CN107419563A - A kind of polymer overmold dispersible pigment color paste and preparation method thereof - Google Patents
A kind of polymer overmold dispersible pigment color paste and preparation method thereof Download PDFInfo
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- CN107419563A CN107419563A CN201710463869.3A CN201710463869A CN107419563A CN 107419563 A CN107419563 A CN 107419563A CN 201710463869 A CN201710463869 A CN 201710463869A CN 107419563 A CN107419563 A CN 107419563A
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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
- D06P1/5257—(Meth)acrylic acid
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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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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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- 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
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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
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
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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
- D06P1/60—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 polyethers
- D06P1/613—Polyethers without nitrogen
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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
- D06P1/673—Inorganic compounds
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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
- 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
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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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
- 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
- D06P3/70—Material containing nitrile groups
-
- 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
- C08F220/1812—C12-(meth)acrylate, e.g. lauryl (meth)acrylate
Abstract
Present invention is disclosed a kind of polymer overmold dispersible pigment color paste available for fiber original liquid coloring, the mill base contains the components such as polymer overmold pigment, surfactant, water-miscible organic solvent, pH value regulator and water, the coated pigment mill base is used for fiber original liquid coloring, has the series of advantages such as uniform coloring, water-fastness, good spinnability.
Description
Technical field
The present invention relates to dispersible pigment color paste technical field, more particularly to a kind of polymer overmold dispersible pigment color paste and its preparation side
Method.
Background technology
The wet spinning fiber such as viscose rayon, acrylic fiber, it is the common fiber species of field of textiles.At present, using dye
Expect to dye the fabric that above-mentioned fiber and fiber manufacture, be the major way that above-mentioned fiber product is coloured.However, dye
Expect that energy consumption, the discharge of wastewater problem of dyeing course are increasingly serious, the larger energy-saving and emission-reduction pressure of traditional dyeing and finishing industry faces.It is fine
Tie up original liquid coloring technology to refer to add the technique that colouring agent directly spins colored fibre in the spinning solution of fiber, the technology is kept away
A series of problems, such as having exempted from high energy consumption, a large amount of discharge of wastewater that traditional dyeing is brought.
In recent years, original liquid coloring technology has obtained larger rule in the wet spinning colored fibre production field such as viscose glue, acrylic fibers
The application of mould, granules of pigments is stably dispersed in the aqueous color paste formed in water-based system, turn into the field it is most commonly seen
One of toner.However, because the wet spinning stoste viscosity of the fibers such as viscose glue, acrylic fibers is big, complicated component, electrolyte content are high,
And production process is usually associated with a series of processes such as mixed at high speed, quick flowing, high shear force, stretching, washing, traditional approach
The aqueous color paste of production often because with spinning solution poor compatibility, granules of pigments reunite, dispersant solution desorption etc. reason, lead
Cause the problems such as blocking spinneret orifice, fiber washing color fastness difference occur, water-based pigment colour paste is to influence fiber original liquid coloring technology
Using the critical materials with properties of product.
Granules of pigments can effectively reduce intergranular active force after the processing of chemically or physically method, increase electrostatic
Repulsion and steric hindrance, be advantageous to improve stability of the granules of pigments in water-based system and spinning solution.United States Patent (USP)
US6916862 discloses a kind of method by preparing dispersed ultrafine body in surface of pigments grafting hydrophilic segment；United States Patent (USP)
US7338988, which is disclosed, a kind of to be added polyacrylate dispersion in aqueous pigment dispersions by physical absorption and prepares ink jet ink
The method of water, this method positive effect on the color fastness for improving the plastic basis materials such as polyethylene, polyvinyl chloride；Chinese patent
CN102926224 discloses a kind of method that superfine pigment mill base is prepared by fine emulsion polymerization, complex process, degree of polymerization control
Difficulty height processed.
Acrylic monomer abundance, novel functional monomer emerge in an endless stream, and synthesis technique is ripe, and polymer molecular weight is easy
Control；Suitable monomer is selected to be polymerize in surface of pigments, steric hindrance can be provided for pigment by forming macromolecular chain segment, simultaneously
The polymer of surface of pigments and the polymer of free state can play dispersant；In addition, acronal have into
Film effect, adhesive can be played a part of in the fibre, lift the washing fastness of fiber, reduce the phenomenon that washing is decolourized.
However, at present, there is not yet carrying out cladding to pigment with monomers such as acrylic acid prepares dispersible pigment color paste, and it is former for wet spinning fiber
The report of liquid coloring.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of polymer overmold dispersible pigment color paste, described poly-
Compound coated pigment mill base include pigment, surfactant, polymer, initiator, water-miscible organic solvent, pH value regulator,
The water of antimildew disinfectant and surplus；In terms of the mass percent of polymer overmold dispersible pigment color paste gross mass, including pigment 15~
40%th, surfactant, which accounts for the 10~30% of pigment mass, polymer and accounts for the 10~30% of pigment mass, initiator, accounts for polymer
Monomer mass 0.2~0.5%, water-miscible organic solvent at least 10%.
The surfactant is at least two interworkings in anionic or nonionic surface active agent, and wherein one
Kind is containing the surfactant with general formula structure：
Preferably, in the formula, R1It is the alkyl or aromatic radical containing carbon number between 1~20, includes 1 and 20；N is 1
Integer between~20, includes 1 and 20；M is H, Na, K, NH4In one kind.
Preferably, acrylic acid is contained in the polymer monomer, and contains methyl acrylate, ethyl acrylate, acrylic acid
N-butyl, isobutyl acrylate, sec-butyl acrylate, tert-butyl acrylate, cyclohexyl acrylate, lauryl acrylate, propylene
Acid -2- diethyl acetamidomalonates, 2-Hydroxy ethyl acrylate, 2-hydroxypropyl acrylate, methacrylic acid, methyl methacrylate,
EMA, n-BMA, methacrylic acid -2- ethylhexyls, lauryl methacrylate, benzene second
In the monomers such as alkene, acrylonitrile, vinylacetate, acrylamide, N hydroxymethyl acrylamide, N- butoxy methyl acrylamides
It is a kind of.
Preferably, the water-miscible organic solvent is glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, one
It is one or more in diglycol ethylene monobutyl ether.
Preferably, the initiator is one kind in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate.
Preferably, the pH value regulator is sodium hydroxide, ammoniacal liquor, sodium acid carbonate, sodium dihydrogen phosphate, sodium acetate, three second
One kind in hydramine.
A kind of preparation method of polymer overmold dispersible pigment color paste, method and step are as follows：
S1：Surfactant is dissolved into water, regulation pH value is 8~9, and low whipping speed is under 500~1500r/min
Pigment is added, polymer monomer is added dropwise after stirring again, continues to stand 5~10h after stirring at least 30min, is then transferred into
Maximum particle diameter is ground to less than 1 μm with 1500~3000r/min rotating speed in sand mill, obtains pigment dispersion；
S2：By the pigment dispersion obtained by S1 be transferred to equipped with agitator, thermometer, condenser reaction unit in, lead to
Enter nitrogen, mixing speed control is warming up to 60~80 DEG C under 200~1000r/min, initiator is slowly added dropwise, and reacts 1~8h
Afterwards, filter, obtain coated pigment dispersion；
S3：Under stirring, water-miscible organic solvent is added into the coated pigment dispersion obtained by S2, obtains polymer
Coated pigment mill base.
Addition part antimildew disinfectant can be needed to decide whether to need according to actual product, to prevent long-time storage
Cause mill base occur it is mouldy, distribute the problems such as stench, antimildew disinfectant can be in S3, into the coated pigment dispersion of gained
Added together when adding water-miscible organic solvent.Species and dosage of the invention for antimildew disinfectant used, it is not particularly limited,
But it is typically chosen all kinds of environmental protection standards of textile and antimildew disinfectant species that regulation is not particularly limited, and selection can meet
The minimum addition of antimycotic antiseptic requirement.
In the present invention, surfactant used is at least two interworkings of anionic or nonionic surface active agent,
And the addition suggestion containing the surfactant with logical formula (I) structure is the 0.5 of polymer overmold dispersible pigment color paste gross mass
~4%.In the present invention, for being not particularly limited with the surfactant of the surfactant compound with logical formula (I) structure,
As long as the surfactant for having certain peptizaiton to granules of pigments can use in the present invention, anion can be selected
Surfactant includes sulfonate surfactant, such as sodium alkyl benzene sulfonate, alkylsulfonate, alpha-alkene sulfonate AOS, or
Person's carboxylate fluorocarbon surfactant：Lamepon A, N- acyl amino hydrochlorates, or sulfuric ester type surfactant：Fatty alcohol sulphur
Acid esters salt, secondary alkyl sulphate salt, polyoxyethylene alkyl ether sulfate salt, the sulfuric acid of derivative of fatty acid；Nonionic
Type surfactant, polyoxyethylene alkylphenol condensation product can be selected：OP-7, OP-10 or OP-15, or Polyoxyethylene fatty
Alcohol condensation product：Peregal 0-10, peregal 0-20, peregal 0-25 or peregal A-20, or polyoxyethylene polyols ether fat
Fat acid esters：Tween40, Tween60 or Twenn80, or the polyoxyethylene esters of aliphatic acid：SG-10、SE-10、OE-15.
In the present invention, water-miscible organic solvent used is glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol only son
At least one of ether, diethylene glycol monobutyl ether.It is found by the applicant that the water-miscible organic solvent is with having logical formula (I) knot
The surfactant compound of structure uses, and is advantageous to the spinnability of fully dispersed lifting spinning solution of the mill base in spinning solution,
And lifting prepares the wash durability of fiber.
Preferably, the initiator is the one or more in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate.
Preferably, the pH value regulator is sodium hydroxide, ammoniacal liquor, sodium acid carbonate, sodium dihydrogen phosphate, sodium acetate, three second
One or more in hydramine.
In pigment production and application field, the concrete structure of pigment, such as benzene can be represented using pigment product call number
And imidazolone Huang is named as C.I. pigment yellow 154s (C.I.Pigment Yellow 154), the pigment of phthalocyanine blue 15: 3 is named
For C.I. pigment blue 15s: 3 (C.I.Pigment Blue 15: 3), the specific knot of pigment representated by organic pigment product call number
Structure can according to organic pigment product call number from《Organic pigment index card》Etc. being inquired about in conventional books.In the present invention, to used
There is no particular restriction for pigment, but recommends that tinting strength, tinting power is high, price is relatively cheap, the preferable commercialization pigment of weatherability, used
Pigment can be but not limited to following pigment：Carbon black, C.I. pigment red 4s 8: 2, C.I. pigment red 4s 8: 4, C.I. pigment red 4s 9: 1,
C.I. paratonere 52: 2, C.I. paratoneres 64: 1, C.I. pigment red 81s, C.I. pigment Red 8s 8, C.I. Pigment Red 9s 2, C.I. pigment
Red 101, C.I. paratoneres 104, C.I. paratoneres 105, C.I. paratoneres 106, C.I. paratoneres 108, C.I. pigment red 112s,
C.I. pigment red 122, C.I. pigment red 123s/C.I. pigment red 146s, C.I. pigment red 149s, C.I. paratoneres 166, C.I. face
Expect red 168, C.I. paratoneres 170, C.I. paratoneres 172, C.I. paratoneres 185, C.I. paratoneres 190, C.I. paratoneres
254th, C.I. pigment Yellow 14s, C.I. pigment yellows 74, C.I. pigment yellows 95, C.I. pigment yellows 100, C.I. pigment yellows 104, C.I. face
Material Huang 108, C.I. pigment Yellow 12s 0, C.I. pigment yellows 153, C.I. pigment blue 15s: 3, C.I. pigment blue 15s: 4, C.I. alizarol saphirols
15: 6, one kind in C.I. pigment blue 1s 7: 1, C.I. alizarol saphirols 56, C.I. alizarol saphirols 63.
Compared with prior art, the device have the advantages that being：
The disclosed polymer overmold dispersible pigment color paste for fiber original liquid coloring, can be used for viscose rayon,
The original liquid coloring of the wet spinning fiber such as acrylic fiber, have and be not easily blocked spinneret orifice, continuous spinning time length, wash durability
The advantages that good.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Surfactant used has the structure of logical formula (I)：
Wherein, in surfactant A, R1For methyl, n 20, M H；In surfactant B, R1For C20H41, n 10, M
For Na；In surfactant C, R1For C4H9C6H4, n 1, M NH4。
Embodiment 1
By 30g neopelexes and 15g surfactant As in 500g deionized waters it is fully dispersed after, stirring
Speed is mixed to add 300g pigment red 112s under 500r/min, after being well mixed, the pH value for adding pH value regulator regulation slurry is
8, then 10g acrylic acid and 20g lauryl acrylates is added dropwise, continue to stand 5h after stirring 30min, gained slurry is transferred to sand milling
In machine, 1.5h is ground under 2000r/min, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 70 DEG C are warming up under 600r/min, then is slowly added dropwise molten
In the 0.06g ammonium persulfate solutions of 10g deionized waters, after reacting 6h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 0.05g antimildew disinfectants, 115g diglycol list ether, that is, obtain polymer overmold pigment red 112 mill base.
Embodiment 2
By 50g OP-10 and 40g surfactant B in 390g deionized waters it is fully dispersed after, low whipping speed is
300g carbon blacks are added under 1000r/min, are well mixed, the pH value for adding pH value regulator regulation slurry is 8, then 30g first is added dropwise
Base n-butyl acrylate and 60g acrylic acid, continue to stand 8h after stirring 60min, gained slurry is transferred in sand mill,
4h is ground under 1500r/min, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 80 DEG C are warming up under 200r/min, then is slowly added dropwise molten
In the 0.19g potassium persulfate solutions of 29g deionized waters, after reacting 4h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 101g ethylene glycol monobutyl ethers, that is, obtain polymer overmold carbon black color paste.
Embodiment 3
By 10g peregals 0-20 and 5g surfactant C in 700g deionized waters it is fully dispersed after, low whipping speed is
150g pigment Yellow 14s are added under 800r/min, after being well mixed, the pH value for adding pH value regulator regulation slurry is 8.5, then is dripped
Add 10g acrylic acid and 5g vinylacetates, continue to stand 10h after stirring 50min, gained slurry is transferred in sand mill,
1h is ground under 2500r/min, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 80 DEG C are warming up under 1000r/min, then be slowly added dropwise
The 0.04g sodium peroxydisulfate solution of 10g deionized waters is dissolved in, after reacting 1h, the filter paper for being 1000nm with aperture filters, in stirring shape
0.05g antimildew disinfectants, 110g glycol monoethyl ethers are added under state, that is, obtains polymer overmold pigment Yellow 14 mill base.
Embodiment 4
By 40g OP-15 and 40g surfactant A in 330g deionized waters it is fully dispersed after, low whipping speed is
Addition 400g pigment blue 15s under 1500r/min: 3, after being well mixed, the pH value for adding pH value regulator regulation slurry is 9, then is dripped
Add 40g acrylic acid and 20gN- butoxy methyl acrylamides, continue to stand 8h after stirring 60min, gained slurry is transferred to sand
In grinding machine, 5h is ground under 3000r/min, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 70 DEG C are warming up under 600r/min, then is slowly added dropwise molten
In the 0.30g sodium peroxydisulfate solution of 10g deionized waters, after reacting 8h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 0.05g antimildew disinfectants, 120g diethylene glycol monobutyl ethers, that is, obtain polymer overmold pigment blue 15: 3 mill bases.
Comparative example 5
By 50g OP-10 and 40g surfactant B in 480g deionized waters it is fully dispersed after, low whipping speed is
300g carbon blacks are added under 1000r/min, are well mixed, the pH value for adding pH value regulator regulation slurry is 8, after stirring 60min
8h is stood, gained slurry is transferred in sand mill, 4h is ground under 1500r/min, is tested through particle diameter, its maximum particle diameter is less than
1 μm, the filter paper for being 1000nm with aperture filters, and 101g ethylene glycol monobutyl ethers and 29g deionized waters is added under stirring, i.e.,
Obtain carbon black color paste.
Comparative example 6
By 50g OP-10 and 40g surfactant B in 390g deionized waters it is fully dispersed after, low whipping speed is
300g carbon blacks are added under 1000r/min, are well mixed, the pH value for adding pH value regulator regulation slurry is 8, then 30g first is added dropwise
Base n-butyl acrylate and 60g acrylic acid, continue to stand 8h after stirring 60min, gained slurry is transferred in sand mill,
4h is ground under 1500r/min, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 80 DEG C are warming up under 200r/min, then is slowly added dropwise molten
In the 0.19g potassium persulfate solutions of 29g deionized waters, after reacting 4h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 101g deionized waters, that is, obtain polymer overmold carbon black color paste.Comparative example 7
By 50g OP-10 and 40g surfactant B in 390g deionized waters it is fully dispersed after, low whipping speed is
300g carbon blacks are added under 1000r/min, are well mixed, the pH value for adding pH value regulator regulation slurry is 8, then 90g first is added dropwise
Base n-butyl acrylate, continue to stand 8h after stirring 60min, gained slurry is transferred in sand mill, ground under 1500r/min
4h is ground, is tested through particle diameter, its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 80 DEG C are warming up under 200r/min, then is slowly added dropwise molten
In the 0.19g potassium persulfate solutions of 29g deionized waters, after reacting 4h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 101g ethylene glycol monobutyl ethers, that is, obtain polymer overmold carbon black color paste.
Comparative example 8
By the polymerisable emulsifier of 40g OP-15 and 40g dimeric dibasic acid structures in 330g deionized waters it is fully dispersed after,
Mixing speed is that 400g pigment blue 15s are added under 1500r/min: 3, after being well mixed, add the pH of pH value regulator regulation slurry
It is worth for 9, then 40g acrylic acid and 20gN- butoxy methyl acrylamides is added dropwise, continues to stand 8h after stirring 60min, gained is starched
Material is transferred in sand mill, is ground 5h under 3000r/min, is tested through particle diameter, and its maximum particle diameter is less than 1 μm.
Above-mentioned slurry is transferred in reactor, is passed through nitrogen, 70 DEG C are warming up under 600r/min, then is slowly added dropwise molten
In the 0.30g sodium peroxydisulfate solution of 10g deionized waters, after reacting 8h, the filter paper for being 1000nm with aperture filters, in stirring
Lower addition 0.05g antimildew disinfectants, 120g diethylene glycol monobutyl ethers, that is, obtain polymer overmold pigment blue 15: 3 mill bases.
Application performance test
1) spinnability is tested
The mill base for taking 30 grams of embodiment 1-3 and comparative example 5-7 to prepare respectively, is well mixed with 500 grams of rayon spinning stostes
Afterwards, it is subjected to spinning, spinning by the spinneret orifice of the mm dia of 120 hole 0.08 formed with color spinning stoste through vacuum defoamation
Speed is 5m/min, and in rayon spinning stoste used, Methyl cellulose cellulose content is 8.5%；30 grams of embodiments 4 and contrast are taken respectively
Mill base prepared by example 8, after being well mixed with 500 grams of Polyacrylonitrile Fiber Spinning Solutions, through vacuum defoamation formed with color spinning stoste, is led to
The spinneret orifice for crossing the mm dia of 120 hole 0.08 carries out spinning, and spinning speed 5m/min, Polyacrylonitrile Fiber Spinning Solution used is polypropylene
Nitrile content is 8.0% sodium thiocyanate solution, and technique used is sodium sulfocyanate wet spinning technology.
After continuous spinning 3 hours, observation, which whether there is, blocks spinneret orifice situation.√ represents to have no spinning hole plug；
Zero represents visible a small amount of spinning hole plug；× represent that spinneret orifice largely blocks even whole block.
2) the water-fastness test of fiber
5 grams of above-mentioned fibers are taken respectively, are put into together with 100 grams of deionized waters in the flask with condensing reflux pipe, in 95 DEG C
Lower heating 3 hours, takes out fiber, sees whether solution changes colour.√ represents to have no discoloration；Zero represents slightly to change colour, but unobvious, needs
Examining to find；× represent that solution has obvious discoloration.
3) test result
Above-mentioned test result is as shown in table 1：
The mill base application performance test result of table 1.
Conclusion：Pass through embodiment 2 and comparative example 5 (uncoated granules of pigments), it can be seen that uncoated granules of pigments
Mill base spinnability and wash durability it is poor；
Pass through embodiment 2 and comparative example 6 (being free of water-miscible organic solvent), it can be seen that containing water-soluble is not organic
The mill base of solvent, granules of pigments is poor with fibers adhesion, and wash durability is poor；
Pass through embodiment 2 and comparative example 7 (acrylic monomers is free of in the polymer of coated pigment), it can be seen that
Due to lacking the acrylic monomers with cementation, granules of pigments is poor with fibers adhesion, and wash durability is poor；
Pass through embodiment 4 and comparative example 8, it can be seen that due to lacking with special construction in comparative example 8
Surfactant, granules of pigments is dispersed poor in spinning solution, causes spinnability and water-wash resistance to decline.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of polymer overmold dispersible pigment color paste, it is characterised in that the polymer overmold dispersible pigment color paste includes pigment, surface is lived
Property agent, polymer, initiator, water-miscible organic solvent, pH value regulator, the water of antimildew disinfectant and surplus；With polymer bag
Cover the mass percent meter of dispersible pigment color paste gross mass, including pigment 15~40%, surfactant account for pigment mass 10~
30%th, polymer account for the 10~30% of pigment mass, initiator account for polymer monomer quality 0.2~0.5%, it is water-soluble organic
Solvent at least 10%.
The surfactant is at least two interworkings in anionic or nonionic surface active agent, and one of which is
Contain the surfactant with general formula structure：
A kind of 2. polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that：In the formula, R1It is carbon containing
Alkyl or aromatic radical of the number between 1~20, include 1 and 20；N is the integer between 1~20, includes 1 and 20；M be H, Na, K,
NH4In one kind.
3. a kind of polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that contain in the polymer monomer
Have acrylic acid, and containing methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, sec-butyl acrylate,
Tert-butyl acrylate, cyclohexyl acrylate, lauryl acrylate, acrylic acid-2-ethyl ethyl ester, 2-Hydroxy ethyl acrylate, third
Olefin(e) acid -2- hydroxy propyl esters, methacrylic acid, methyl methacrylate, EMA, n-BMA, first
Base acrylic acid-2-ethyl caproite, lauryl methacrylate, styrene, acrylonitrile, vinylacetate, acrylamide, N- hydroxyl first
One kind in the monomers such as base acrylamide, N- butoxy methyl acrylamides.
A kind of 4. polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that the water-miscible organic solvent
For one or more in glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether.
5. a kind of polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that the initiator is persulfuric acid
One kind in potassium, ammonium persulfate, sodium peroxydisulfate.
6. a kind of polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that the pH value regulator is hydrogen
One kind in sodium oxide molybdena, ammoniacal liquor, sodium acid carbonate, sodium dihydrogen phosphate, sodium acetate, triethanolamine.
A kind of 7. preparation method of polymer overmold dispersible pigment color paste according to claim 1, it is characterised in that method and step
It is as follows：
S1：Surfactant is dissolved into water, regulation pH value is 8~9, and low whipping speed is to be added under 500~1500r/min
Pigment, polymer monomer is added dropwise after stirring again, continues to stand 5~10h after stirring at least 30min, be then transferred into sand milling
Maximum particle diameter is ground to less than 1 μm with 1500~3000r/min rotating speed in machine, obtains pigment dispersion；
S2：By the pigment dispersion obtained by S1 be transferred to equipped with agitator, thermometer, condenser reaction unit in, be passed through nitrogen
Gas, mixing speed control is warming up to 60~80 DEG C under 200~1000r/min, initiator is slowly added dropwise, after reacting 1~8h, mistake
Filter, obtains coated pigment dispersion；
S3：Under stirring, water-miscible organic solvent is added into the coated pigment dispersion obtained by S2, obtains polymer overmold
Dispersible pigment color paste.
8. the answering in fiber original liquid coloring technology of the polymer overmold dispersible pigment color paste obtained by claim 1-5 any one
With.
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| CN111826027A (en) * | 2020-08-05 | 2020-10-27 | 常熟世名化工科技有限公司 | Carbon black color paste and preparation method and application thereof |
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Application publication date: 20171201 |