CN103233368B - Preparation and application of modified melamine resin essence microcapsule finishing agent - Google Patents
Preparation and application of modified melamine resin essence microcapsule finishing agent Download PDFInfo
- Publication number
- CN103233368B CN103233368B CN201310165451.6A CN201310165451A CN103233368B CN 103233368 B CN103233368 B CN 103233368B CN 201310165451 A CN201310165451 A CN 201310165451A CN 103233368 B CN103233368 B CN 103233368B
- Authority
- CN
- China
- Prior art keywords
- melamine resin
- modified melamine
- essence microcapsule
- preparation
- solution
- 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.)
- Expired - Fee Related
Links
- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 77
- 239000004640 Melamine resin Substances 0.000 title claims abstract description 74
- 239000003094 microcapsule Substances 0.000 title claims abstract description 71
- 150000007974 melamines Chemical class 0.000 title claims abstract description 67
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000004744 fabric Substances 0.000 claims abstract description 40
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000000839 emulsion Substances 0.000 claims description 35
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000013019 agitation Methods 0.000 claims description 21
- 239000011162 core material Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 230000000740 bleeding effect Effects 0.000 claims description 10
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- 239000007767 bonding agent Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 239000004902 Softening Agent Substances 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000002736 nonionic surfactant Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000004753 textile Substances 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004663 anionic softener Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000000835 fiber Substances 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 230000008859 change Effects 0.000 abstract description 5
- 239000002304 perfume Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003995 emulsifying agent Substances 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract 2
- 239000002775 capsule Substances 0.000 abstract 1
- 239000003205 fragrance Substances 0.000 description 12
- 235000013599 spices Nutrition 0.000 description 7
- 238000005538 encapsulation Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000002045 lasting effect Effects 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000001143 conditioned effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 206010011732 Cyst Diseases 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 208000031513 cyst Diseases 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 244000215068 Acacia senegal Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- 241000322338 Loeseliastrum Species 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- -1 can pad Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses preparation and applications of a modified melamine resin essence microcapsule finishing agent. The preparation comprises the steps of: firstly, preparing a modified melamine resin essence microcapsule by taking styrene-maleic anhydride copolymer as an emulsifying agent, essence as a capsule core and a low-methylesterification melamine resin as a wall material, then preparing a modified melamine resin essence microcapsule finishing agent by taking the modified melamine resin essence microcapsule as raw materials. The invention also provides a method for applying the modified melamine resin essence microcapsule finishing agent. According to the invention, the solid content of the modified melamine resin essence microcapsule obtained by adopting a simple, convenient and environment-friendly preparation method can achieve 30-35%, which is improved by 10-15% compared with the solid content of other essence microcapsule products sold in the market, the essence envelop rate can achieve 90-95%, and the modified melamine resin essence microcapsule has good stability. In addition, the modified melamine resin essence microcapsule finishing agent prepared by taking the essence microcapsule as raw materials has a good bonding effect with fabric fibers, is long in fabric perfume retention time, the standing perfume retention time can last six months, and the perfume has no obvious change after the fabric is washed for three times.
Description
Technical field
The invention belongs to spinning post-finishing technical field, be specifically related to one with low methyl-etherified melamine resin for wall material, essence is core, the preparations and applicatio of a kind of modified melamine resin essence microcapsule finishing agent prepared by situ aggregation method.
Background technology
Microcapsules technology is that one utilizes macromolecular material, active material embedding is got up, and forms the microencapsulation technology with semipermeable or sealing cyst membrane.It can improve the physical property being wrapped material, active component and external environment is completely cut off and comes, strengthen stability, reduce volatility, extend storage life, have Co ntrolled release function in addition.
Textile with aromatic odor is well received by consumers.But the composition of essence is very complicated.The composition wherein contained mostly is volatile, the material of unstable chemcial property, so in order to protect essence from the impact of external environment between use and storage life, making fragrance slowly-releasing, reaching and extending the object that it protects the fragrant phase, preferably essence microcapsule.Then by different purposes and requirement, prepare pastil on various light textile goods in modes such as emulsion dispersions, spice finish is carried out to fiber or fabric.This product starts to be only limitted to calico, has developed on the multiple textiles such as clothes, necktie, scarf, sheet, handkerchief, socks at present.
Italy Eurand develops the microcapsules containing spices by condensation technique, as being encapsulated in the microcapsules of gum arabic and gelatin by the spices of swallow clothing grass or pine tar; Euracli company of France produces microcapsules containing spices or cosmetic moisturizers, can pad, coating or sparge on textile, and with polyacrylic acid or the adhesion of polyurethane adhesive.Produce the product of many fiber types at present, as fragrance scarf, lingerie, women's dress, dewing and energization tight socks etc.; Britain L.J.Specialitles produces the spices had wide range of applications, as the microcapsules that cologne and fruity odours (smell as fresh in apple, orange etc.) are made, for the Final finishing of sheet, towel and clothes, mild wear in routine use can discharge spices. and microcapsules can make dispersant with adhesive, application is padded, exhaust or the method such as wire mark puts on bafta, can cyclic washing be stood, but usually with softening agent to improve feel.Germany Hako-Werke GmbH fabric, can discharge fresh fragrance between the normal operating period.
But the encapsulation ratio that nowadays sold on the market essence microcapsule often exists essence is low, the mechanical strength of cyst wall is low, and fragrance remaining time is short, the shortcoming such as, bonding difficulty low with the affinity of fabric fibre.Find after deliberation, adopt situ aggregation method with cross-linking modified melamine resin for wall material essence for a kind of totally-enclosed pressure sensitive aromatic micro-capsule prepared by core, can fragrance remaining time be extended; Outer wall layer functionalization enhances the binding strength with fabric fibre, this product can be made to meet difference and benefit from object-oriented requirements, widen the accommodation of microcapsule essence.
Summary of the invention
The object of the invention is the preparations and applicatio providing a kind of modified melamine resin essence microcapsule finishing agent, be beneficial to the volatilization and the spoilage problems that reduce essence, make it in application process, be easy to fabric fibre to combine, extend and release the fragrant time, and make to release perfume (or spice) there is controllability.
For achieving the above object, the technical scheme of employing is to provide a kind of preparations and applicatio method of modified melamine resin essence microcapsule finishing agent, comprises the steps:
(1) preparation of styrene-maleic anhydride copolymer powder
By weight 20-30 part styrene, 20-30 part maleic anhydride, 100-120 part acetone and 0.2-0.5 part benzoyl peroxide initator are put into four-hole bottle, by nitrogen bubble 5-15 minute, slowly heat up under agitation, 50-70 DEG C is maintained the temperature at after raw material all dissolves, reaction 1-3 hour, add 10-15 part ethanol, obtain White Flocculus, and after dry, grinding styrene-maleic anhydride copolymer powder;
(2) preparation of styrene-maleic anhydride copolymer solution
Styrene-maleic anhydride copolymer powder and 85-95 part deionized water of preparation in 5-15 part step (1) is added by weight in four-hole bottle, be heated temperature under agitation at 60-80 DEG C, pH is regulated by the NaOH solution that concentration is 30%, pH is 7-10 to terminal, water white transparency or thick pale yellow solution, i.e. styrene-maleic anhydride copolymer solution is obtained after 3-5 hour;
(3) preparation of modified melamine resin solution
By weight 70-90 part modified melamine resin and 30-50 part deionized water are stirred in beaker miscible after, obtain modified melamine resin solution, for subsequent use;
(4) preparation of modified melamine resin essence microcapsule emulsion
By weight the styrene-maleic anhydride copolymer solution of preparation in 20-40 part step (2), 20-40 part deionized water, 10-30 part essence, 1-5 part non-ionic surfactant OP-10,1-5 part sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification by high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, pH to 5-7 is regulated with glacial acetic acid solution, and the modified melamine resin solution of preparation in adding 6-18 part step (3) by weight, again regulate pH to 3-5 with glacial acetic acid solution, be warming up to 60-70 DEG C under agitation, solidification 0.5-1.5 hour, Temperature fall, ageing 1-3 hour, then by the NaOH solution that concentration is 30%, pH is adjusted to neutrality, obtain modified melamine resin essence microcapsule emulsion;
(5) preparation of modified melamine resin essence microcapsule finishing agent
To get in 5-10 part step (4) obtained modified melamine resin essence microcapsule emulsion by weight, 1-3 part bleeding agent, 1-3 part bonding agent, 1-3 part softening agent stir fully mixing in beaker, obtain modified melamine resin essence microcapsule finishing agent.
A kind of application of modified melamine resin essence microcapsule finishing agent is also provided simultaneously.
Effect of the present invention is:
(1) solid content of modified melamine resin essence microcapsule can reach 30%-35%, and comparing other essence microcapsule product solid contents commercially available can improve 10%-15%, and it can reach 90%-95% to the encapsulation ratio of essence.
(2) adopt modification wall material, make the building-up process of essence microcapsule be more prone to control, have good storage stability, after washing 3 times, fragrance is without significant change.Meanwhile, the finishing agent prepared for raw material with it and fabric fibre adhesive effect good, fabric aroma retaining effect is long, and standing lasting can reach 6 months.
Detailed description of the invention
Be described in detail in conjunction with the preparations and applicatio of embodiment to modified melamine resin essence microcapsule finishing agent of the present invention.
The preparation of modified melamine resin essence microcapsule finishing agent of the present invention, be first take styrene-maleic anhydride copolymer as emulsifying agent, essence is capsule-core, and low methyl-etherified melamine resin is wall material, prepares modified melamine resin essence microcapsule.Then, with this essence microcapsule emulsion for raw material has prepared a kind of modified melamine resin essence microcapsule finishing agent.Finally, the application process of this modified melamine resin essence microcapsule finishing agent is provided.
The preparation method of modified melamine resin essence microcapsule finishing agent comprises the following steps:
(1) preparation of styrene-maleic anhydride copolymer powder
By weight 20-30 part styrene, 20-30 part maleic anhydride, 100-120 part acetone and 0.2-0.5 part benzoyl peroxide initator are put into four-hole bottle, by nitrogen bubble 5-15 minute, slowly heat up under agitation, 50-70 DEG C is maintained the temperature at after raw material all dissolves, reaction 1-3 hour, add 10-15 part ethanol, obtain White Flocculus, and after dry, grinding styrene-maleic anhydride copolymer powder;
(2) preparation of styrene-maleic anhydride copolymer solution
Styrene-maleic anhydride copolymer powder and 85-95 part deionized water of preparation in 5-15 part step (1) is added by weight in four-hole bottle, be heated temperature under agitation at 60-80 DEG C, pH is regulated by the NaOH solution that concentration is 30%, pH is 7-10 to terminal, water white transparency or thick pale yellow solution, i.e. styrene-maleic anhydride copolymer solution is obtained after 3-5 hour;
(3) preparation of modified melamine resin solution
By weight 70-90 part modified melamine resin and 30-50 part deionized water are stirred in beaker miscible after, obtain modified melamine resin solution, for subsequent use;
(4) preparation of modified melamine resin essence microcapsule emulsion
By weight the styrene-maleic anhydride copolymer solution of preparation in 20-40 part step (2), 20-40 part deionized water, 10-30 part essence, 1-5 part non-ionic surfactant OP-10,1-5 part sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification by high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, pH to 5-7 is regulated with glacial acetic acid solution, and the modified melamine resin solution of preparation in adding 6-18 part step (3) by weight, again regulate pH to 3-5 with glacial acetic acid solution, be warming up to 60-70 DEG C under agitation, solidification 0.5-1.5 hour, Temperature fall, ageing 1-3 hour, then by the NaOH solution that concentration is 30%, pH is adjusted to neutrality, obtain modified melamine resin essence microcapsule emulsion;
(5) preparation of modified melamine resin essence microcapsule finishing agent
To get in 5-10 part step (4) obtained modified melamine resin essence microcapsule emulsion by weight, 1-3 part bleeding agent, 1-3 part bonding agent, 1-3 part softening agent stir fully mixing in beaker, obtain modified melamine resin essence microcapsule finishing agent.Described bleeding agent is bleeding agent AEO JFC, and bonding agent is polyacrylate, aqueous polyurethane, and softening agent is NON IONIC SOFTNER and anionic softener.
The application process of modified melamine resin essence microcapsule finishing agent of the present invention is: get 1-5 part modified melamine resin essence microcapsule finishing agent by weight and be placed in beaker, and be mixed to form finish solution with 95-99 part water.Fabric is placed in finish solution, flood 10-20 minute at temperature is 40-60 DEG C after, taking-up fabric dries, obtain the band liquid fabric that liquid carrying rate (i.e. finish solution content) is 70-90%, at temperature is 40 DEG C, band liquid fabric is baked 30min, finally the fabric after baking is dried naturally, obtain finish fabric.Described fabric is bafta.
Embodiment:
Embodiment 1
By weight 20 parts of styrene, 20 parts of maleic anhydrides, 100 parts of acetone and 0.2 part of initator benzoyl peroxide BPO are put into four-hole bottle.Nitrogen bubble 15 minutes, is warming up to raw material under agitation and all dissolves.After 3 hours 70 DEG C of conditioned responses, use alcohol settling product, obtain White Flocculus, after being taken out drying, grinding, obtain styrene-maleic anhydride copolymer powder.
In four-hole bottle, add 5 parts of styrene-maleic anhydride copolymer powder and 95 parts of deionized waters by weight, be heated to 60 DEG C under agitation, then regulate pH to 10 by the NaOH solution of concentration 30%.React and obtain styrene-maleic anhydride copolymer solution after 3 hours.
Get 20 parts of styrene-maleic anhydride copolymer solution by weight, 40 parts of water, 15 parts of essence, 5 parts of non-ionic surfactant OP-10s, 1 part of sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 5000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, regulate pH to 5 with glacial acetic acid solution.Add 6 parts by weight by 70 parts low methyl-etherified melamine resins and 50 parts of miscible modified melamine resin solution obtained of deionized water, and again regulate pH to 3 with glacial acetic acid solution.Solidification is stirred 1 hour, Temperature fall, ageing 2 hours under 60 DEG C of conditions.Being adjusted to neutrality by the NaOH solution that concentration is 30% again makes it stablize, and obtains modified melamine resin essence microcapsule emulsion.The solid content 31.06% of this microcapsule emulsion, essence encapsulation ratio 91.25%.
Finally, by weight 5 parts of obtained modified melamine resin essence microcapsule emulsions, 1 part of AEO JFC bleeding agent, 3 parts of polyacrylate bonding agents, 1 part of NON IONIC SOFTNER are uniformly mixed in beaker, obtained modified melamine resin essence microcapsule finishing agent emulsion.In its application process, in beaker, get 5 parts of modified melamine resin essence microcapsule finishing agents by weight, 95 parts of water are mixed to get finish solution, fabric is put into finish solution, flood 20 minutes at 60 DEG C, then fabric is taken out and dry, obtain the band liquid fabric that liquid carrying rate (i.e. finish solution content) is 90%, band liquid fabric is baked 30min at 40 DEG C in an oven, finally the fabric after baking is dried naturally, obtain finish fabric.
The finish fabric obtained leaves standstill lasting can reach 6 months, and after washing 3 times, fragrance there is no significant change.Leave standstill fragrance remaining time compared with similar products and improve 30%, and possess the wash durability not available for other products.
Embodiment 2
By weight 30 parts of styrene, 30 parts of maleic anhydrides, 120 parts of acetone and 0.2 part of initator benzoyl peroxide BPO are put into four-hole bottle.Nitrogen bubble 15 minutes, is warming up to raw material under agitation and all dissolves.After 3 hours 70 DEG C of conditioned responses, use alcohol settling product, obtain White Flocculus, after being taken out drying, grinding, obtain styrene-maleic anhydride copolymer powder.
In four-hole bottle, add 10 parts of styrene-maleic anhydride copolymer powder and 90 parts of deionized waters by weight, be heated to 70 DEG C under agitation, then regulate pH to 9 by the NaOH solution of concentration 30%.React and obtain styrene-maleic anhydride copolymer solution after 4 hours.
Get 40 parts of styrene-maleic anhydride copolymer solution by weight, 30 parts of water, 25 parts of essence, 1 part of non-ionic surfactant OP-10,1 part of sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 10000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, regulate pH to 5 with glacial acetic acid solution.Add 18 parts by weight by 90 parts low methyl-etherified melamine resins and 30 parts of miscible modified melamine resin solution obtained of deionized water, and again regulate pH to 4 with glacial acetic acid solution.Solidification is stirred 1 hour, Temperature fall, ageing 2 hours under 60 DEG C of conditions.Being adjusted to neutrality by the NaOH solution that concentration is 30% again makes it stablize, and obtains modified melamine resin essence microcapsule emulsion.The solid content 32.45% of this microcapsule emulsion, essence encapsulation ratio 92.63%.
Finally, by weight 5 parts of obtained modified melamine resin essence microcapsule emulsions, 1 part of AEO JFC bleeding agent, 3 parts of aqueous polyurethane bonding agents, 1 part of NON IONIC SOFTNER are uniformly mixed in beaker, obtained modified melamine resin essence microcapsule finishing agent emulsion.In its application process, in beaker, get 1 part of modified melamine resin essence microcapsule finishing agent by weight, 97 parts of water are mixed to get finish solution, fabric is put into finish solution, flood 10 minutes at 40 DEG C, then fabric is taken out and dry, obtain the band liquid fabric that liquid carrying rate (i.e. finish solution content) is 70%, band liquid fabric is baked 30min at 40 DEG C in an oven, finally the fabric after baking is dried naturally, obtain finish fabric.
The finish fabric obtained leaves standstill lasting can reach 6 months, and after washing 3 times, fragrance there is no significant change.Leave standstill fragrance remaining time compared with similar products and improve 30%, and possess the wash durability not available for other products.
Embodiment 3
By weight 25 parts of styrene, 25 parts of maleic anhydrides, 120 parts of acetone and 0.2 part of initator benzoyl peroxide BPO are put into four-hole bottle.Nitrogen bubble 15 minutes, is warming up to raw material under agitation and all dissolves.After 3 hours 70 DEG C of conditioned responses, use alcohol settling product, obtain White Flocculus, after being taken out drying, grinding, obtain styrene-maleic anhydride copolymer powder.
In four-hole bottle, add 10 parts of styrene-maleic anhydride copolymer powder and 90 parts of deionized waters by weight, be heated to 70 DEG C under agitation, then regulate pH to 9 by the NaOH solution of concentration 30%.React and obtain styrene-maleic anhydride copolymer solution after 5 hours.
Get 30 parts of styrene-maleic anhydride copolymer solution by weight, 40 parts of water, 20 parts of essence, 3 parts of non-ionic surfactant OP-10s, 1 part of sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, regulate pH to 4 with glacial acetic acid solution.Add 12 parts by weight by 90 parts low methyl-etherified melamine resins and 30 parts of miscible modified melamine resin solution obtained of deionized water, and again regulate pH to 4 with glacial acetic acid solution.Solidification is stirred 1 hour, Temperature fall, ageing 2 hours under 60 DEG C of conditions.Being adjusted to neutrality by the NaOH solution that concentration is 30% again makes it stablize, and obtains modified melamine resin essence microcapsule emulsion.The solid content 30.87% of this microcapsule emulsion, essence encapsulation ratio 90.51%.
Finally, by weight 5 parts of obtained modified melamine resin essence microcapsule emulsions, 1 part of AEO JFC bleeding agent, 3 parts of polyacrylate bonding agents, 1 part of anionic softener are uniformly mixed in beaker, obtained modified melamine resin essence microcapsule finishing agent emulsion.In its application process, in beaker, get 3 parts of modified melamine resin essence microcapsule finishing agents by weight, 99 parts of water are mixed to get finish solution, fabric is put into finish solution, flood 15 minutes at 50 DEG C, then fabric is taken out and dry, obtain the band liquid fabric that liquid carrying rate (i.e. finish solution content) is 85%, band liquid fabric is baked 30min at 40 DEG C in an oven, finally the fabric after baking is dried naturally, obtain finish fabric.
The finish fabric obtained leaves standstill lasting can reach 6 months, and after washing 3 times, fragrance there is no significant change.Leave standstill fragrance remaining time compared with similar products and improve 30%, and possess the wash durability not available for other products.
Claims (2)
1. a preparation for modified melamine resin essence microcapsule finishing agent, this preparation comprises the following steps:
(1) preparation of styrene-maleic anhydride copolymer powder
By weight 20-30 part styrene, 20-30 part maleic anhydride, 100-120 part acetone and 0.2-0.5 part benzoyl peroxide initator are put into four-hole bottle, by nitrogen bubble 5-15 minute, slowly heat up under agitation, 50-70 DEG C is maintained the temperature at after raw material all dissolves, reaction 1-3 hour, add 10-15 part ethanol, obtain White Flocculus, and after dry, grinding styrene-maleic anhydride copolymer powder;
(2) preparation of styrene-maleic anhydride copolymer solution
Styrene-maleic anhydride copolymer powder and 85-95 part deionized water of preparation in 5-15 part step (1) is added by weight in four-hole bottle, be heated temperature under agitation at 60-80 DEG C, pH is regulated by the NaOH solution that concentration is 30%, pH is 7-10 to terminal, water white transparency or thick pale yellow solution, i.e. styrene-maleic anhydride copolymer solution is obtained after 3-5 hour;
(3) preparation of modified melamine resin solution
By weight 70-90 part modified melamine resin and 30-50 part deionized water are stirred in beaker miscible after, obtain modified melamine resin solution, described modified melamine resin is by carbinol-modified low etherificate melamine resin, for subsequent use;
(4) preparation of modified melamine resin essence microcapsule emulsion
By weight the styrene-maleic anhydride copolymer solution of preparation in 20-40 part step (2), 20-40 part deionized water, 10-30 part essence, 1-5 part non-ionic surfactant OP-10,1-5 part sodium metnylene bis-naphthalene sulfonate NNO are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification by high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, pH to 5-7 is regulated with glacial acetic acid solution, and the low etherificate melamine resin of preparation in adding 6-18 part step (3) by weight, again regulate pH to 3-5 with glacial acetic acid solution, be warming up to 60-70 DEG C under agitation, solidification 0.5-1.5 hour, Temperature fall, ageing 1-3 hour, then by the NaOH solution that concentration is 30%, pH is adjusted to neutrality, obtain low etherificate melamine resin essence microcapsule emulsion;
(5) preparation of modified melamine resin essence microcapsule finishing agent
To get in 5-10 part step (4) obtained low etherificate melamine resin essence microcapsule emulsion by weight, 1-3 part bleeding agent, 1-3 part bonding agent, 1-3 part softening agent stir and fully mix in beaker, obtained modified melamine resin essence microcapsule finishing agent, described bleeding agent is bleeding agent AEO JFC, bonding agent is polyacrylate, aqueous polyurethane, and softening agent is NON IONIC SOFTNER and anionic softener.
2. the application process of modified melamine resin essence microcapsule finishing agent according to claim 1, the method gets 1-5 part modified melamine resin essence microcapsule finishing agent to be by weight placed in beaker, and be mixed to form finish solution with 95-99 part water, bafta is placed in finish solution, flood 10-20 minute at temperature is 40-60 DEG C after, taking-up fabric dries, obtain the band liquid bafta that liquid carrying rate is 70-90%, at temperature is 40 DEG C, band liquid bafta is baked 30min, finally the fabric after baking is dried naturally, obtain finishing of cotton textiles.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310165451.6A CN103233368B (en) | 2013-05-08 | 2013-05-08 | Preparation and application of modified melamine resin essence microcapsule finishing agent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310165451.6A CN103233368B (en) | 2013-05-08 | 2013-05-08 | Preparation and application of modified melamine resin essence microcapsule finishing agent |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103233368A CN103233368A (en) | 2013-08-07 |
CN103233368B true CN103233368B (en) | 2015-03-04 |
Family
ID=48881432
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310165451.6A Expired - Fee Related CN103233368B (en) | 2013-05-08 | 2013-05-08 | Preparation and application of modified melamine resin essence microcapsule finishing agent |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103233368B (en) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103741496B (en) * | 2013-12-27 | 2016-04-20 | 天津城建大学 | The preparation method of long-acting height is affine essence microcapsule softener and application |
CN105419945B (en) * | 2015-12-29 | 2020-07-03 | 唐山师范学院 | Essence microcapsule and preparation method thereof |
CN105780504A (en) * | 2016-05-19 | 2016-07-20 | 广东妮可儿服饰有限公司 | Manufacture method of cotton series healthy pajamas with sleep-promoting function |
CN106758267A (en) * | 2016-12-23 | 2017-05-31 | 句容市申兔工艺针织厂 | A kind of finishing technique of function of driving mosquitoes fabric |
CN108004788A (en) * | 2017-12-20 | 2018-05-08 | 贺州宝兴新材料有限公司 | A kind of preparation method of modified melamine resin essence microcapsule finishing agent |
CN107904929A (en) * | 2017-12-20 | 2018-04-13 | 贺州宝兴新材料有限公司 | A kind of modified melamine resin essence microcapsule preparation method |
CN107998999A (en) * | 2017-12-21 | 2018-05-08 | 贺州宝兴新材料有限公司 | A kind of technique for preparing melamine resin essence microcapsule |
CN108085995A (en) * | 2017-12-21 | 2018-05-29 | 贺州宝兴新材料有限公司 | A kind of technique for preparing melamine resin finishing agent |
CN108097185A (en) * | 2017-12-21 | 2018-06-01 | 贺州宝兴新材料有限公司 | A kind of method for preparing melamine resin essence microcapsule finishing agent |
CN115430371A (en) * | 2022-06-29 | 2022-12-06 | 上海宾佑新材料科技有限公司 | Meyer sedge essential oil microcapsule, preparation method and application |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1030510C (en) * | 1990-12-07 | 1995-12-13 | 陈玉琦 | Productive method and usage of Chinese-medicinal health-care cloth |
CN101099928A (en) * | 2006-07-07 | 2008-01-09 | 崇裕科技股份有限公司 | Method for preparing microcapsule more than three-layer shell material coating |
CN1966847A (en) * | 2006-11-24 | 2007-05-23 | 华明浩 | Method for preparing inorganic clad nano silver-supported antibacterial composite polyurethane microcapsule aromatic fabrics |
CN102127864B (en) * | 2010-12-24 | 2012-07-04 | 天津市双马香精香料新技术有限公司 | Preparation method and application of aromatic microcapsule finishing agent with double-layer wall materials |
CN102720070A (en) * | 2012-07-03 | 2012-10-10 | 东华大学 | Esthetic carpet fragrance microcapsule finishing agent and preparation thereof |
-
2013
- 2013-05-08 CN CN201310165451.6A patent/CN103233368B/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CN103233368A (en) | 2013-08-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103233368B (en) | Preparation and application of modified melamine resin essence microcapsule finishing agent | |
CN103230766B (en) | Preparation and application of self-adhesive double-wall essence microcapsule | |
EP1792004B1 (en) | Binder systems for microcapsule treatments to fibers, fabrics and garments | |
Nelson | Application of microencapsulation in textiles | |
WO1991001801A1 (en) | Microcapsule, treatment liquid containing microcapsules, and textile structure having microcapsules stuck thereto | |
CN102958497A (en) | Process for producing microcapsules | |
CN102586017B (en) | Essence microcapsule with softening function and preparation method of essence microcapsule | |
CN109957972A (en) | The method of microcapsules and its arrangement into textile fabric based on plants essential oil | |
CN107724094A (en) | A kind of microcapsules gauze kerchief finishing agent of antiultraviolet and preparation method thereof | |
KR20090025095A (en) | Fabric having aromatic microcapsule, mixure and method of manufacturing thereof | |
CN103741496B (en) | The preparation method of long-acting height is affine essence microcapsule softener and application | |
CN107998999A (en) | A kind of technique for preparing melamine resin essence microcapsule | |
CN108097185A (en) | A kind of method for preparing melamine resin essence microcapsule finishing agent | |
CN107858836A (en) | A kind of osmanthus flower fragrance microcapsules textile finish and its preparation application method | |
CN108085995A (en) | A kind of technique for preparing melamine resin finishing agent | |
CN103276591A (en) | Preparation method of antiallergic aroma type woolen sweater | |
CN108004788A (en) | A kind of preparation method of modified melamine resin essence microcapsule finishing agent | |
CN104988741A (en) | Fragrance easy-care treating method of cotton shirt | |
CN107904929A (en) | A kind of modified melamine resin essence microcapsule preparation method | |
CN107724095A (en) | A kind of microcapsules necktie finishing agent and preparation method thereof | |
CN114933939A (en) | Essence microcapsule with biodegradable wall material and application thereof in liquid detergent | |
CN108097183A (en) | A kind of melamine resin essence microcapsule preparation method | |
CN108043337A (en) | A kind of self bonding double-walled essence microcapsule preparation method | |
CN108097184A (en) | A kind of double-walled essence microcapsule preparation method | |
KR100489318B1 (en) | Fabric softner composition containing microcapsulated vitamin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150304 |
|
CF01 | Termination of patent right due to non-payment of annual fee |