CN109453724A - A kind of inside is the preparation method of the slow-release type microcapsule of multicore - Google Patents
A kind of inside is the preparation method of the slow-release type microcapsule of multicore Download PDFInfo
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- CN109453724A CN109453724A CN201811391917.3A CN201811391917A CN109453724A CN 109453724 A CN109453724 A CN 109453724A CN 201811391917 A CN201811391917 A CN 201811391917A CN 109453724 A CN109453724 A CN 109453724A
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- multicore
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- starch
- release type
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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
Abstract
The invention discloses a kind of preparation methods for the slow-release type microcapsule that inside is multicore; it is that the suspension for being mixed with acrylate polymer, volatile organic solvent, liquid essence and porous-starch is distributed in colloid protective agent aqueous solution by mechanical stirring to form oil-in-water system; then the volatile organic solvent in decompression removal oil-in-water system; acrylate polymer occurs interface with liquid essence and porous-starch and mutually separates, and forms the acrylate polymer microcapsules of internal package liquid essence and porous-starch；Ethylene glycol dimethacrylate prepolymer is further added, after the curing that heated up, obtains the internal crosslinked acrylate polymers essence microcapsule for multicore, i.e., the internal slow-release type microcapsule for multicore.This method is easy to operate, and efficiently, the essence wrapped up can discharge with having levels, lasting fragrance, can be widely applied to the fields such as cosmetics, household or personal care articles, functional form material for preparation.
Description
Technical field
The present invention relates to field of daily chemicals, in particular to a kind of inside is the preparation side of the slow-release type microcapsule of multicore
Method.
Background technique
Core material can be isolated from the outside by microcapsules, and release core material at a different rate under certain conditions, extensively
It is general to be applied to textile, wash the industry fields such as shield product, food, biological medicine, catalyst load.
Currently, essence microcapsule generally existing essence package in the application of consumer products is unstable (vulnerable to external environment
Influence causes essence to leak), the problems such as slow release effect is poor, and fragrance is not lasting.For these problems, people have developed multicore packet
Wrap up in the microcapsules of type.Chinese patent CN102256588A reports a kind of multicore containing fragrance with internal water phase and interior oil phase
Microcapsules production method, be dispersed in the oil-continuous phase containing perfuming component or perfume composition water phase composition
Core, the organic compound by polyisocyanate and comprising permanent quaternary ammonium group and primary ammonium or hydroxyl are contained by interfacial polymerization formation
There are the polyureas or polyurethane microcapsule of fragrance multicore.It is micro- that CN104353401A reports a kind of multicore plants essential oil sustained release of cohesion again
Capsule selects chitosan to be wrapped up outside plants essential oil core material with Arabic gum as compound wall materials, it is more to obtain regular spherical
The slow release microcapsules of nuclear structure.CN107890841A reports a kind of preparation side for the compound microcapsules that inside is multicore
Method has wrapped up liquid essence and polymer microcapsule/microballoon using spray drying, has obtained water-soluble composite micro-capsule, pass through
Dissolution wall material enables liquid essence and polymer microcapsule/microballoon to release in the different stages.Using above method
The microcapsules that coenocytism can be prepared, stability or slow release to active matter play certain improvement result.But pass through
Microcapsules that these methods obtain or the substance wrapped up are single, can not wrap up the substance of variform simultaneously or obtain
Microcapsules mechanical strength it is poor, in water be easy dissolution.
Summary of the invention
It is an object of the invention to overcome disadvantage existing in the prior art, provide a kind of stability is high, mechanical strength is good,
Inside easy to operate is the preparation method of the slow-release type microcapsule of multicore, can coat the variforms such as liquid and solid-state simultaneously
Substance, and use cross-linked polymer for wall material, improve the stability for being wrapped by substance.
The purpose of the invention is achieved by the following technical solution:
A kind of inside is the preparation method of the slow-release type microcapsule of multicore, internal package liquid essence and porous-starch,
Wall material is crosslinked acrylate polymers, is that will be mixed with acrylate polymer, volatile organic solvent, liquid by mechanical stirring
The suspension of body note essence and porous-starch is distributed in colloid protective agent aqueous solution and forms oil-in-water system, and then decompression goes to remove water
Volatile organic solvent in packet oil systems, acrylate polymer occur interface with liquid essence and porous-starch and mutually separate,
Form the acrylate polymer microcapsules of internal package liquid essence and porous-starch；Ethylene glycol dimethyl is further added
Acrylic ester prepolymer obtains the internal crosslinked acrylate polymers essence microcapsule for multicore after heating curing, i.e., interior
Portion is the slow-release type microcapsule of multicore.
Inside is the preparation method of the slow-release type microcapsule of multicore, is included the following steps:
(1) at room temperature, liquid essence, porous-starch, acrylate polymer are added in volatile organic solvent,
It is thoroughly mixed the suspension for uniformly obtaining that viscosity is 400~3000mPas；
(2) reactor equipped with agitating device is placed in water-bath, bath temperature is 50~60 DEG C, and deionized water is added
And colloid protective agent cools the temperature to 25~30 DEG C after stirring is completely dissolved to colloid protective agent；Then in 400~5000rpm
Revolving speed under, be added step (1) suspension, be dispersed with stirring 10~15min；It is removed again by vacuum pump pressure volatile organic
Solvent obtains the internal acrylate polymer essence microcapsule for multicore until volatile organic solvent completely removes；
(3) under the revolving speed of 500~3000rpm, the ethyleneglycol dimethacrylate that molecular weight is 5000~80000 is added
Ester prepolymer after then heating to 60~75 DEG C of 1~2h of reaction, obtains the internal crosslinked acrylate polymers essence for multicore
Microcapsules, i.e., the internal slow-release type microcapsule for multicore.
In step (1), acrylate polymer is methyl methacrylate-Isooctyl acrylate monomer copolymer, metering system
Sour methyl esters-butyl acrylate copolymer, methacrylic acid-styrol copolymer, Styrene And Butyl-acrylate copolymer, methyl
One of methyl acrylate-acrylic acid copolymer.
Liquid essence is natural oil soluble liquid essence or artificial synthesized oil soluble liquid essence.
The partial size of porous-starch is 400nm-90 μm, preferably 1 μm -30 μm；The inside of porous-starch is adsorbed with liquid perfume
Essence.
Volatile organic solvent is one of methylene chloride, chloroform, acetone, dimethyl carbonate.
In step (1), the dosage of porous-starch is the 7~80% of liquid essence quality.The dosage of acrylate polymer
It is the 8~120% of liquid essence and porous-starch gross mass.
In step (2), the dosage of colloid protective agent is the 0.3~5% of deionized water quality.
Colloid protective agent is one of polyvinyl alcohol, gelatin, Arabic gum.
In step (3), the dosage of ethylene glycol dimethacrylate prepolymer is the 3~75% of liquid essence quality.
Ethylene glycol dimethacrylate prepolymer is added in step (3), is pre- using ethylene glycol dimethacrylate
Polymers and non-crosslinked acrylate polymer have the characteristics that compatibility.Acrylate polymer is non-cross-linked polymer, can be molten
In organic solvent；But non-cross-linked polymer is by thermal fusible solution, therefore its poor heat resistance；Glycol dinitrate is added when further
When base acrylic ester prepolymer, ethylene glycol dimethacrylate prepolymer can move to acrylate polymer microcapsules table
Further crosslinking curing is done by heating in face, and the microcapsule wall is cross-linked polymer after polymerization, can bear higher temperature
Degree, and its mechanical strength is better than non-cross-linked polymer, therefore improves the mechanical strength of slow-release type microcapsule of the present invention and steady
It is qualitative.
The present invention has the following advantages that compared with prior art and effect:
(1) present invention wraps up liquid essence and porous-starch using solvent evaporation method, realizes liquid and solid
The package of equal different shapes active matter, easy to operate, preparation is efficiently, versatile.
(2) multicore essence microcapsule prepared by the present invention, it is internal to have wrapped up liquid essence simultaneously and adsorbed the more of essence
Hole starch overcomes the disadvantage of fragrance evanescence in perfumed products, aroma retaining effect difference, realizes a variety of shapes such as liquid and solid-state
It is coated while state substance, and is wrapped by between substance and is independent of each other, can discharged with having levels to each other, strengthen fragrance
Slow release and persistence, after liquid essence releases, porous-starch can continue to sustained release essence, mutually complementary between the two
It fills, so that microcapsules fragrance on products application is more lasting.
(3) it is wall material that the present invention, which selects environmentally friendly crosslinked acrylate polymers, avoids traditional microcapsules and deposits
The free formaldehyde the problem of, and the acrylate polymer being crosslinked improves machine of the essence microcapsule in daily personal care class product
Tool intensity and thermal stability.
Detailed description of the invention
Fig. 1 is the SEM figure after the crushing for the slow-release type microcapsule that inside of the invention is multicore.
Specific embodiment
Further detailed description is done to the present invention below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) at room temperature by 10g sunflower oil, the porous-starch for being adsorbed with sunflower oil that 1.5g average grain diameter is 20 μm
It is placed in 100ml beaker with 1.7g methyl methacrylate-butyl acrylate copolymer, 20ml methylene chloride is added, sufficiently stirs
Mix the suspension for being 1000mPas to system viscosity；
(2) the 500ml three-necked flask equipped with agitating device is placed in water-bath, bath temperature is 50 DEG C, and 100g is added
Temperature of reaction system is down to 30 DEG C after stirring is completely dissolved to Arabic gum by deionized water and 1.0g Arabic gum,
Under the revolving speed of 1000rpm, the suspension of step (1) is added, is dispersed with stirring 15min, dichloro is then removed by vacuum pump pressure
For methane until completely removing, the methyl methacrylate-butyl acrylate for obtaining internal package sunflower oil and porous-starch is poly-
Close the microcapsules of object；
(3) under the revolving speed of 800rpm, the ethylene glycol dimethacrylate pre-polymerization that 1.0g molecular weight is 10000 is added
Object reacts 2h at 60 DEG C, the methyl methacrylate-butyl acrylate polymer sunflower oil microcapsules being crosslinked.
Sunflower oil microcapsules obtained have apparent multicore coated structure, and internal structure is as shown in Figure 1, from this
It can intuitively prove to be coenocytism inside sunflower oil microcapsules in figure.It is added in liquid detergent, stores 3 at room temperature
A month, microencapsulated forms were full, do not found apparent leakage scenarios.Liquid detergent added with the microcapsules is used for fabric washing
It washs, the fabric after rubbing washing, finds still with the presence of strong fragrance after two weeks.And under equal conditions prepare only package sunflower
The microcapsules of seed oil, are added in liquid detergent, and are used for fabric washing.The fabric after rubbing washing, discovery are knitted after two weeks
Flat aroma on object.
Embodiment 2
(1) at room temperature by 5g lavender oil, the porous-starch for being adsorbed with lavender oil that 0.4g average grain diameter is 10 μm
It is placed in 50ml beaker with 0.6g Styrene And Butyl-acrylate copolymer, 10ml dimethyl carbonate is added, is stirred well to system
Viscosity is the suspension of 500mPas；
(2) the 250ml three-necked flask equipped with agitating device is placed in water-bath, bath temperature is 60 DEG C, and 100g is added
Temperature of reaction system is down to 25 DEG C, in the revolving speed of 200rpm after stirring is completely dissolved to gelatin by deionized water and 0.5g gelatin
Under, the suspension of step (1) is added, is dispersed with stirring 10min, dimethyl carbonate is then removed by vacuum pump pressure until completely
It removes, obtains the Styrene And Butyl-acrylate polymer microcapsule of internal package lavender oil and porous-starch；
(3) under the revolving speed of 500rpm, the ethylene glycol dimethacrylate prepolymer that 3.8g molecular weight is 5000 is added,
1.5h is reacted at 70 DEG C, the acrylate polymer lavender oil microcapsules being crosslinked.
Lavender oil microcapsules obtained have apparent multicore coated structure.It is added in liquid detergent, in room
Temperature lower storage 3 months, microencapsulated forms were full, do not find apparent leakage scenarios.The liquid detergent of the microcapsules will be added with
For fabric washing, the fabric after rubbing washing, is found still with the presence of strong fragrance after two weeks；And it under equal conditions prepares
The microcapsules for only wrapping up lavender oil, are added in liquid detergent, and are used for fabric washing.Knitting after rubbing washing after two weeks
Object finds the flat aroma on fabric.Therefore illustrate that internal is that the acrylate polymer essence microcapsule of multicore has preferably
Slow release, lasting fragrance.
Embodiment 3
(1) at room temperature by 20g lemongrass oil, 16g be adsorbed with lemongrass oil, average grain diameter be 1 μm porous-starch and
2.9g methyl methacrylate-Isooctyl acrylate monomer copolymer is placed in 100ml beaker, and 20ml chloroform is added, sufficiently stirs
Mix the suspension for being 3000mPas to system viscosity；
(2) the 500ml three-necked flask equipped with agitating device is placed in water-bath, bath temperature is 55 DEG C, and 150g is added
Temperature of reaction system is down to 27 DEG C after stirring is completely dissolved to gelatin by deionized water and 0.5g gelatin, in turning for 3000rpm
Under speed, the suspension of step (1) is added, is dispersed with stirring 12min, chloroform is then removed by vacuum pump pressure until completely
It removes, obtains methyl methacrylate-Isooctyl acrylate monomer polymer microcapsule of internal package lemongrass oil and porous-starch；
(3) under the revolving speed of 1500rpm, the ethylene glycol dimethacrylate pre-polymerization that 0.6g molecular weight is 80000 is added
Object reacts 1.5h at 65 DEG C, the acrylate polymer lavender oil microcapsules being crosslinked.
Lemongrass oil microcapsules obtained have apparent multicore coated structure.It is added in liquid detergent, in room
Temperature lower storage 3 months, microencapsulated forms were full, do not find apparent leakage scenarios.The liquid detergent of the microcapsules will be added with
For fabric washing, the fabric after rubbing washing, is found still with the presence of strong fragrance after two weeks；And it under equal conditions prepares
The microcapsules for only wrapping up lemongrass oil, are added in liquid detergent, and are used for fabric washing.Knitting after rubbing washing after two weeks
Object finds the flat aroma on fabric.Therefore illustrate that internal is that the acrylate polymer essence microcapsule of multicore has preferably
Slow release, lasting fragrance.
Embodiment 4
(1) at room temperature by 50g Rosa Damascana, the porous-starch for being adsorbed with Rosa Damascana that 10g average grain diameter is 30 μm
It is placed in 500ml beaker with 36g methyl methacrylate-acrylic acid copolymer, 180ml acetone is added, is stirred well to system
Viscosity is the suspension of 400mPas；
(2) the 1000ml three-necked flask equipped with agitating device is placed in water-bath, bath temperature is 55 DEG C, and 200g is added
Temperature of reaction system is down to 25 DEG C after stirring is completely dissolved to Arabic gum by deionized water and 10g Arabic gum,
Under the revolving speed of 3000rpm, the suspension of step (1) is added, is dispersed with stirring 12min, acetone is then removed by vacuum pump pressure
Until completely removing, the micro- glue of methyl methacrylate-acrylate copolymer of internal package Rosa Damascana and porous-starch is obtained
Capsule；
(3) under the revolving speed of 2000rpm, the ethylene glycol dimethacrylate pre-polymerization that 20g molecular weight is 57000 is added
Object reacts 2h at 68 DEG C, the acrylate polymer lavender oil microcapsules being crosslinked.
Rose essential-oil microcapsule obtained has apparent multicore coated structure.It is added in liquid detergent, in room
Temperature lower storage 3 months, microencapsulated forms were full, do not find apparent leakage scenarios.The liquid detergent of the microcapsules will be added with
For fabric washing, the fabric after rubbing washing, is found still with the presence of strong fragrance after two weeks；And it under equal conditions prepares
The microcapsules for only wrapping up Rosa Damascana, are added in liquid detergent, and are used for fabric washing.Knitting after rubbing washing after two weeks
Object finds the flat aroma on fabric.Therefore illustrate that internal is that the acrylate polymer essence microcapsule of multicore has preferably
Slow release, lasting fragrance.
Embodiment 5
(1) at room temperature by 30g tea oil, 13.5g average grain diameter be 8 μm the porous-starch for being adsorbed with tea oil and
52g methacrylic acid-styrol copolymer is placed in 500ml beaker, and 220ml dimethyl carbonate is added, is stirred well to system
Viscosity is the suspension of 3000mPas；
(2) the 1000ml three-necked flask equipped with agitating device is placed in water-bath, bath temperature is 60 DEG C, and 200g is added
Deionized water and 4g polyvinyl alcohol 1788 (trade names), after stirring is completely dissolved to polyvinyl alcohol 1788, by reaction system temperature
Degree is down to 30 DEG C, under the revolving speed of 1600rpm, the suspension of step (1) is added, is dispersed with stirring 10min, then passes through vacuum pump
Decompression removal dimethyl carbonate obtains methacrylic acid-benzene second of internal package tea oil and porous-starch up to completely removing
Alkene polymer microcapsules；
(3) under the revolving speed of 2000rpm, the ethylene glycol dimethacrylate pre-polymerization that 7.5g molecular weight is 9000 is added
Object reacts 2h at 75 DEG C, the acrylate polymer tea tree oil microcapsule being crosslinked.
Tea tree oil microcapsule obtained has apparent multicore coated structure.It is added in liquid detergent, in room temperature
Lower storage 3 months, microencapsulated forms are full, do not find apparent leakage scenarios.Liquid detergent added with the microcapsules is used
In fabric washing, the fabric after rubbing washing, is found still with the presence of strong fragrance after two weeks；And it under equal conditions prepares only
The microcapsules for wrapping up lavender oil, are added in liquid detergent, and are used for fabric washing.Knitting after rubbing washing after two weeks
Object finds the flat aroma on fabric.Therefore illustrate that internal is that the acrylate polymer essence microcapsule of multicore has preferably
Slow release, lasting fragrance.
Claims (10)
1. the preparation method that a kind of inside is the slow-release type microcapsule of multicore, it is characterised in that: its internal package liquid essence and
Porous-starch, wall material are crosslinked acrylate polymers, are that will be mixed with acrylate polymer by mechanical stirring, volatile have
The suspension of solvent, liquid essence and porous-starch is distributed in colloid protective agent aqueous solution and forms oil-in-water system, then
Boundary occurs for the volatile organic solvent in decompression removal oil-in-water system, acrylate polymer and liquid essence and porous-starch
Face mutually separates, and forms the acrylate polymer microcapsules of internal package liquid essence and porous-starch；Second is further added
Diol dimethacrylate prepolymer obtains the internal crosslinked acrylate polymers essence for multicore after heating curing
Microcapsules, i.e., the internal slow-release type microcapsule for multicore.
2. the preparation method that inside according to claim 1 is the slow-release type microcapsule of multicore, it is characterised in that including under
State step:
(1) at room temperature, liquid essence, porous-starch, acrylate polymer are added in volatile organic solvent, sufficiently
It is uniformly mixed, obtains the suspension that viscosity is 400~3000mPas；
(2) reactor equipped with agitating device is placed in water-bath, bath temperature is 50~60 DEG C, and deionized water and glue is added
Body protective agent cools the temperature to 25~30 DEG C after stirring is completely dissolved to colloid protective agent；Then turn in 400~5000rpm
Under speed, the suspension of step (1) is added, is dispersed with stirring 10~15min；It is removed again by vacuum pump pressure volatile organic molten
Agent obtains the internal acrylate polymer essence microcapsule for multicore until volatile organic solvent completely removes；
(3) under the revolving speed of 500~3000rpm, it is pre- that the ethylene glycol dimethacrylate that molecular weight is 5000~80000 is added
Polymers after then heating to 60~75 DEG C of 1~2h of reaction, obtains the internal micro- glue of crosslinked acrylate polymers essence for multicore
Capsule, i.e., the internal slow-release type microcapsule for multicore.
3. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: third
Olefine acid ester polymer is methyl methacrylate-Isooctyl acrylate monomer copolymer, methyl methacrylate-butyl acrylate copolymerization
Object, methacrylic acid-styrol copolymer, Styrene And Butyl-acrylate copolymer, methyl methacrylate-acrylic acid copolymer
One of object.
4. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: liquid
Body note essence is natural oil soluble liquid essence or artificial synthesized oil soluble liquid essence.
5. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: more
The partial size of hole starch is 400nm-90 μm, and the inside of porous-starch is adsorbed with liquid essence.
6. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: easily
Volatile organic solvent is one of methylene chloride, chloroform, acetone, dimethyl carbonate.
7. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: more
The dosage of hole starch is the 7~80% of liquid essence quality；The dosage of acrylate polymer is liquid essence and porous-starch
The 8~120% of gross mass.
8. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: glue
Body protective agent is one of polyvinyl alcohol, gelatin, Arabic gum.
9. the preparation method that inside according to claim 2 is the slow-release type microcapsule of multicore, it is characterised in that: step
(2) in, the dosage of colloid protective agent is the 0.3~5% of deionized water quality.
10. the preparation method that inside according to claim 1 or 2 is the slow-release type microcapsule of multicore, it is characterised in that: second
The dosage of diol dimethacrylate prepolymer is the 3~75% of liquid essence quality.
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| CN111450077A (en) * | 2020-03-12 | 2020-07-28 | 上海海洋大学 | Millimeter-sized multinuclear capsule for delivering nutrient substances/medicines to small intestine and slowly releasing nutrients/medicines, and preparation method and application thereof |
| CN112089529A (en) * | 2020-08-24 | 2020-12-18 | 浙江珍琦护理用品有限公司 | Paper diaper capable of keeping skin clean and healthy |
| CN113584894A (en) * | 2021-08-27 | 2021-11-02 | 广东优凯科技有限公司 | Fragrance-retaining particle composition and preparation method thereof |
| WO2024023598A1 (en) | 2022-07-25 | 2024-02-01 | S H Kelkar And Company Limited | Microcapsules and encapsulation thereof |
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