone bases and preparation method thereof |
| CN104004131B (en) * | 2014-02-25 | 2017-04-12 | 江苏海普功能材料有限公司 | High specific surface area amphoteric adsorption resin containing pyrrolidone bases and preparation method thereof |
| CN105037630A (en) * | 2015-09-21 | 2015-11-11 | 南京大学 | Hydrophilic polymer microsphere and simple preparing method thereof |
| CN105037630B (en) * | 2015-09-21 | 2017-09-05 | 南京大学 | A kind of hydrophilic polymer microballoon and its simple method for preparing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101757880A (en) | Preparation method of mono-dispersion microballoon resin | |
| CN102382227B (en) | Swelling copolymerization preparation method of N-vinyl pyrrolidone and divinylbenzene monodisperse microsphere | |
| CN102964539B (en) | The preparation method of porous magnetic polystyrene microsphere | |
| CN101434673A (en) | Preparation of monodisperse porous polymer microsphere | |
| CN104926975B (en) | Strong basicity composite resin material and preparation method thereof | |
| CN104861102B (en) | A kind of porous crosslinked polystyrene microballoon and preparation method thereof | |
| CN103159891B (en) | Magnetic amino-modified superhighly-crosslinked resin and preparation method thereof | |
| CN101058614B (en) | Method of preparing micron-level magnetic polymer micro-sphere by polarity seed swelling method | |
| CN102603929B (en) | Preparation method of polymer particles | |
| CN102382226B (en) | Preparation method of poly-N-vinylpyrrodidone-divinylbenzene microsphere | |
| CN102641753B (en) | Method for preparing magnetic strong-basicity ion exchange resin for removing organic matters in water | |
| CN105461846A (en) | Magnetic acrylic-acid polyamine resin capable of removing heavy metal ions and preparation method thereof | |
| CN104262521A (en) | Preparation method of styrene-divinylbenzene copolymer hydrophobic catalyst support | |
| CN102627718A (en) | Preparation method for crosslinked polystyrene microspheres of 10-100 microns | |
| CN103694405B (en) | A kind of preparation method of Macroporous weak acid cation exchange resin | |
| CN102814199A (en) | Preparation method of magneitc polymer microspheres for in situ immobilization of noble metal catalyst | |
| CN102430434B (en) | Preparation method of PVC semi-homogeneous phase anion/cation exchange membrane | |
| CN102936355A (en) | Preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution | |
| CN103432971A (en) | Preparation method of dissymmetric hollow microspheres based on polymer template particles | |
| CN102234344A (en) | Preparation method of macroporous long alkyl side chain acrylic acid ester-styrene-ethylene dimethacrylate crosslinking copolymerization microballoon | |
| CN102408508B (en) | Preparation method for monodisperse cationic polystyrene microballoon sphere with controllable grain diameter | |
| CN104558260B (en) | Terpolymer preparation method for carrier for olefin polymerization catalyst | |
| CN102937781B (en) | Preparation method for toner adopting polyester and styrene-acrylate copolymer as binding resins | |
| CN102863646B (en) | Preparation method for rosin-based porous polymer microsphere | |
| CN104788609A (en) | Highly cross-linked monodisperse epoxy-group-containing polymeric microsphere and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100630 |