CN108716141A - A kind of high resistance to settling, the pigment Nano capsule coating of high color depth, preparation method and application - Google Patents
A kind of high resistance to settling, the pigment Nano capsule coating of high color depth, preparation method and application Download PDFInfo
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- CN108716141A CN108716141A CN201810387621.8A CN201810387621A CN108716141A CN 108716141 A CN108716141 A CN 108716141A CN 201810387621 A CN201810387621 A CN 201810387621A CN 108716141 A CN108716141 A CN 108716141A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
- C09D133/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/45—Anti-settling agents
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1818—C13or longer chain (meth)acrylate, e.g. stearyl (meth)acrylate
Abstract
The invention discloses a kind of high resistance to settling, the pigment Nano capsule coating of high color depth, have good resistance to settling energy, and the invention also discloses the preparation methods of the pigment Nano capsule coating, including：A large amount of low-density, inertia, volatilizable decamethylcyclopentaandoxane or octamethylcy-clotetrasiloxane are added in acrylic ester monomer, and nanoencapsulation processing is carried out to organic pigment by mini-emulsion polymerization, the Nano capsule coating of stable homogeneous is made.This method preparation process is environmentally protective, raw materials used to be easy to get, simple for process, and pigment coating efficiency is high.The present invention also provides the pigment Nano capsule coating is applied to textile coating stamp, the deep-colour fabric of value >=25 K/S, the gas permeability retention rate of PRINTED FABRIC are obtained>70%, stiffness amplification<30%, the crock fastness of resistance to dry and wet >=4 grade, feel subjectivity is graded >=4 grades.
Description
Technical field
The present invention relates to the technical fields of pigment capsule coating in fine chemistry industry, and in particular to high resistance to settling, high color depth
Pigment Nano capsule coating mini-emulsion polymerization in situ prepare and application.
Background technology
Pigment printing is will be to knitting by the adhesive attraction of binder using the principle that binder forms a film in fabric surface
Object does not have compatibility and the adherency of reactive coloring agent particle on the fabric, to obtain the printing technique of required coloring effect.This
Kind coloring principle so that it is wide to the applicability of fabric, can be significantly especially to the coloring of a large amount of blended fabric without selectivity
Simplify coloring processing flow, improve converted products when the percentage of A-class goods, process velocity.
Binder macromolecule can be coated on organic pigment surface in advance, substantially increased by the nanoencapsulation of pigment
Organic pigment dispersibility in water and dispersion stabilization.By the emulsion applications after organic pigment nanoencapsulation in pigment printing
It can substantially reduce the dosage of binder under the premise of ensureing fastness, improve the utilization ratio of binder.
But current organic pigment Nano capsule coating is poor in the prevalence of resistance to settling, it is difficult to the keys such as deep-colour fabric be made
Problem limits its scope of application.Resistance to settling difference be primarily due to the density of most of organic pigment generally 1.3~
2.1g/cm3Between, it is much larger than water, thus the density of pigment capsule is also typically larger than water, naturally tends to be deposited to bottom.
More crucially the Adhering capacity of pigment capsule surface polymer is strong, once collided between pigment capsule, be easy for assembling it is blocking,
" caking " phenomenon occurs, is unfavorable for the stabilization of system.It is directed to problems at present, industrial common solution is that addition is big
The emulsifier and dispersant of amount, but actual conditions show nothing if being added to a large amount of emulsifier and dispersant in lotion
Method keeps not settling for a long time, once and pigment capsule is deposited to container bottom, the polymer of capsule surface will bind to be formed
Irreversible aggregation, seriously affects coating quality.
It is difficult to obtained deep-colour fabric and is primarily due to the pigment capsule prepared using mini-emulsion polymerization in situ, excessive is organic
Pigment can make former pigment/monomer dispersion liquid gelation, can not carry out fine crankshaft polymerization and prepare.Currently, research shows that pigment glue
The mass fraction of organic pigment is difficult and pigment capsule commonly used painting when carrying out pigment printing more than 12% in cyst membrane
Expect that total amount is less, therefore current pigment capsule pigment printing fabric is difficult to ensure color depth again while ensureing feel, fastness
Degree and brightness.
Invention content
In view of the above technical problems, the present invention provides a kind of high resistance to settling, the pigment Nano capsule coating of high color depth,
With good resistance to settling energy, the deep-colour fabric of value >=25 K/S, the gas permeability retention rate of PRINTED FABRIC can be prepared>70%, firmly
Deflection amplification<30%, the crock fastness of resistance to dry and wet >=4 grade, feel subjectivity is graded >=4 grades.
Pigment Nano capsule coating provided by the invention is obtained by miniemulsion preparation method in situ, this method preparation process
Environmentally protective, raw materials used to be easy to get, simple for process, pigment coating efficiency is high.
A kind of high resistance to settling, high color depth pigment Nano capsule coating preparation method, including：
1) octamethylcy-clotetrasiloxane (D4) or decamethylcyclopentaandoxane (D5) and acrylic ester monomer, You Jiyan
Material obtains oil phase mixed liquor, as A phases, wherein the quality of D4 or D5 accounts for the 30~60% of A phase quality after ultrasound is uniform；
The structural formula of the D4 is shown in formula I；The structural formula of D5 is as shown in Formula II：
2) emulsifier is added in aqueous solution until be completely dissolved, and as B phases, the A phases in step 1) are mixed with B,
Ultrasonic homogenation obtains miniemulsion；Miniemulsion is transferred in reaction unit later, is acted in inert gas shielding, initiator
Under, carry out the polymerisation of miniemulsion, obtain high resistance to settling, high color depth pigment Nano capsule coating；
The ultrasonic homogenation temperature is -5~0 DEG C, and ultrasonic time is 10~20min.
Acrylic ester monomer described in step 1) is methyl methacrylate (MMA), octadecyl acrylate (OA), third
Olefin(e) acid butyl ester (BA), ethylene glycol dimethacrylate (EGDMA), hydroxy-ethyl acrylate (HEMA) and glycidyl acrylate
(GMA) mixture.
Its polarity of the selection Main Basiss of acrylic ester monomer and functionality, wherein methyl methacrylate in step 1)
Ester, octadecyl acrylate, butyl acrylate provide main cohesion as main binder monomer；Dimethacrylate
Glycol ester, glycidyl acrylate promote binder crosslinking degree as crosslinking agent；Hydroxy-ethyl acrylate primarily to
Promote the hydrophily of binder.
Organic pigment described in step 1) is C.I. pigment blue 15s, C.I. pigment green 36s, C.I. pigment violet 1s 9, C.I. face
Expect one in red 122, C.I. pigment yellows 191, C.I. pigment yellow 81s, C.I. pigment yellows 1, C.I. pigment yellows 3, carbon black, graphene
Kind is a variety of；The addition of pigment is the 5~12% of A phase quality.
Organic pigment filter cake selection is mainly based upon that lipophile is strong, the good organic pigment with organosilicon compatibility, C.I. face
Material basket 15, C.I. pigment green 36s, C.I. pigment violet 1s 9, C.I. pigment red 122s, C.I. pigment yellows 191, C.I. pigment yellow 81s,
C.I. the organic pigments such as pigment yellow 1, C.I. pigment yellows 3, carbon black, graphene have a relatively stable chemical constitution, surface strong oil-wet,
It is thus good with the compatibility of organosilicon, acrylate monomer.
The currently preferred D4 or D5 dosages of step 1) be A phase quality 30%~60%, D4 and D5 be two kinds of low-density,
Low viscosity, not double bond containing liquid, are not involved in the Raolical polymerizable of vinyl monomer, always with liquid shape in system
Formula is present in inside fine crankshaft drop and final pigment capsule, can effectively reduce the density of pigment capsule, it is prevented to be deposited to
Container bottom.In addition, during pigment capsule emulsion film forming, D4, D5 will gradually volatilize in heated baking process, wherein
Granules of pigments shared by quality proportion will gradually increase, the thickness of glued membrane also can constantly decline, and finally obtain slim, high color
Deep pigment compound cutan.When D4 or D5 dosages are less than 30%, content is too low can not preferably to reduce the close of pigment capsule
Degree, thus the resistance to settling of Nano capsule lotion is bad.And when D4 or D5 dosages are higher than 60%, the density of pigment capsule is down to
Sufficiently low, lotion resistance to settling can be fabulous, but since D4 or D5 dosages are excessively high, acrylate polymer content is too low, pigment
The cohesion of compound cutan is greatly reduced, and causes the crock fastness of resistance to dry and wet of pigment capsule PRINTED FABRIC that can be down to 1 grade.
Preferably, A phases use following weight：
In step 2), the emulsifier is lauryl sodium sulfate (SDS), nonylphenol polyoxyethylene ether (OP-10), first
Base acrylic acid hydroxypropyl azochlorosulfonate acid sodium (HMPS) is compounded and is obtained.Since the surface energy of D4, D5 are relatively low, thus need stronger emulsifying power
Power stablizes the polymerized monomer drop containing a large amount of D4, D5.SDS, HMPS are the stronger two kinds of ionic emulsifying agents of emulsifying capacity,
And OP-10 is common nonionic emulsifier, three kinds of mixing are used in compounding the stable emulsifying ability that can effectively improve B phases.It is excellent
The emulsifier of choosing is the 5~10% of A phases.
In step 2), the initiator is dibenzoyl peroxide or potassium peroxydisulfate, and dosage is the 2~3% of A phases；Institute
The reaction temperature for the mini-emulsion polymerization stated is 60~70 DEG C, and the reaction time is 1~2h.Since D4, D5 in the present invention are in high temperature
Under it is volatile, thus mini-emulsion polymerization temperature of the present invention cannot be excessively high, and the reaction time cannot be too long, otherwise D4, D5
It can largely volatilize, it is difficult to preferably be stored in inside pigment capsule, therefore currently preferred reaction temperature is 63~66 DEG C.Together
When, the dosage of initiator has been properly increased in the time present invention in order to reduce reaction, through being preferably A phase quality 2.3~
2.5%.
In step 2), the inert gas selects the broad scope of inert gas in this field, can be selected nitrogen, argon gas,
One kind in helium etc., from the point of view of cost-effective, preferred nitrogen.
The present invention also provides the pigment Nano capsule coating of the high resistance to settling, high color depth to be printed in textile coating
Application in flower field, specifically includes：
By high resistance to settling, high color depth pigment Nano capsule coating in addition thickener and water, according to practical application need
Paint-printing colour size is made after adjusting viscosity, paint-printing colour size is then used for textile printing using PLATE SCREAM PRINTING technology.
The paint-printing colour size is prepared using the raw material of following parts by weight：
80-90 parts of Nano capsule coating；
1-5 parts of thickener；
10-15 parts of water.
The thickener is anion thickener PTF made of polyacrylate copolymerization, viscosity≤60cps, pH value
For 4-5, solid content is 18~29%.
In the present invention, it is described stir, ultrasound, PLATE SCREAM PRINTING etc. are typical unit during chemical industry and dye printing
Operation can be used existing conventional equipment and realize.
The present invention adds a large amount of low-density, low viscosity, inert in the miniemulsion of convention pigment capsule prepares formula
Organosilicon composition octamethylcy-clotetrasiloxane (D4) or decamethylcyclopentaandoxane (D5), change the density and table of pigment capsule
Surface properties enhance its resistance to settling in water phase.Coating provided by the invention is applied to textile coating stamp, by hot baked
Afterwards, the heated volatilizations of D4 or D5, improve mass fraction and color depth of the pigment in final solid glued membrane, and reduce glue
The thickness of film finally can form well dispersed, ultra-thin, the dark compound adhesive cyst membrane of pigment in fiber surface, and then be taken into account
The PRINTED FABRIC of fastness, feel, gas permeability, color depth, the color depth (K/S values) of gained PRINTED FABRIC more than 25, PRINTED FABRIC it is saturating
Gas retention rate>70%, stiffness amplification<30%, the crock fastness of resistance to dry and wet >=4 grade.
Compared with prior art, the present invention has the advantages that：
(1) present invention is on the basis of to organic pigment nanoencapsulation, and low-density, low viscosity, lazy is introduced in capsule
Property organosilicon composition (D4 or D5), change the density of capsule, improve resistance to settling of the pigment capsule in water phase.
(2) new coating provided by the invention is attached to fabric surface applied to textile coating stamp after by hot baked
Nano capsule inside D4, D5 volatilized together with moisture, during volatilization, the thickness of pigment compound cutan will be by
Gradually decline, color gradually deepens.Thus coating of the present invention can get color depth (K/S values) in the case of relatively low amount of pigment
More than 25, the gas permeability retention rate of PRINTED FABRIC>70%, stiffness amplification<30%, the coating of the crock fastness of resistance to dry and wet >=4 grade
PRINTED FABRIC.
(3) high resistance to settling, the pigment Nano capsule dope preparing process of high color depth prepared by the present invention are environmentally protective, institute
It is easy to get with raw material, simple for process, product can be directly used for the production process of existing pigment printing, General Promotion PRINTED FABRIC product
Matter.
Description of the drawings
Fig. 1 be high resistance to settling in the embodiment of the present invention 1~15, high color depth pigment Nano capsule coating breast in situ thin
Liquid polymerization prepares and application flow schematic diagram.
Fig. 2 is the surface SEM figures of Na capsule lotion printed polyester fabric in the embodiment of the present invention 4~5 and comparative example 2,
Middle a is the surface SEM figures of the Na capsule lotion printed polyester fabric of comparative example 2；B is that the Na capsule lotion terylene of embodiment 5 prints
The surface SEM of loom figured schemes；C is the surface SEM figures of the Na capsule lotion printed polyester fabric of embodiment 4.
Fig. 3 is Na capsule emulsion particle diameter comparison diagram in the embodiment of the present invention 1,4,7,8,12 and comparative example 2.
Fig. 4 is the Na capsule lotion transmission electron microscope photo in the embodiment of the present invention 4.
Fig. 5 is the Na capsule lotion transmission electron microscope photo in the embodiment of the present invention 8.
Specific implementation mode
Synthesizing formula composition is shown in Table 1 in each embodiment, comparative example in the specific embodiment of the invention, and emulsifier component is shown in Table
2, corresponding the performance test results are shown in Table 3.
Characterizing method explanation involved in embodiment and comparative example：
1, the settleability test of Nano capsule lotion：
A certain amount of Nano capsule lotion is weighed, its solid content is tested and (is denoted as W1), lotion is in TGL-16G type high speeds later
In 10000rmin in centrifuge-1It is centrifuged under rotating speed, centrifuges 60min, take out supernatant liquid later, measured solid content and (be denoted as
W2)。
Define rate of weight loss W=W2/W1* 100%, resistance to settling energy is assessed with W sizes, W values range is in 0-100%, W
Numerical value is bigger to illustrate that lotion resistance to settling can be better.
2, the measurement of pigment printing effect：
1) chromatic value of PRINTED FABRIC measures
Pigment depth refers to that the color of opaque solid matter gives the intuitive depth preception of people or the concentration of color,
Its size often in by solid matter coloring matter content number, the physical state of coloring matter, the optical property of the surface of solids
The influence of equal various factors, the size of color depth value usually indicate that K/S values are bigger with K/S values, indicate that color is deeper；K/S
It is worth smaller, then it represents that color is more shallow.
Test method measures the K/S values of dyeing sample using Datacolor650 type color measurement and color match instrument, and each sample takes five
A difference colour examining is averaged.
2) test for the colorfastness to rubbing of resistance to dry and wet
The crock fastness of resistance to dry and wet test is with reference to GB/T3920-1997 standards.Sample is 50mm × 200mm, through broadwise each two
Block, standard friction are 50mm × 50mm with cotton.
3) hand feel performance is tested
It closes the fabric that mesh touches after arranging to grade using 5-10 people as a small group, is knitted stamp according to different feels
Object carries out hand feel evaluation, and specific assessment method is：Feel grading is carried out in terms of flexibility, smooth feeling two, is divided into 5 grades, 1 grade most
Difference, fabric feeling is harder, and sliding glutinous sense is poor, and 5 grades preferably, and fabrics feel soft, cunning are glutinous.
4) permeability test
With reference to GB/T5453-1997《The measurement of textile fabric gas permeability》, using Ningbo textile Instrument Factory production
The digital air permeation volume gauge of YG461E types tests the gas permeability of PRINTED FABRIC.
Gas permeability/former cloth gas permeability of gas permeability retention rate %=PRINTED FABRICs.
Embodiment 1~15
The first step：According to the formula of table 1 by the D4 of certain mass or D5 and organic pigment (Pigment), esters of acrylic acid
Monomer (Acr) is stirred, and oil phase mixed liquor is obtained after ultrasound is uniform, as A phases.
Second step：Three kinds of emulsifiers are added in aqueous solution until being completely dissolved, as B phases according to the formula of table 2.
Third walks：A phases are mixed with B, ultrasonic homogenation obtains miniemulsion；Miniemulsion is transferred to reaction dress later
In setting, under nitrogen protection, the effect of initiator dibenzoyl peroxide, carry out mini-emulsion polymerization reaction, obtain high resistance to settling,
The pigment Nano capsule coating of high color depth.
4th step：Take the Nano capsule lotion 20g and 0.5g thickening agent PTFs (anion thickener, viscosity of preparation
40cps~50cps, pH value 4.5, solid content 23%) it is uniformly mixed, add water stirring to be adjusted to certain consistency, fabric is carried out
PLATE SCREAM PRINTING.PRINTED FABRIC preliminary drying 5min in low temperature (60 DEG C) baking oven, is then placed in 120 DEG C of baking ovens and bakes, printed again
Flower finished product.
Mini-emulsion polymerization in situ described in above-described embodiment prepares and application flow schematic diagram is as shown in Figure 1.Embodiment 4
~5 and comparative example 2 in Na capsule lotion printed polyester fabric surface SEM figures as shown in Fig. 2, as shown in Figure 2, with D4 contents
Increase, glued membrane can gradually it is thinning, protrusion can also obviously increase.D4 contents are high in the Na capsule lotion of embodiment 4, carried out with it
Pigment printing finds that the polymer film of PRINTED FABRIC baking rear surface is very thin, fits tightly on fiber surface (in Fig. 2
C figure).This structure can not only ensure that PRINTED FABRIC had good fastness, but also PRINTED FABRIC can be made to possess soft hand
Sense.
In addition, Na capsule emulsion particle diameter comparison diagram is as shown in Figure 3 in embodiment 1,4,7,8,12 and comparative example 2.In embodiment 4
Na capsule lotion transmission electron microscope photo it is as shown in Figure 4；Na capsule lotion transmission electron microscope photo in embodiment 8 is as shown in Figure 5.
Comparative example 1
After being mixed with emulsifier aqueous solution according to the organic pigment quality (10g) in embodiment 4, through zirconium pearl ball milling 3h, obtain
To organic pigment suspension.It is mixed then to suitable commercial polypropylene acid esters binder is added in organic pigment suspension
Uniformly, its resistance to settling energy is tested, takes the thickener of mixed liquor (20g) quality in the same manner as in Example 4 to mix later, modulates
To the print paste with certain viscosity.Warp-wise is carried out to terylene plain cloth to scrape by hand, PRINTED FABRIC is in 60 DEG C of baking ovens
Preliminary drying 5min is then placed in 120 DEG C of baking ovens and bakes, obtains stamp finished product again.
Comparative example 2
The first step：According to the formula of table 1 by the D4 of certain mass or D5 and organic pigment (Pigment), esters of acrylic acid
Monomer (Acr) is stirred, and oil phase mixed liquor is obtained after ultrasound is uniform, as A phases.
Second step：Three kinds of emulsifiers are added in aqueous solution until being completely dissolved, as B phases according to the formula of table 2.
Third walks：A phases are mixed with B, ultrasonic homogenation obtains miniemulsion；Miniemulsion is transferred to reaction dress later
In setting, under nitrogen protection, the effect of initiator dibenzoyl peroxide, carry out mini-emulsion polymerization reaction, obtain high resistance to settling,
The pigment Nano capsule coating of high color depth, tests its resistance to settling energy.
4th step：The Nano capsule lotion (20g) of preparation is taken to be uniformly mixed with appropriate thickener, stirring is adjusted to certain thick
Degree uses PLATE SCREAM PRINTING to terylene plain cloth.PRINTED FABRIC preliminary drying 5min in low temperature (60 DEG C) baking oven, is then placed in again
It is baked in 120 DEG C of baking ovens, obtains stamp finished product.
As shown in Table 3, using the present invention --- high resistance to settling pigment Nano capsule coating carries out textile coating stamp, can
The crock fastness of resistance to dry and wet is obtained to 4-5 grades, the gas permeability retention rate of PRINTED FABRIC reaches as high as 90% or more, color depth height, feel
Soft pigment printing fabric.The polyacrylate face of comparison and the blending type color paste of printing coating and routine of pigment+coating
Expect that capsule pigment printing paste, pigment Nano capsule coating prepared by the present invention have high resistance to settling and stability.
Table 1
Table 2
| Embodiment | SDS/g | OP-10/g | HMPS/g |
| Embodiment 1 | 4 | 1 | 2 |
| Embodiment 2 | 1 | 1 | 5 |
| Embodiment 3 | 1 | 3 | 5 |
| Embodiment 4 | 2 | 3 | 2 |
| Embodiment 5 | 3 | 1 | 2 |
| Embodiment 6 | 3 | 2 | 2 |
| Embodiment 7 | 3 | 1 | 1 |
| Embodiment 8 | 2 | 3 | 2 |
| Embodiment 9 | 2 | 3 | 2 |
| Embodiment 10 | 5 | 2 | 1 |
| Embodiment 11 | 2 | 3 | 2 |
| Embodiment 12 | 2 | 3 | 2 |
| Embodiment 13 | 2 | 4 | 2 |
| Embodiment 14 | 2 | 3 | 2 |
| Embodiment 15 | 4 | 3 | 1 |
| Comparative example 2 | 2 | 3 | 2 |
Table 3
The above content is only the better embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to this hair
Bright limitation.
Claims (10)
1. a kind of preparation method of the pigment Nano capsule coating of high resistance to settling, high color depth, including：
1) D4 or D5, acrylic ester monomer and organic pigment obtain oil phase mixed liquor, as A phases after ultrasound is uniform, wherein
The quality of D4 or D5 accounts for the 30~60% of A phase quality；
The structural formula of the D4 is shown in formula I；
The structural formula of the D5 is as shown in Formula II：
2) emulsifier is added in aqueous solution up to being completely dissolved, and as B phases, the A phases in step 1) is mixed with B, ultrasound
It homogenizes, obtains miniemulsion；Under inert gas shielding, initiator effect, the polymerisation of miniemulsion is carried out, it is heavy to obtain highly resistance
The pigment Nano capsule coating of drop property, high color depth.
2. the preparation method of the pigment Nano capsule coating of high resistance to settling according to claim 1, high color depth, feature
It is, in step 1), the acrylic ester monomer is methyl methacrylate, octadecyl acrylate, butyl acrylate, two
The mixture of methacrylic acid glycol ester, hydroxy-ethyl acrylate and glycidyl acrylate.
3. according to the preparation method of high resistance to settling described in claim 1, the pigment Nano capsule coating of high color depth, feature exists
In in step 1), A phases use following weight：
4. the preparation method of the pigment Nano capsule coating of high resistance to settling according to claim 1, high color depth, feature
It is, in step 2), the emulsifier is lauryl sodium sulfate, nonylphenol polyoxyethylene ether and methacrylic acid hydroxypropyl
Sodium sulfonate is compounded and is obtained；The addition of emulsifier is the 5~10% of A phase quality.
5. the preparation method of the pigment Nano capsule coating of high resistance to settling according to claim 1, high color depth, feature
It is, in step 2), the initiator is dibenzoyl peroxide or potassium peroxydisulfate, and dosage is the 2~3% of A phases.
6. the preparation method of the pigment Nano capsule coating of high resistance to settling according to claim 1, high color depth, feature
It is, in step 2), the reaction temperature of the polymerisation of the miniemulsion is 60~70 DEG C, and the reaction time is 1~2h.
7. the preparation method of the pigment Nano capsule coating of high resistance to settling according to claim 6, high color depth, feature
It is, in step 2), the reaction temperature of the polymerisation of the miniemulsion is 63~66 DEG C.
8. the face with high resistance to settling, high color depth being prepared according to claim 1~7 any one of them preparation method
Expect Nano capsule coating.
9. it is according to claim 8 with high resistance to settling, high color depth pigment Nano capsule coating in textile coating
Application in stamp field.
10. application according to claim 9, which is characterized in that apply required pigment printing paste of fabric, use with
The raw material of lower parts by weight is prepared：
80-90 parts of Nano capsule coating
1-5 parts of thickener
10-15 parts of water；
The thickener is anion thickener PTF made of polyacrylate copolymerization, viscosity≤60cps, pH value 4
~5, solid content is 18~29%.
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| CN112227094A (en) * | 2020-10-11 | 2021-01-15 | 李军 | Coating for textile printing and dyeing and preparation method thereof |
| CN113088142A (en) * | 2021-04-26 | 2021-07-09 | 宇虹颜料股份有限公司 | Method for preparing acrylic paint by directly using organic pigment filter cake |
| CN113308915A (en) * | 2021-05-17 | 2021-08-27 | 英德科迪颜料技术有限公司 | Printing paste and preparation method thereof |
| CN113584904A (en) * | 2021-08-23 | 2021-11-02 | 浙江理工大学 | Preparation method of pigment printed fabric |
| EP4011922A4 (en) * | 2019-08-05 | 2023-09-06 | Nippon Shokubai Co., Ltd. | Emulsion particle-containing aqueous dispersion |
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