CN108097185A - A kind of method for preparing melamine resin essence microcapsule finishing agent - Google Patents
A kind of method for preparing melamine resin essence microcapsule finishing agent Download PDFInfo
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- CN108097185A CN108097185A CN201711389842.0A CN201711389842A CN108097185A CN 108097185 A CN108097185 A CN 108097185A CN 201711389842 A CN201711389842 A CN 201711389842A CN 108097185 A CN108097185 A CN 108097185A
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- maleic anhydride
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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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- 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
- B01J13/16—Interfacial polymerisation
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/005—Compositions containing perfumes; Compositions containing deodorants
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
- D06M15/233—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated aromatic, e.g. styrene
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/31—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated nitriles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention discloses a kind of methods for preparing melamine resin essence microcapsule finishing agent, first using styrene maleic anhydride copolymer as emulsifier, essence is capsule-core, using melamine resin and polyacrylate as wall material, packing is carried out to essence respectively by situ aggregation method and interfacial polymerization respectively, melamine resin essence microcapsule is prepared.Effect of the present invention is to be made self bonding double-walled essence microcapsule using a kind of preparation method of safety and environmental protection, and solid content is 35% 38%, other essence microcapsule solid contents are higher by 10% 15% more on the market.Double-deck wall building is carried out by situ aggregation method and interfacial polymerization, to essence encapsulation ratio up to 91% 95%, product lotion is with good stability.Self bonding double-walled essence microcapsule enables it to possess self-adhesiveness, simplifies Cellulase Finishing Process for Cotton Fabric while holding microcapsules peculiar advantage.And the cotton fabric aroma retaining effect arranged is good, stands lasting up to 8 months, pleasant fragrance still can be kept after washing 12 times.
Description
Technical field
The invention belongs to spinning post-finishing technical fields, and in particular to one kind is fragrant using low methyl-etherified melamine resin as wall material
Essence is core, passes through a kind of method for preparing melamine resin essence microcapsule finishing agent of situ aggregation method preparation.
Background technology
With the development of economy and improvement of living standard, requirement of the people to textile have changed a lot,
From it is past it is practical to decoration, enjoy, health conversion, textile flavoring complied with this trend.Due to fragrant textile
There is antibacterial expelling parasite, covering smell, make body and mind comfortable, thus obtained generally liking for people.Ancient Times in China just has
The custom of sachet is sewed on clothes；Just using on clothing, perfumes are as graceful style since Middle Ages in Europe, later,
There is the method for perfume again；Foreign countries also have adsorbs fragrance using activated carbon fiber, is attached on clothes.In the 60-70 ages in 20th century, use
Leaching is fragrant and applies fragrant method that fragrance is transmitted to fabric is rather popular.The microencapsulation coating technology of the eighties, really opens fragrance
The market of textile.
Microcapsules technology refers to be coated on purpose thing wherein using natural or synthesis high molecular material, formation
Diameter is from several to hundreds of μm or even the small container of thousands of μm of nucleocapsid structure.Essence completely cuts off with external environment after microencapsulation,
Its property is basically unchanged, and essence during beginning in microcapsules outer layer is fragrant；Then in the wearing process of textile, by
In be subjected to rubbing, the external effect such as be heated, the essence inside microcapsules is made gently to discharge fragrance, plays the work of long-acting slow-release
With so that textile has quite lasting aromatic function.Traditional microcapsules technology is usually prepared various with physical method
Then microcapsules using adhesive and crosslinking agent are mechanically adhered on fabric fibre, stayed by the essence microcapsule of open cell type
The fragrant time is not grown；Simultaneously because the presence of adhesive, feel is bad, comfort when influencing to wear.
However encapsulation ratio of the essence microcapsule nowadays sold on the market often there are essence is low, the mechanical strength of cyst wall
The shortcomings of low, fragrance remaining time is short, low with the affinity of fabric fibre, Nian Jie difficulty.It has been investigated that use situ aggregation method with
Cross-linking modified melamine resin is that wall material essence is that core prepares a kind of totally-enclosed pressure sensitive aromatic micro-capsule, when can extend lasting
Between；Outer wall layer functionalization enhances the binding strength with fabric fibre, and the product can be made to meet difference and benefit from object-oriented requirements, widened
The accommodation of microcapsule essence.
The content of the invention
The present invention seeks to be intended to provide a kind of method for preparing melamine resin essence microcapsule finishing agent, in favor of subtracting
The volatilization of few essence and spoilage problems make it be easy to fabric fibre combination in application process, and the fragrant time is released in extension, and makes to release perfume (or spice)
With controllability.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
(1) preparation of styrene-maleic anhydride copolymer powder
Monomer maleic anhydride, styrene and initiator are added in solvent and fully dissolved, then mixes above-mentioned reaction
Object is heated to 100-130 DEG C of reaction 1.5-24h, obtains the metastable state dispersion of copolymer, after the completion of reaction, is centrifuged
And filtering, it finally dries, obtains styrene-maleic anhydride copolymer powder；
Wherein, the initiator is organic peroxide；The solvent is organic acid alkylester did；Styrene and Malaysia
Acid anhydrides uses magnitude relation, is in molar ratio 9.7:0.3-5:5, the mass concentration of monomer styrene and maleic anhydride in reaction system
The sum of be 15%-55%；The quality of initiator is the 0.5-5% of monomer gross mass in reaction system；
(2) preparation of styrene-maleic anhydride copolymer solution
Added in by weight in four-hole bottle the styrene-maleic anhydride copolymer powder that is prepared in 1-3 part steps (1) with
17-19 parts of deionized waters, heating temperature is to 65-85 DEG C under agitation, and adjusts pH with the NaOH solution that concentration is 25%
To 8-10, when reaction 3-5 is small after obtain styrene-maleic anhydride copolymer solution；
(3) preparation of melamine resin performed polymer
5-10 parts of melamines and 37% formalin of 10-20 parts are put into four-hole bottle by weight, in stirring bar
60-80 DEG C is warming up under part, after melamine is entirely molten, 0.1-1 parts of triethanolamines is added in, adjusts pH to 7-10, react 10-30
Minute can obtain the melamine resin performed polymer of clear viscous；
(4) preparation of self bonding double-walled essence microcapsule
By weight by 10-30 parts of essence, 2-5 parts of methyl methacrylates, 2-5 parts of acrylonitrile, 1-3 parts of acrylic acid fourths
Ester, 1-3 part Isooctyl acrylate monomer, 0.2-0.5 parts of methacrylic acids, 0.2-0.5 parts of hydroxy-ethyl acrylates, 0.1-0.3 parts double third
Ketone acrylamide, 0.1-0.3 part adipic dihydrazide, 0.02-0.05 parts of azodiisobutyronitriles are collectively disposed in beaker, in temperature
It is stirred at 30-50 DEG C and is configured to homogeneous oil solution；
By above-mentioned homogeneous oil solution and the phenylethylene-maleic anhydride of the middle preparation of 20-40 part steps (2) weighed by weight
AEO-9,0.5-2 parts of copolymer solution, 30-50 part water, 1-5 portions of nonionic surfactants lauryl sodium sulfate SDS are common
It is placed in beaker, and is emulsified with high-shearing dispersion emulsifying machine under the rotating speed of 5000-15000r/min, obtain core breast
Liquid；
Core material emulsion is moved in four-hole bottle, under agitation, adjusts pH to 6-7 with glacial acetic acid solution, by weight
The melamine resin performed polymer prepared in 5-10 parts of steps (3) is added in, pH to 4-5 is adjusted with glacial acetic acid solution again, at 50-70 DEG C
Under the conditions of stirring cure 0.5-1 it is small when, form melamine resin wall, then under nitrogen protection, 1- kept the temperature at 70-90 DEG C of temperature
3 it is small when, formed with adhesive property acrylate wall, Temperature fall, then with concentration be 30% NaOH solution adjust pH to
6-8 obtains self bonding double-walled essence microcapsule.
It further limits, in step (1), organic acid alkylester did is ethyl butyrate, isoamyl acetate, ethyl propionate.
Beneficial effects of the present invention：
(1) self bonding double-walled essence microcapsule solid content is 35%-38%, more on the market other essence microcapsule solid contents
10%-15% can be higher by.Double-walled wraps up essence simultaneously, and encapsulation ratio is up to 91%-95%.
(2) double-deck wall building is carried out by situ aggregation method and interfacial polymerization, while holding microcapsules peculiar advantage,
It is enable to possess self-adhesiveness, simplifies Cellulase Finishing Process for Cotton Fabric.And the cotton fabric aroma retaining effect arranged is good, stands lasting
Up to 8 months, pleasant fragrance still can be kept after washing 12 times.
Specific embodiment
In order to make those skilled in the art that the present invention may be better understood, with reference to embodiment to the technology of the present invention
Scheme further illustrates.
A kind of method for preparing melamine resin essence microcapsule finishing agent, includes the following steps：
(1) preparation of styrene-maleic anhydride copolymer powder
Monomer maleic anhydride, styrene and initiator are added in solvent and fully dissolved, then mixes above-mentioned reaction
Object is heated to 100-130 DEG C of reaction 1.5-24h, obtains the metastable state dispersion of copolymer, after the completion of reaction, is centrifuged
And filtering, it finally dries, obtains styrene-maleic anhydride copolymer powder；
Wherein, the initiator is organic peroxide；The solvent is organic acid alkylester did；Styrene and Malaysia
Acid anhydrides uses magnitude relation, is in molar ratio 9.7:0.3-5:5, the mass concentration of monomer styrene and maleic anhydride in reaction system
The sum of be 15%-55%；The quality of initiator is the 0.5-5% of monomer gross mass in reaction system；
(2) preparation of styrene-maleic anhydride copolymer solution
Added in by weight in four-hole bottle the styrene-maleic anhydride copolymer powder that is prepared in 1-3 part steps (1) with
17-19 parts of deionized waters, heating temperature is to 65-85 DEG C under agitation, and adjusts pH with the NaOH solution that concentration is 25%
To 8-10, when reaction 3-5 is small after obtain styrene-maleic anhydride copolymer solution；
(3) preparation of melamine resin performed polymer
5-10 parts of melamines and 37% formalin of 10-20 parts are put into four-hole bottle by weight, in stirring bar
60-80 DEG C is warming up under part, after melamine is entirely molten, 0.1-1 parts of triethanolamines is added in, adjusts pH to 7-10, react 10-30
Minute can obtain the melamine resin performed polymer of clear viscous；
(4) preparation of self bonding double-walled essence microcapsule
By weight by 10-30 parts of essence, 2-5 parts of methyl methacrylates, 2-5 parts of acrylonitrile, 1-3 parts of acrylic acid fourths
Ester, 1-3 part Isooctyl acrylate monomer, 0.2-0.5 parts of methacrylic acids, 0.2-0.5 parts of hydroxy-ethyl acrylates, 0.1-0.3 parts double third
Ketone acrylamide, 0.1-0.3 part adipic dihydrazide, 0.02-0.05 parts of azodiisobutyronitriles are collectively disposed in beaker, in temperature
It is stirred at 30-50 DEG C and is configured to homogeneous oil solution；
By above-mentioned homogeneous oil solution and the phenylethylene-maleic anhydride of the middle preparation of 20-40 part steps (2) weighed by weight
AEO-9,0.5-2 parts of copolymer solution, 30-50 part water, 1-5 portions of nonionic surfactants lauryl sodium sulfate SDS are common
It is placed in beaker, and is emulsified with high-shearing dispersion emulsifying machine under the rotating speed of 5000-15000r/min, obtain core breast
Liquid；
Core material emulsion is moved in four-hole bottle, under agitation, adjusts pH to 6-7 with glacial acetic acid solution, by weight
The melamine resin performed polymer prepared in 5-10 parts of steps (3) is added in, pH to 4-5 is adjusted with glacial acetic acid solution again, at 50-70 DEG C
Under the conditions of stirring cure 0.5-1 it is small when, form melamine resin wall, then under nitrogen protection, 1- kept the temperature at 70-90 DEG C of temperature
3 it is small when, formed with adhesive property acrylate wall, Temperature fall, then with concentration be 30% NaOH solution adjust pH to
6-8 obtains self bonding double-walled essence microcapsule.
In step (1), organic acid alkylester did is ethyl butyrate, isoamyl acetate, ethyl propionate.
Embodiment 1
(1) preparation of styrene-maleic anhydride copolymer powder
Monomer maleic anhydride, styrene and initiator are added in solvent and fully dissolved, then mixes above-mentioned reaction
Object is heated to 100 DEG C of reaction 1.5h, obtains the metastable state dispersion of copolymer, after the completion of reaction, is centrifuged and filters,
It finally dries, obtains styrene-maleic anhydride copolymer powder；
Wherein, the initiator is organic peroxide；The solvent is organic acid alkylester did；Styrene and Malaysia
Acid anhydrides uses magnitude relation, is in molar ratio 9.7:0.3, the sum of mass concentration of monomer styrene and maleic anhydride in reaction system
For 15%；The quality of initiator is the 0.5% of monomer gross mass in reaction system；
(2) preparation of styrene-maleic anhydride copolymer solution
1 part of styrene-maleic anhydride copolymer powder and 17 parts of deionized waters are added in by weight in four-hole bottle, are being stirred
65 DEG C are heated under the conditions of mixing, pH to 8 is adjusted with the NaOH solution of concentration 25%, 3 it is small when after polyelectrolyte styrene-
Copolymer-maleic anhydride solution.
(3) preparation of melamine resin performed polymer
5 parts of melamines and 10 part of 37% formalin are put into four-hole bottle by weight.Stirring is warming up to 60 DEG C,
After melamine is entirely molten, 0.1 part of triethanolamine is added in by weight, adjusts pH to 7, and reaction obtains clear viscous after ten minutes
Melamine resin performed polymer.
(4) preparation of self bonding double-walled essence microcapsule
By weight by 10 parts of essence, 2 parts of methyl methacrylates, 2 parts of acrylonitrile, 1 part of butyl acrylate, 1 part of propylene
The different monooctyl ester of acid, 0.2 part of methacrylic acid, 0.2 part of hydroxy-ethyl acrylate, 0.1 part of Diacetone Acrylamide, 0.1 part of adipic acid two
Hydrazides, 0.02 part of azodiisobutyronitrile are collectively disposed in beaker, are stirred at 30 DEG C, are configured to homogeneous oil solution.
By homogeneous oil solution with prepared before by weight weigh 20 parts styrene-maleic anhydride copolymer solution,
30 parts of water, 1 part of nonionic surfactant AEO-9,0.5 part of lauryl sodium sulfate SDS are collectively disposed in beaker, and are cut with height
It cuts dispersion emulsifying machine to be emulsified under the rotating speed of 5000r/min, obtains core material emulsion.Core material emulsion is moved in four-hole bottle,
Under agitation, pH to 6 is adjusted with glacial acetic acid solution.5 parts of melamine resin performed polymers are added in by weight, use glacial acetic acid again
Solution adjusts pH to 4.When stirring curing 0.5 is small under the conditions of 50 DEG C, melamine resin wall is formed.Then under nitrogen protection, exist
When heat preservation 1 is small at 70 DEG C, the acrylate wall with adhesive property is formed.Temperature fall, then adjusted with 30% NaOH solution
PH to 6 obtains self bonding double-walled essence microcapsule.In the application process of this self bonding double-walled essence microcapsule, by weight
Part takes 2 parts of self bonding double-walled essence microcapsules and 95 parts of water, and the two is mixed to obtain essence microcapsule lotion in beaker, cotton is knitted
Object is put into essence microcapsule lotion, is impregnated 10 minutes at 40 DEG C, is then dried cotton fabric, obtain liquid carrying rate (i.e. essence
Microcapsule emulsion content) be 70% band liquid cotton fabric, will be baked at 50 DEG C with liquid cotton fabric 10 minutes, finally by its nature
It dries, obtains finishing of cotton textiles.
The solid content 34.05% of gained self bonding double-walled microcapsule emulsion, essence encapsulation ratio 90.54%.Obtained arrangement
Fabric stood fragrance remaining time up to 6 months, remained to keep pleasant fragrance after washing 10 times.When standing lasting compared with similar products
Between improve 30%, and possess the self-adhesiveness not available for other products can and outstanding wash durability.
The application of the melamine resin essence microcapsule of the present invention, by weight by 2-5 parts of self bonding double-walled essence microcapsules
Essence microcapsule lotion is mixed to obtain with 95-98 parts of water, cotton fabric is put into essence microcapsule lotion, is impregnated at 40-60 DEG C
10-20 minutes, then cotton fabric is dried, obtain the band liquid cotton fabric that liquid carrying rate is 70%-90%, the micro- glue of liquid carrying rate, that is, essence
Capsule emulsion content.It will be baked at 50-70 DEG C with liquid cotton fabric 10-30 minutes, and finally by its naturally dry, obtain arrangement cotton and knit
Object.
Embodiment 2
(1) preparation of styrene-maleic anhydride copolymer powder
Monomer maleic anhydride, styrene and initiator are added in solvent and fully dissolved, then mixes above-mentioned reaction
Object is heated to 130 DEG C of reactions for 24 hours, obtains the metastable state dispersion of copolymer, after the completion of reaction, is centrifuged and filters,
It finally dries, obtains styrene-maleic anhydride copolymer powder；
Wherein, the initiator is organic peroxide；The solvent is organic acid alkylester did；Styrene and Malaysia
Acid anhydrides uses magnitude relation, is in molar ratio 5:5, the sum of mass concentration of monomer styrene and maleic anhydride is in reaction system
55%；The quality of initiator is the 5% of monomer gross mass in reaction system；
(2) preparation of styrene-maleic anhydride copolymer solution
3 parts of styrene-maleic anhydride copolymer powder and 17 parts of deionized waters are added in by weight in four-hole bottle, are being stirred
85 DEG C are heated under the conditions of mixing, pH to 10 is adjusted with the NaOH solution of concentration 25%, 5 it is small when after polyelectrolyte benzene second
Alkene-copolymer-maleic anhydride solution.
(3) preparation of melamine resin performed polymer
10 parts of melamines and 20 part of 37% formalin are put into four-hole bottle by weight.Stirring is warming up to 80
DEG C, after melamine is entirely molten, 11 parts of triethanolamines are added in by weight, adjust pH to 10, and reaction obtains transparent after 30 minutes
Sticky melamine resin performed polymer.
(4) preparation of self bonding double-walled essence microcapsule
By weight by 30 parts of essence, 5 parts of methyl methacrylates, 5 parts of acrylonitrile, 3 parts of butyl acrylates, 3 parts of propylene
The different monooctyl ester of acid, 0.5 part of methacrylic acid, 0.5 part of hydroxy-ethyl acrylate, 0.3 part of Diacetone Acrylamide, 0.3 part of adipic acid two
Hydrazides, 0.05 part of azodiisobutyronitrile are collectively disposed in beaker, are stirred at 50 DEG C, are configured to homogeneous oil solution.
By homogeneous oil solution with prepared before by weight weigh 40 parts styrene-maleic anhydride copolymer solution,
50 parts of water, 5 parts of nonionic surfactant AEO-9,0.5 part of lauryl sodium sulfate SDS are collectively disposed in beaker, and are cut with height
It cuts dispersion emulsifying machine to be emulsified under the rotating speed of 15000r/min, obtains core material emulsion.Core material emulsion is moved in four-hole bottle,
Under agitation, pH to 7 is adjusted with glacial acetic acid solution.10 parts of melamine resin performed polymers are added in by weight, again with ice vinegar
Acid solution adjusts pH to 5.When stirring curing 1 is small under the conditions of 70 DEG C, melamine resin wall is formed.Then under nitrogen protection, exist
When heat preservation 3 is small at 70 DEG C, the acrylate wall with adhesive property is formed.Temperature fall, then adjusted with 30% NaOH solution
PH to 8 obtains self bonding double-walled essence microcapsule.In the application process of this self bonding double-walled essence microcapsule, by weight
Part takes 5 parts of self bonding double-walled essence microcapsules and 98 parts of water, and the two is mixed to obtain essence microcapsule lotion in beaker, cotton is knitted
Object is put into essence microcapsule lotion, is impregnated 20 minutes at 60 DEG C, is then dried cotton fabric, obtain liquid carrying rate (i.e. essence
Microcapsule emulsion content) be 90% band liquid cotton fabric, will be baked at 70 DEG C with liquid cotton fabric 30 minutes, finally by its nature
It dries, obtains finishing of cotton textiles.
The solid content 30.78% of gained self bonding double-walled microcapsule emulsion, essence encapsulation ratio 93.69%.Obtained arrangement
Fabric stood fragrance remaining time up to 8 months, remained to keep pleasant fragrance after washing 12 times.When standing lasting compared with similar products
Between improve 30%, and possess the self-adhesiveness not available for other products can and outstanding wash durability.
Detailed Jie has been carried out to a kind of method for preparing melamine resin essence microcapsule finishing agent provided by the invention above
It continues.The explanation of specific embodiment is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that for this skill
For the those of ordinary skill in art field, without departing from the principle of the present invention, several change can also be carried out to the present invention
Into and modification, these improvement and modification are also fallen into the protection domain of the claims in the present invention.
Claims (2)
- A kind of 1. method for preparing melamine resin essence microcapsule finishing agent, it is characterised in that：Include the following steps,(1) preparation of styrene-maleic anhydride copolymer powderMonomer maleic anhydride, styrene and initiator are added in solvent and fully dissolved, then adds above-mentioned reaction mixture Heat obtains the metastable state dispersion of copolymer, after the completion of reaction, is centrifuged and mistake to 100-130 DEG C of reaction 1.5-24h Filter, finally dries, obtains styrene-maleic anhydride copolymer powder；Wherein, the initiator is organic peroxide；The solvent is organic acid alkylester did；Styrene and maleic anhydride Use magnitude relation, be in molar ratio 9.7:0.3-5:5, the sum of mass concentration of monomer styrene and maleic anhydride in reaction system For 15%-55%；The quality of initiator is the 0.5-5% of monomer gross mass in reaction system；(2) preparation of styrene-maleic anhydride copolymer solutionThe styrene-maleic anhydride copolymer powder and 17- prepared in 1-3 parts of steps (1) is added in by weight in four-hole bottle 19 parts of deionized waters, heating temperature is to 65-85 DEG C under agitation, and adjusts pH to 8- with the NaOH solution that concentration is 25% 10, reaction 3-5 it is small when after obtain styrene-maleic anhydride copolymer solution；(3) preparation of melamine resin performed polymer5-10 parts of melamines and 37% formalin of 10-20 parts are put into four-hole bottle by weight, under agitation 60-80 DEG C is warming up to, after melamine is entirely molten, 0.1-1 parts of triethanolamines is added in, adjusts pH to 7-10, react 10-30 minutes It can obtain the melamine resin performed polymer of clear viscous；(4) preparation of self bonding double-walled essence microcapsuleBy weight by 10-30 parts of essence, 2-5 parts of methyl methacrylates, 2-5 parts of acrylonitrile, 1-3 parts of butyl acrylates, 1-3 Part Isooctyl acrylate monomer, 0.2-0.5 parts of methacrylic acids, 0.2-0.5 parts of hydroxy-ethyl acrylates, 0.1-0.3 parts of diacetone acrylamides Amide, 0.1-0.3 part adipic dihydrazide, 0.02-0.05 parts of azodiisobutyronitriles are collectively disposed in beaker, in temperature 30-50 It is stirred at DEG C and is configured to homogeneous oil solution；By above-mentioned homogeneous oil solution and the styrene-maleic anhydride copolymer of the middle preparation of 20-40 part steps (2) weighed by weight AEO-9,0.5-2 parts of object solution, 30-50 part water, 1-5 portions of nonionic surfactants lauryl sodium sulfate SDS are collectively disposed at It in beaker, and is emulsified with high-shearing dispersion emulsifying machine under the rotating speed of 5000-15000r/min, obtains core material emulsion；Core material emulsion is moved in four-hole bottle, under agitation, pH to 6-7 is adjusted with glacial acetic acid solution, adds in by weight The melamine resin performed polymer prepared in 5-10 parts of steps (3) adjusts pH to 4-5, in 50-70 DEG C of condition with glacial acetic acid solution again Lower stirring cure 0.5-1 it is small when, form melamine resin wall, then under nitrogen protection, it is small that 1-3 kept the temperature at 70-90 DEG C of temperature When, the acrylate wall with adhesive property, Temperature fall are formed, then pH to 6-8 is adjusted with the NaOH solution that concentration is 30%, Obtain self bonding double-walled essence microcapsule.
- 2. a kind of method for preparing melamine resin essence microcapsule finishing agent according to claim 1, it is characterised in that：Step Suddenly in (1), organic acid alkylester did is ethyl butyrate, isoamyl acetate, ethyl propionate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110952305A (en) * | 2019-12-24 | 2020-04-03 | 福建恒安集团有限公司 | Solid fragrance type clothing cleaning additive |
| CN112457777A (en) * | 2020-11-30 | 2021-03-09 | 江苏科技大学 | Water-based asphalt waterproof coating and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230766A (en) * | 2013-05-08 | 2013-08-07 | 天津城市建设学院 | Preparation and application of self-adhesive double-wall essence microcapsule |
| CN103233368A (en) * | 2013-05-08 | 2013-08-07 | 天津城市建设学院 | Preparation and applications of modified melamine resin essence microcapsule finishing agent |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230766A (en) * | 2013-05-08 | 2013-08-07 | 天津城市建设学院 | Preparation and application of self-adhesive double-wall essence microcapsule |
| CN103233368A (en) * | 2013-05-08 | 2013-08-07 | 天津城市建设学院 | Preparation and applications of modified melamine resin essence microcapsule finishing agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110952305A (en) * | 2019-12-24 | 2020-04-03 | 福建恒安集团有限公司 | Solid fragrance type clothing cleaning additive |
| CN110952305B (en) * | 2019-12-24 | 2022-05-10 | 福建恒安集团有限公司 | Solid fragrance type clothing cleaning additive |
| CN112457777A (en) * | 2020-11-30 | 2021-03-09 | 江苏科技大学 | Water-based asphalt waterproof coating and preparation method and application thereof |
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