CN106632874A - Preparation method for polymer microcapsule - Google Patents
Preparation method for polymer microcapsule Download PDFInfo
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- CN106632874A CN106632874A CN201610887669.6A CN201610887669A CN106632874A CN 106632874 A CN106632874 A CN 106632874A CN 201610887669 A CN201610887669 A CN 201610887669A CN 106632874 A CN106632874 A CN 106632874A
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- Prior art keywords
- water
- preparation
- poly
- polymer microcapsule
- methacrylate
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- 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to a preparation method for a polymer microcapsule. The preparation method comprises the steps of using polyglycidyl methacrylate with surface activity and monomer polymerization function as a macromolecule emulgator and an initiator, triggering the polymerization of hydrophobe monomer under the condition of heating to obtain the polymer microcapsule. Compared with the current preparation method for the polymer microcapsule, the micromolecule emulgator and the initiator do not need to be added additionally, the system and the preparation process are simple, the post-treatment is simple and convenient, the universality is strong, and the cost is lower. The preparation method is suitable for the industrial large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of polymer microcapsule, and in particular to have surface-active and initiation simultaneously
The poly (glycidyl methacrylate) of monomer polymerizable functional is macromole emulsifying agent and initiator, is not additionally adding small molecule
Under conditions of emulsifying agent and initiator, cause hydrophobic monomer polymerization, obtain polymer microcapsule.
Background technology
Polymer microcapsule energy Protective substances change material surface performance from ambient influnence, isolate active component, reduce
Volatility and toxicity, control various effects such as sustainable release, many in medicine, food, cosmetics, coating, agricultural chemicals, additive etc.
Individual field is widely used.According to encystation mechanism and condition, the preparation method of polymer microcapsule can be divided into template, layer by layer
Self-assembly method, complex coacervation, spray drying process, interfacial polymerization, phase separation method and situ aggregation method etc..
In above-mentioned preparation method, interfacial polymerization, the phase separation method and situ aggregation method quilt because of extensive monomer applicability
For preparing polymer microcapsule of the particle diameter from tens nanometers to up to a hundred microns.The principle of interfacial polymerization is that two kinds of activity are single
Body is dissolved in respectively in immiscible solvent, when a kind of solution is dispersed in another kind of solution, the list in two phase liquid
Capsule formed and polymerisation in boundary in body there is.The method needs the proportioning of the species, concentration and two-phase solvent in monomer
Etc. aspect carry out meticulous design and selection, therefore restrictive condition is more, is difficult the polymer microcapsule for preparing multi items.Phase point
It is that the core of microcapsules and wall material are codissolved in organic solvent and are emulsified in water to form emulsion from method, by solvent volatilization process
Phase separation between middle core and wall material, is obtained the microcapsules of different morphologies.But, the method is needed using substantial amounts of organic molten
Agent, can cause serious environmental pollution in volatilization process.Situ aggregation method be using the reactive monomer as core or its can
Dissolubility performed polymer is dispersion phase with initiator, is emulsified in dispersion phase by adding surfactant in water, the monomer in core
Or there is phase separation and form microcapsules in the polymer formed after performed polymer polymerization because incompatible with monomer or performed polymer.The method
Being disadvantageous in that needs to use substantial amounts of surfactant and initiator, and system is complex.
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of preparation method of polymer microcapsule.
Technical scheme
A kind of preparation method of polymer microcapsule, it is characterised in that step is as follows：
Step 1：By the poly (glycidyl methacrylate) with surface-active and trigger monomer polymerizable functional, hydrophobicity
Monomer and water are 0.1～1 in mass ratio:1～10:Emulsification after 10～100 ratio mixing obtains oil-in-water breast for 1～30 minute
Liquid；
Step 2：60～100 DEG C of polymerisations with trigger monomer are then heated to, insulation terminates anti-after 2～24 hours
Should；
Step 3：Clean reacted emulsion with water to remove unreacted monomer, polymethylacrylic acid soluble in water contracting
Water glyceride, obtains polymer microcapsule.
The hydrophobic monomer is styrene, 4- hydroxymethylstyrenes, 4- 1-chloro-4-methyl-benzenes, methyl acrylate, propylene
Acetoacetic ester, propyl acrylate, butyl acrylate, glycidyl acrylate, methyl methacrylate, EMA,
Propyl methacrylate, butyl methacrylate, GMA, divinylbenzene, dimethacrylate second
Glycol or ethylene glycol diacrylate.
Beneficial effect
The preparation method of a kind of polymer microcapsule proposed by the present invention, using simultaneously with surface-active and trigger monomer
The poly (glycidyl methacrylate) of polymerizable functional is macromole emulsifying agent and initiator, and hydrophobicity is caused in a heated condition
The polymerization of monomer, obtains polymer microcapsule.It is extra little without the need for adding compared with existing polymer microcapsule preparation method
Molecule emulsifying agent and initiator etc., system and preparation process is simple, post processing is easy, and highly versatile, cost is relatively low, is adapted to industry
Change large-scale production.
Polymer microcapsule preparation method involved in the present invention belongs to situ aggregation method, is advantageous in that introducing simultaneously
Poly (glycidyl methacrylate) with surface-active and trigger monomer polymerizable functional is macromole emulsifying agent and initiator,
Under conditions of small-molecular emulsifier and initiator is not additionally added, you can cause hydrophobic monomer polymerization, obtain polymer micro-
Capsule.Party's law system and preparation process is simple, post processing is easy, and highly versatile, cost is relatively low, is adapted to industrialization extensive raw
Produce.
Description of the drawings
Fig. 1：The scanning electricity of poly (glycidyl methacrylate) Methyl Methacrylate resulting polymers microcapsules
Mirror photo.
Fig. 2：Poly (glycidyl methacrylate) causes the ESEM of divinylbenzene resulting polymers microcapsules to shine
Piece.
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：Poly (glycidyl methacrylate) causes styrene polymerization to prepare polymer microcapsule
After by 6g poly (glycidyl methacrylate)s, 40g styrene monomers, the mixing of 100g water, emulsification is stirred at room temperature
10 minutes, 60 DEG C are heated to, after reacting 12 hours, with water the unpolymerized styrene of removing and poly- first soluble in water are fully cleaned
Base glycidyl acrylate, obtains polystyrene microcapsules.
Embodiment 2：Poly (glycidyl methacrylate) causes divinyl benzene polymer to prepare polymer microcapsule
After by 4g poly (glycidyl methacrylate)s, 40g divinylbenzene monomers, the mixing of 100g water, it is stirred at room temperature
Emulsification 10 minutes, is heated to 70 DEG C, after reacting 12 hours, fully cleans the unpolymerized divinylbenzene of removing with water and is dissolved in water
In poly (glycidyl methacrylate), obtain polydivinylbenezene microcapsules.
Embodiment 3：Poly (glycidyl methacrylate) causes 4- hydroxymethylstyrene polymerizations to prepare polymer microcapsule
After by 4g poly (glycidyl methacrylate)s, 40g 4- hydroxymethylstyrene monomers, the mixing of 100g water, in room temperature
Stirring and emulsifying 30 minutes, is heated to 70 DEG C, after reacting 12 hours, with water the unpolymerized 4- hydroxymethylstyrenes of removing is fully cleaned
And poly (glycidyl methacrylate) soluble in water, obtain poly- (4- hydroxymethylstyrenes) microcapsules.
Embodiment 4：Poly (glycidyl methacrylate) causes 4- 1-chloro-4-methyl-benzene polymerizations to prepare polymer microcapsule
After by 6g poly (glycidyl methacrylate)s, 60g 4- 1-chloro-4-methyl-benzene monomers, the mixing of 150g water, in room temperature
Stirring and emulsifying 30 minutes, is heated to 80 DEG C, after reacting 10 hours, with water the unpolymerized 4- 1-chloro-4-methyl-benzenes of removing is fully cleaned
And poly (glycidyl methacrylate) soluble in water, obtain poly- (4- 1-chloro-4-methyl-benzenes) microcapsules.
Embodiment 5：Poly (glycidyl methacrylate) Methyl Methacrylate polymerization prepares polymer microcapsule
After by 8g poly (glycidyl methacrylate)s, 40g methyl methacrylate monomers, the mixing of 100g water, in room temperature
Stirring and emulsifying 30 minutes, is heated to 60 DEG C, after reacting 12 hours, with water the unpolymerized methyl methacrylate of removing is fully cleaned
And poly (glycidyl methacrylate) soluble in water, obtain polymethyl methacrylate microcapsules.
Embodiment 6：Poly (glycidyl methacrylate) causes butyl methacrylate polymerization to prepare polymer microcapsule
After by 4g poly (glycidyl methacrylate)s, 40g butylmethacrylate monomers, the mixing of 100g water, in room temperature
Stirring and emulsifying 20 minutes, is heated to 60 DEG C, after reacting 12 hours, with water the unpolymerized butyl methacrylate of removing is fully cleaned
And poly (glycidyl methacrylate) soluble in water, obtain polybutyl methacrylate microcapsules.
Embodiment 7：Poly (glycidyl methacrylate) causes ethylene glycol diacrylate polymerization to prepare the micro- glue of polymer
Capsule
After by 4g poly (glycidyl methacrylate)s, 40g ethylene glycol diacrylate monomers, the mixing of 100g water, in room
Warm stirring and emulsifying 20 minutes, is heated to 70 DEG C, after reacting 12 hours, with water the unpolymerized diacrylate second two of removing is fully cleaned
Alcohol ester and poly (glycidyl methacrylate) soluble in water, obtain poly- ethylene glycol diacrylate microcapsules.
Embodiment 8：It is poly- that poly (glycidyl methacrylate) causes styrene and methyl methacrylate copolymer to close preparation
Complex microcapsule
By 6g poly (glycidyl methacrylate)s, 20g styrene monomers, 20g methyl methacrylate monomers, 100g water
After mixing, emulsification 10 minutes is stirred at room temperature, is heated to 60 DEG C, after reacting 12 hours, fully clean removing with water unpolymerized
Styrene, methyl methacrylate and poly (glycidyl methacrylate) soluble in water, obtain poly- (styrene-methyl third
E pioic acid methyl ester) microcapsules.
Claims (2)
1. a kind of preparation method of polymer microcapsule, it is characterised in that step is as follows：
Step 1：By the poly (glycidyl methacrylate) with surface-active and trigger monomer polymerizable functional, hydrophobic monomer
In mass ratio it is 0.1～1 with water:1～10:Emulsification after 10～100 ratio mixing obtains oil-in-water emulsion in 1～30 minute；
Step 2：60～100 DEG C of polymerisations with trigger monomer are then heated to, insulation terminates reaction after 2～24 hours；
Step 3：Reacted emulsion is cleaned with water and shrinks sweet to remove unreacted monomer, polymethylacrylic acid soluble in water
Grease, obtains polymer microcapsule.
2. the preparation method of polymer microcapsule according to claim 1, it is characterised in that：The hydrophobic monomer is benzene second
Alkene, 4- hydroxymethylstyrenes, 4- 1-chloro-4-methyl-benzenes, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate,
Glycidyl acrylate, methyl methacrylate, EMA, propyl methacrylate, butyl methacrylate,
GMA, divinylbenzene, ethylene glycol dimethacrylate or ethylene glycol diacrylate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610887669.6A CN106632874A (en) | 2016-10-11 | 2016-10-11 | Preparation method for polymer microcapsule |
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| CN201610887669.6A CN106632874A (en) | 2016-10-11 | 2016-10-11 | Preparation method for polymer microcapsule |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107337745A (en) * | 2017-08-04 | 2017-11-10 | 西北工业大学 | A kind of preparation method of water-in-oil type polymer microcapsule |
| CN108079915A (en) * | 2018-01-31 | 2018-05-29 | 湘潭大学 | A kind of preparation method and device of the microencapsulation material based on base material and the double regulation and control of shell material granularity |
| CN108102033A (en) * | 2017-12-05 | 2018-06-01 | 西北工业大学 | A kind of preparation method of surface wrinkles polymer particle |
| CN109181582A (en) * | 2018-08-08 | 2019-01-11 | 陕西科技大学 | A kind of pH response type low viscosity high intensity stone material adhesive and preparation method thereof |
| CN109456446A (en) * | 2017-12-05 | 2019-03-12 | 西北工业大学 | A kind of preparation method of high-specific surface polymer microcapsules |
| CN116675802A (en) * | 2023-06-05 | 2023-09-01 | 扬州市祥华新材料科技有限公司 | Electroluminescent microcapsule shell material and preparation method thereof |
-
2016
- 2016-10-11 CN CN201610887669.6A patent/CN106632874A/en active Pending
Non-Patent Citations (7)
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107337745A (en) * | 2017-08-04 | 2017-11-10 | 西北工业大学 | A kind of preparation method of water-in-oil type polymer microcapsule |
| CN108102033A (en) * | 2017-12-05 | 2018-06-01 | 西北工业大学 | A kind of preparation method of surface wrinkles polymer particle |
| CN109456446A (en) * | 2017-12-05 | 2019-03-12 | 西北工业大学 | A kind of preparation method of high-specific surface polymer microcapsules |
| CN108079915A (en) * | 2018-01-31 | 2018-05-29 | 湘潭大学 | A kind of preparation method and device of the microencapsulation material based on base material and the double regulation and control of shell material granularity |
| CN108079915B (en) * | 2018-01-31 | 2020-11-17 | 湘潭大学 | Preparation method and device of microcapsule material based on double regulation and control of base material and shell material granularity |
| CN109181582A (en) * | 2018-08-08 | 2019-01-11 | 陕西科技大学 | A kind of pH response type low viscosity high intensity stone material adhesive and preparation method thereof |
| CN109181582B (en) * | 2018-08-08 | 2020-09-22 | 陕西科技大学 | PH-responsive low-viscosity high-strength stone adhesive and preparation method thereof |
| CN116675802A (en) * | 2023-06-05 | 2023-09-01 | 扬州市祥华新材料科技有限公司 | Electroluminescent microcapsule shell material and preparation method thereof |
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Application publication date: 20170510 |