CN105944634A - Preparation method of color composite microspheres with high reactive dye adsorption capacity - Google Patents
Preparation method of color composite microspheres with high reactive dye adsorption capacity Download PDFInfo
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- CN105944634A CN105944634A CN201610304132.2A CN201610304132A CN105944634A CN 105944634 A CN105944634 A CN 105944634A CN 201610304132 A CN201610304132 A CN 201610304132A CN 105944634 A CN105944634 A CN 105944634A
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- dye
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- microsphere
- complex microsphere
- dispersion liquid
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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
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Coloring (AREA)
Abstract
The invention relates to a preparation method of color composite microspheres with high reactive dye adsorption capacity and belongs to the field of functional polymer materials. The color composite microspheres have the advantages of large specific surface area, bright color, high light stability and the like and has wide application prospect in the fields of ink-jet printing, textile printing and dyeing, photonic crystals and the like, however, the dye content of the color composite microspheres directly affects the effects of following ink-jet printing, textile printing and dyeing and the like. According to the preparation method of the color composite microspheres with high reactive dye adsorption capacity, cationic polymer microspheres carrying large quantities of positive charges on the surfaces are prepared firstly, then a reactive dye is used for dyeing, and large quantities of dye molecules are adsorbed on the surfaces of the polymer microspheres by changing the use quantity of the dye in the cationic polymer microspheres and the stirring speed in a dyeing process. The color composite microspheres prepared with the method have the advantages of uniform particle size distribution and high dye adsorption capacity.
Description
(1) technical field:
The present invention relates to the preparation method of a kind of high activity dye adsorption amount colour complex microsphere, belong to
In functional high polymer material field.
(2) background technology:
The chromogen bonded polymer complex microsphere of combination dye or pigment has that specific surface area is big, color is fresh
The advantages such as gorgeous, light fastness stability is good, inkjet printing, textile printing and dyeing, biomarker and detection,
The fields such as drug release, clinical diagnosis and photonic crystal are with a wide range of applications.But,
The size of dye content in chromogen bonded polymer nanosphere, directly affects subsequent i alphakjet and prints, weaves
The effect of printing and dyeing etc..Therefore, prepare that to have the colored complex microsphere of high dye content be to realize
The key of its application.
CN200610118671.3 discloses the preparation side of a kind of nano-coloring material aqueous dispersions
Method, utilizes the mini-emulsion polymerization improved reaction that hydrophobic dye is fixed on cross linked polymer nanometer
In microsphere, obtain prepolymer seeds, followed by involucrum polymerization technique at the surface of the seed structure
Build modification, the cross linked polymer shell of protectiveness, finally obtain nano-coloring material aqueous dispersions.
CN200710119034.2 discloses synthesis and the application thereof of a kind of color micro-sphere for electronic paper,
Use polysulfonate acid stain to having the ion-type of strong colouring power and having surface activity
Polymer microsphere dye, prepare color micro-sphere.CN201310505120.2 discloses
A kind of color toner using mini-emulsion polymerization to prepare and method thereof, utilize resin-coating pigment,
The nucleocapsid composite emulsion particle of wax and electric charge agent, the method system being then combined by electrolyte cohesion
Obtain color toner.The most all patents, employ emulsifying agent in preparation process, depositing of emulsifying agent
The performance of emulsion can affected, and removing difficulty, hardly result in pure product.
CN201210199843.X discloses a kind of color polyacrylate polymer microsphere
Preparation method, first this method synthesizes the Functional dye with double bond functional group, then with this type of
Dyestuff, acrylic ester monomer, dispersion stabilizer and initiator are raw material, preparation coloured silk in alcohol
Color polyacrylate polymer microsphere.CN201110034028.3 discloses a kind of colored breast
The preparation method of glue granule, by Latex Particles suspension and fluorescein, rhodamine series dyes,
One or more in coumarine dye, fluorine boron class dyestuff, side's type dye or cyanine class dyestuff
Mixing, during dye molecule inlays latex particle upon inflation after heating, then removes particle surface
Dye molecule, obtain colored latex particles.CN201310096951.9 discloses colored two
The preparation method of silicon oxide microsphere, organic dyestuff is connected to two by chemical bond by silane coupler
On silicon oxide ball, controlled the particle diameter of microsphere by the ratio of water and surfactant, obtain colour
Silicon dioxide microsphere.These patents, in preparation process, method therefor is complicated, time-consumingly.
The present invention is first with reactive dyestuff molecule with cationic polymer microsphere surface institute band just
Electrostatic force between electric charge makes the dye adsorption surface at polymer microballoon, follow-up relies on again
Active force between dye molecule makes dyestuff adsorb further at microsphere surface, prepares high adsorption capacity color
Color polymer composite microsphere.
(3) summary of the invention:
It is an object of the invention on the premise of the even particle size distribution controlling complex microsphere, it is provided that
The preparation method of a kind of high activity dye adsorption amount colour complex microsphere, improves this dispersion liquid dye
Color, the color depth of stamp.
Technical scheme: the preparation of a kind of high activity dye adsorption amount colour complex microsphere
Method, it is characterised in that its concrete preparation process is as follows:
(1) prepared polymer Nano microsphere dispersion liquid: preparing solid content with distilled water is 1.0g/L
~the Polystyrene-acrylate cationoid Nano microsphere dispersion liquid of 10.0g/L, and with ultrasonic
Ripple disperses;
(2) preparation dye liquor: preparing dye strength with redistilled water is 0.1g/L~5.0g/L
Reactive dye dye liquor;
(3) the colored complex microsphere of preparation: be warming up to certain temperature, add in the reactor
The reactive dye solution that a certain amount of configuration is good, under agitation adds a certain amount of scattered cation
Polymer nanocomposite ball dispersion liquid, the mass percent of cationic polymer nanosphere is by dyestuff
15%~75%, the pH value of regulation mixed liquor, to 4.0~6.0, starts timing, and reaction is certain
Time, it is cooled to room temperature discharging, even particle size distribution, high the answering of dye adsorption amount can be obtained
Close microsphere dispersion liquid.
Polymer microballoon of the present invention refers to the surface styrene-the third with quaternary ammonium salt group
Olefin(e) acid lipin polymer microsphere.Such as polystyrene-ethyl acrylate-methylacryoyloxyethyl three
Ammonio methacrylate microsphere, Polyphenylethylene-butyl acrylate-methylacryoyloxyethyl trimethyl chlorine
Change ammonium microsphere, polystyrene-ethyl acrylate-to vinylbenzyltrimethyl ammonium chloride microsphere,
Polyphenylethylene-butyl acrylate-to vinylbenzyltrimethyl ammonium chloride microsphere etc..
Reactive dye of the present invention refer in molecular structure containing anionic groups such as sulfonic groups
Reactive dye, such as active red 1,6,195, reactive orange 4,5,95, reactive yellow 1,2,
174, active blue 19,49,81, reactive violet 4,5,46, reactive black 5,45 etc..
The beneficial effects of the present invention is: (1) preparation method is simple, gained colour complex microsphere
Pure product can be obtained by saltouing, be centrifuged, washing.(2) can be dyeed by regulation
The mixing speed of process prepares even particle size distribution and the high chromogen bonded polymer of dye adsorption amount is multiple
Close microsphere.(3) can be by adjusting the dye molecule dyeing concentration to cationic polymer microsphere
Prepare the complex microsphere of stable chemical nature.
(4) accompanying drawing explanation:
Fig. 1 is chromogen bonded polymer complex microsphere transmission electron microscope photo prepared by the embodiment of the present invention,
Amplification is 50,000 times.
(5) detailed description of the invention:
Embodiment 1
Set reaction temperature as 30 DEG C, regulate the mechanical agitation of digital display agitator as required
(200rpm, 300rpm, 400rpm, 500rpm, 600rpm, 700rpm, 800rpm),
By the Polystyrene-acrylate cationoid nanosphere dispersion liquid that 10mL concentration is 1.0g/L
It is added drop-wise in reactive blue 49 dye liquor that 15mL concentration is 0.1g/L that (dyestuff is to cationic polymerization
The mass percent of thing nanosphere is 15%), the pH=5 of regulation mixed liquor, dye 2 hours,
Obtain colored complex microsphere dispersion liquid.
Embodiment 2
Set reaction temperature as 30 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
The Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 1.0g/L is added to 15mL and lives
Property blue 49 dye liquors in (dyestuff is 15% to the mass percent of cationic polymer nanosphere,
24%, 36%, 43.5%, 51.0%, 60%, 75%), the pH=5 of regulation mixed liquor, dye
Color 2 hours, obtains colored complex microsphere dispersion liquid.
Embodiment 3
Set reaction temperature as 30 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
It is dense that the Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 1.0g/L is added to 15mL
Degree is the (dyestuff quality to cationic polymer nanosphere in reactive blue 49 dye liquor of 0.34g/L
Percentage ratio is 51.0%), the pH=4~6 of regulation mixed liquor, dyes 2 hours, obtains colour
Complex microsphere dispersion liquid.
Embodiment 4
Set reaction temperature as 30 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
It is dense that the Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 1.0g/L is added to 15mL
Degree is the (dyestuff quality to cationic polymer nanosphere in reactive blue 49 dye liquor of 0.34g/L
Percentage ratio is 51.0%), the pH=5 of regulation mixed liquor, dyes 0.5~3 hour, obtains colour
Complex microsphere dispersion liquid.
Embodiment 5
Set reaction temperature as 20~60 DEG C, under 500rpm mechanical agitation, 10mL is dense
Degree is added to 15m for the Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 1.0g/L
Concentration is in reactive blue 49 dye liquor of 0.34g/L, and the pH=5 of regulation mixed liquor, dyeing 2 is little
Time, obtain colored complex microsphere dispersion liquid.
Embodiment 6
Set reaction temperature as 25 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
The Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 10.0g/L is added to 15m concentration
For (the dyestuff quality hundred to cationic polymer nanosphere in reactive blue 49 dye liquor of 1.0g/L
Proportion by subtraction is 15.0%), the pH=5 of regulation mixed liquor, dyes 2 hours, obtains colored compound micro-
Ball dispersion liquid.
Embodiment 7
Set reaction temperature as 25 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
The Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 10.0g/L is added to 15m concentration
For (the dyestuff quality hundred to cationic polymer nanosphere in reactive blue 49 dye liquor of 3.4g/L
Proportion by subtraction is 51.0%), the pH=5 of regulation mixed liquor, dyes 2 hours, obtains colored compound micro-
Ball dispersion liquid.
Embodiment 8
Set reaction temperature as 25 DEG C, under 500rpm mechanical agitation, by 10mL concentration be
The Polystyrene-acrylate cationoid nanosphere dispersant liquid drop of 10.0g/L is added to 15m concentration
For (the dyestuff quality hundred to cationic polymer nanosphere in reactive blue 49 dye liquor of 5.0g/L
Proportion by subtraction is 75.0%), the pH=5 of regulation mixed liquor, dyes 2 hours, obtains colored compound micro-
Ball dispersion liquid.
The performance of the complex microsphere of preparation in table 1 embodiment
The preparation method that the present invention provides is can be seen that by table 1, the uniform particle sizes of complex microsphere, adopts
Being measured complex microsphere with laser nano particle size analyzer, the polydispersity index of complex microsphere can
Good with explanation granule monodispersity, use on the complex microsphere of equilibrium dialysis mensuration dye adsorption
Amount is big.Fig. 1 can also illustrate that complex microsphere uniform particle diameter prepared by the present invention, monodispersity are good.
Claims (5)
1. a preparation method for high activity dye adsorption amount colour complex microsphere, its feature exists
In, the concrete operation step of the method is as follows:
(1) prepared polymer Nano microsphere dispersion liquid: preparing solid content with distilled water is 1.0g/L
~the Polystyrene-acrylate cationoid Nano microsphere dispersion liquid of 10.0g/L, and with ultrasonic
Ripple disperses;
(2) preparation dye liquor: preparing dye strength with redistilled water is 0.1g/L~5.0g/L
Reactive dye dye liquor;
(3) the colored complex microsphere of preparation: be warming up to certain temperature, add in the reactor
The reactive dye solution that a certain amount of configuration is good, under agitation adds a certain amount of scattered cation
Polymer nanocomposite ball dispersion liquid, the mass percent of cationic polymer nanosphere is by dyestuff
15%~75%, the pH value of regulation mixed liquor, to 4.0~6.0, starts timing, and reaction is certain
Time, it is cooled to room temperature discharging, even particle size distribution, high the answering of dye adsorption amount can be obtained
Close microsphere dispersion liquid.
A kind of high activity dye adsorption amount colour complex microsphere the most according to claim 1
Preparation method, it is characterised in that the reaction temperature set as 20~60 DEG C, set reaction
Time is 0.5~3 hour, and the mixing speed set is as 200~800rpm.
A kind of high activity dye adsorption amount colour complex microsphere the most according to claim 1
Preparation method, it is characterised in that polymer microballoon dispersion liquid used is polystyrene-acrylic acid
Esters Cationic nanospheres dispersion liquid.
A kind of high activity dye adsorption amount colour complex microsphere the most according to claim 1
Preparation method, it is characterised in that dyestuff used is with sulfonic group, in the solution with anion
The reactive dye that form exists.
A kind of high activity dye adsorption amount colour complex microsphere the most according to claim 1
Preparation method, it is characterised in that dyeing terminate after, with sodium chloride solution to complex microsphere disperse
Liquid processes, after centrifugal and sodium chloride solution wash, by precipitation distilled water wash,
Last drying can get pure colored complex microsphere powder.
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106590028A (en) * | 2016-11-24 | 2017-04-26 | 华南理工大学 | Polydopamine-based high-saturation-degree structural color pigment and preparation method thereof |
CN107486112A (en) * | 2017-08-08 | 2017-12-19 | 浙江工商大学 | A kind of preparation method of the single dispersing colour silicon dioxide nanosphere of nondiscoloration |
CN108442149A (en) * | 2018-04-28 | 2018-08-24 | 天津工业大学 | A kind of dyeing cycle method of reactive dye color micro-sphere to fabric |
CN109667170A (en) * | 2018-12-29 | 2019-04-23 | 苏州恒瑞迦俐生生物医药科技有限公司 | A kind of coloring process of polymer microsphere |
CN110006886A (en) * | 2019-04-24 | 2019-07-12 | 江苏大学 | A kind of nanosizing color sensitive sensor and its method for differentiating wheat moulding ability |
CN111206440A (en) * | 2020-03-12 | 2020-05-29 | 蚌埠学院 | Preparation method of color nanospheres with uniform particle size |
CN113861737A (en) * | 2021-09-08 | 2021-12-31 | 浙江天画家居用品有限公司 | Environment-friendly antibacterial finger painting pigment containing nano-silver modified silicon dioxide colored composite microspheres |
CN114516931A (en) * | 2022-02-25 | 2022-05-20 | 苏州仁端生物医药科技有限公司 | Preparation method of nanoscale colored microspheres based on electrostatic effect |
CN114775306A (en) * | 2022-04-12 | 2022-07-22 | 天津工业大学 | Preparation method of polyethyleneimine composite dye nanospheres |
CN115193414A (en) * | 2021-04-09 | 2022-10-18 | 中国科学院理化技术研究所 | Application of heterogeneous porous polymer microspheres in dye adsorption |
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Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106590028A (en) * | 2016-11-24 | 2017-04-26 | 华南理工大学 | Polydopamine-based high-saturation-degree structural color pigment and preparation method thereof |
CN107486112A (en) * | 2017-08-08 | 2017-12-19 | 浙江工商大学 | A kind of preparation method of the single dispersing colour silicon dioxide nanosphere of nondiscoloration |
CN107486112B (en) * | 2017-08-08 | 2020-01-21 | 浙江工商大学 | Preparation method of non-decolored monodisperse colored silicon dioxide nano-microspheres |
CN108442149B (en) * | 2018-04-28 | 2020-12-29 | 天津工业大学 | Cyclic dyeing method of fabric by using reactive dye colored microspheres |
CN108442149A (en) * | 2018-04-28 | 2018-08-24 | 天津工业大学 | A kind of dyeing cycle method of reactive dye color micro-sphere to fabric |
CN109667170A (en) * | 2018-12-29 | 2019-04-23 | 苏州恒瑞迦俐生生物医药科技有限公司 | A kind of coloring process of polymer microsphere |
CN110006886B (en) * | 2019-04-24 | 2022-01-11 | 江苏大学 | Nanocrystallization color-sensitive sensor and method for judging wheat mildew degree by using same |
CN110006886A (en) * | 2019-04-24 | 2019-07-12 | 江苏大学 | A kind of nanosizing color sensitive sensor and its method for differentiating wheat moulding ability |
CN111206440A (en) * | 2020-03-12 | 2020-05-29 | 蚌埠学院 | Preparation method of color nanospheres with uniform particle size |
CN115193414A (en) * | 2021-04-09 | 2022-10-18 | 中国科学院理化技术研究所 | Application of heterogeneous porous polymer microspheres in dye adsorption |
CN113861737A (en) * | 2021-09-08 | 2021-12-31 | 浙江天画家居用品有限公司 | Environment-friendly antibacterial finger painting pigment containing nano-silver modified silicon dioxide colored composite microspheres |
CN114516931A (en) * | 2022-02-25 | 2022-05-20 | 苏州仁端生物医药科技有限公司 | Preparation method of nanoscale colored microspheres based on electrostatic effect |
CN114775306A (en) * | 2022-04-12 | 2022-07-22 | 天津工业大学 | Preparation method of polyethyleneimine composite dye nanospheres |
CN114775306B (en) * | 2022-04-12 | 2023-12-22 | 天津工业大学 | Preparation method of polyethyleneimine composite dye nanospheres |
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