CN102127312A - Preparation method of superfine coating pigment paste for coloring of Lyocell fiber stock solution - Google Patents
Preparation method of superfine coating pigment paste for coloring of Lyocell fiber stock solution Download PDFInfo
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- CN102127312A CN102127312A CN2010105755103A CN201010575510A CN102127312A CN 102127312 A CN102127312 A CN 102127312A CN 2010105755103 A CN2010105755103 A CN 2010105755103A CN 201010575510 A CN201010575510 A CN 201010575510A CN 102127312 A CN102127312 A CN 102127312A
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Abstract
本发明涉及一种Lyocell纤维原液着色用超细包覆颜料色浆的制备方法，属于精细化工领域。本发明以可聚合分散剂为主要助剂，通过高速分散制备了超细颜料分散体，然后向体系中滴加引发剂和共聚单体，继续高速分散，升温反应一段时间，使聚合物包覆到颜料表面。制备的Lyocell纤维原液着色用超细包覆颜料色浆的分散稳定性高，与Lyocell纤维纺丝液相容性好、可纺性高，且纺丝得到的Lyocell纤维着色丝着色均匀、色光纯正、色牢度优良，省去了后续染色加工。The invention relates to a preparation method of an ultrafine coated pigment paste for Lyocell fiber stock solution coloring, which belongs to the field of fine chemicals. In the present invention, the polymerizable dispersant is used as the main auxiliary agent to prepare an ultrafine pigment dispersion through high-speed dispersion, and then the initiator and comonomer are added dropwise to the system to continue the high-speed dispersion, and the temperature is raised for a period of time to make the polymer coating to the paint surface. The prepared ultra-fine coated pigment paste for Lyocell fiber stock solution coloring has high dispersion stability, good compatibility with Lyocell fiber spinning solution, high spinnability, and the Lyocell fiber colored yarn obtained by spinning is evenly colored and pure in shade , Excellent color fastness, eliminating the need for subsequent dyeing processing.
Description
Technical field
The invention belongs to field of fine chemical, be specifically related to the preparation method of a kind of Lyocell fiber original liquid coloring with ultra-fine coating dispersible pigment color paste.
Technical background
Compare with viscose fiber, Lyocell fiber production flow process is simple, environmental pollution is little, characteristics such as fibre property excellence, and extremely people pay close attention in recent years.Lyocell fiber original liquid coloring is that dispersible pigment color paste is directly added in the Lyocell fiber spinning solution, after mixing, forms colored gluey thread by spinning nozzle, passes through precipitation bath then, generates the coloured silk of Lyocell.In the original liquid coloring process, the mill base of adding is to the spinning property of spinning solution, and the color of coloured fiber and mechanical property influence are very big, are the keys that can Lyocell fiber staining silk be produced smoothly.The original liquid coloring of realizing the Lyocell fiber promotes the energy-saving and emission-reduction of industry to promoting the color characteristics of fiber, has great importance.
Though the research about the preparation of superfine pigment mill base has a lot, the research of Lyocell fiber original liquid coloring usefulness superfine pigment mill base seldom.Literature search is found about the research document of the original liquid coloring of Lyocell fiber also considerably less, only there are people such as Austrian Avinash P.Manian and Hartmut Ruef to adopt vat dyes that it is carried out dyed in the mass, their specific practice is after vat dyes is reduced into leuco compound, add in the Lyocell spinning solution, spray in the back in the wire process more at last leuco compound is carried out oxidative color-developing, thereby realized the original liquid coloring of Lyocell fiber.Patent WO01/11121 discloses the mineral dye that a kind of employing contains a small amount of heavy metal ion to be added in the cellulose spinning fluid, spin after the mixing the method for Lyocell fiber staining silk.
The present invention is tinting material with pigment, and the vinyl monomer that adopts the polymerizable dispersion agent and contain two keys has prepared the Lyocell original liquid coloring with ultra-fine coating dispersible pigment color paste by mini-emulsion polymerization.The ultra-fine coating dispersible pigment color paste particle diameter of the present invention preparation is little, narrow particle size distribution, advantage such as the high and Lyocell fiber spinning solution consistency of stability is good.
Summary of the invention
The object of the invention provides the preparation method of a kind of Lyocell fiber original liquid coloring with ultra-fine coating dispersible pigment color paste.Promptly adopt the polymerizable dispersion agent to prepare the superfine pigment dispersion earlier, drip vinyl monomer and initiator to it then, pass through mini-emulsion polymerization, make polymer overmold to surface of pigments, it is little that the ultra-fine coating pigment that this method prepares has a particle diameter, narrow particle size distribution with advantages such as Lyocell fiber spinning solution consistency are good, can reach the purpose that improves original liquid coloring fiber colour fastness.
Technical scheme of the present invention: a kind of Lyocell fiber original liquid coloring is with the preparation method of ultra-fine coating dispersible pigment color paste, with the polymerizable dispersion agent is main auxiliary agent, adopt high speed dispersion to prepare the superfine pigment dispersion, in system, drip initiator and comonomer continuation high speed dispersion then, dispersion liquid transferred in the reactor heat up, after isothermal reaction for some time, preparation Lyocell fiber original liquid coloring is with ultra-fine coating dispersible pigment color paste.
Concrete processing parameter is: pigment accounts for 5～30% (being massfraction) of whole system, and the polymerizable dispersion agent is 10～30% to pigment ratio, and composite anion surfactant is 0.2～2% to pigment ratio, and all the other add water and mend full 100%.The superfine pigment dispersion prepared jitter time 1～4 hour.Drip comonomer then, the mass ratio of comonomer and pigment is 1～5%, continues to disperse after 0.5 hour, transfer in the reactor, feed nitrogen, be warming up to 60～90 ℃, drip initiator, initiator is 1～5% to monomeric ratio, isothermal reaction 1～4 hour.
Here selected pigment can be a kind of in carbon black, azo class pigment, triarylmethane compound pigment, phthalocyanine pigment, dioxazines pigment, quinophthalone class pigment, nitrogen methyne class pigment, nitro and nitrous base class pigment, condensed ring ketone pigment, pyrazolo quinolinones pigment, pyroles pigment or the indoline-like pigment.
Here selected polymerizable dispersion agent can be allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ammonium sulfate (ANPS), allyloxy hydroxypropyl azochlorosulfonate acid sodium (AHPS), hydroxyethyl methacrylate propyl sulfonic acid sodium (HMPS); Or cation dispersing agent: one or more in methylacryoyloxyethyl hexadecyldimethyl benzyl ammonium brometo de amonio (DMHB), methacrylate based quaternary ammonium salt (PMQ), the methacrylate based bi-quaternary ammonium salt (PDQ).
Selected anion surfactant can be a metal carboxylate: N-acyl amino hydrochlorate, Lei Mibang-A or alcohol ether carboxylate; Sulfonates: Sodium dodecylbenzene sulfonate, dispersing agent C NF, sulfonated AOS; sulfuric ester salt: ether alcohol sulfate (AES), secondary alkyl sulfate (Teep01) or Sodium Lauryl Sulphate BP/USP, one or more of sodium lignosulfonate.
Selected comonomer can be one or both in (methyl) methyl acrylate, (methyl) butyl acrylate, vinylformic acid bay alcohol ester, (methyl) vinylformic acid, vinyl cyanide, vinylbenzene, n-methylolacrylamide, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, glycidyl acrylate, methacrylic acid urea groups ester, the diacetone-acryloamide(DAA).
Selected initiator is an oil-soluble initiator, can be azo-initiator, a kind of as in Diisopropyl azodicarboxylate, azo dicyclohexyl formonitrile HCN, 2,2'-Azobis(2,4-dimethylvaleronitrile), 2,2'-Azobis(2,4-dimethylvaleronitrile), the azo-bis-iso-dimethyl.
Beneficial effect of the present invention: the ultra-fine coating dispersible pigment color paste of the present invention's preparation can be applied to Lyocell fiber original liquid coloring, the dispersion effect of the ultra-fine coating dispersible pigment color paste of preparation is good, does not have deposited phenomenon, and stability is high, mill base and Lyocell fiber spinning solution consistency are good, the spinning property height.And the ultra-fine coating dispersible pigment color paste that uses the present invention's preparation spin Lyocell fiber staining wire coloring even, coloured light is pure, colour fastness is good, has saved follow-up dyeing processing.
Embodiment
Below by examples of implementation, further set forth outstanding advantage of the present invention and distinguishing feature, but the present invention is in no way limited to examples of implementation.
Example 1
Get carbon black 15g, polymerizable dispersant A NPS 3g, Sodium dodecylbenzene sulfonate 0.3g and deionized water 281.7g, place sand mill to grind 1 hour with 1800r/min speed, make black superfine pigment water-base disperse system, continue to grind 0.5 hour to wherein dripping the solution that contains Diisopropyl azodicarboxylate 0.006g, styrene solution 0.3g then, transfer in the reactor, feed nitrogen, be warming up to 60 ℃, 2 hours cooling discharges of isothermal reaction, the filtering with microporous membrane with 500nm can obtain the ultra-fine coating dispersible pigment color paste of black.Physical index is as follows: surface tension σ=37.4mN/m, viscosities il=6.58cP, the equal particle diameter d=152.4nm of Z.
Example 2
Get C.I. pigment Yellow 14 30g, polymerizable dispersion agent PMQ 6g, anion surfactant CNF 0.6g and deionized water 263.4g, place sand mill to grind 1.5 hours with 1800r/min speed, make yellow superfine pigment water-base disperse system, contain azo-bis-iso-dimethyl 0.024g to wherein dripping then, the solution of methyl methacrylate solution 1.2g continues to grind 0.5 hour, transfer in the reactor, feed nitrogen, be warming up to 70 ℃, 2.5 hours cooling discharges of isothermal reaction, the filtering with microporous membrane with 500nm can obtain yellow ultra-fine coating dispersible pigment color paste.Physical index is as follows: surface tension σ=21.7mN/m, viscosities il=6.12cP, the equal particle diameter d=148.7nm of Z.
Example 3
Get C.I. pigment Blue 15: 360g, polymerizable dispersant A HPS 12g, anion surfactant Lei Mibang-A 1.2g and deionized water 226.8g, place sand mill to grind 2 hours with 1800r/min speed, make blue superfine pigment water-base disperse system, contain 2,2'-Azobis(2,4-dimethylvaleronitrile) 0.048g to wherein dripping then, the solution of methylol vinylformic acid methane amide 2.4g continues to grind 0.5 hour, transfer in the reactor, feed nitrogen, be warming up to 90 ℃, 3 hours cooling discharges of isothermal reaction, the filtering with microporous membrane with 500nm can obtain blue ultra-fine coating dispersible pigment color paste.Physical index is as follows: surface tension σ=18.84mN/m, viscosities il=5.76cP, the equal particle diameter d=155.6nm of Z.
Example 4
Get C.I. pigment violet 1 990g, polymerizable dispersion agent DMHB 18g, anion surfactant sodium lignosulfonate 1.8g and deionized water 190.2g, place sand mill to grind 4 hours with 1800r/min speed, make purple superfine pigment water-base disperse system, contain azo dicyclohexyl formonitrile HCN 0.072g to wherein dripping then, vinylbenzene 2.4g, the solution of vinylformic acid bay alcohol ester 1.2g, continue to grind 0.5 hour, transfer in the reactor, feed nitrogen, be warming up to 75 ℃, 4 hours cooling discharges of constant temperature, with the filtering with microporous membrane of 500nm, can obtain the ultra-fine coating dispersible pigment color paste of purple.Physical index is as follows: surface tension σ=24.7mN/m, viscosities il=7.44cP, the equal particle diameter d=143.5nm of Z.
Claims (6)
1. a Lyocell fiber original liquid coloring is with the preparation method of ultra-fine coating dispersible pigment color paste, with the polymerizable dispersion agent is main auxiliary agent, prepared the superfine pigment dispersion by high speed dispersion, in system, drip comonomer then and continue high speed dispersion, dispersion liquid transferred in the reactor heat up, and drip initiator isothermal reaction for some time, prepare Lyocell fiber dyed in the mass with ultra-fine coating dispersible pigment color paste; Concrete processing parameter is: pigment accounts for 5～30% (the following massfractions that also are) of whole system, and the polymerizable dispersion agent is 10～30% to pigment ratio, and composite anion surfactant is 0.2～2% to pigment ratio, and all the other add water and mend full 100%.Under the effect of high speed dispersor high speed dispersion, disperseed 1～4 hour earlier, make the superfine pigment dispersion, drip comonomer then, the mass ratio of comonomer and pigment is 1～5%, continues to disperse after 0.5 hour, transfer in the reactor, feed nitrogen, be warming up to 60～90 ℃, drip initiator, initiator is 0.2～1.5% to monomeric ratio, isothermal reaction 1～4 hour.
2. Lyocell fiber original liquid coloring as claimed in claim 1 is with ultra-fine coating dispersible pigment color paste, it is characterized in that described pigment can be a kind of in carbon black, azo class pigment, triarylmethane compound pigment, phthalocyanine pigment, dioxazines pigment, quinophthalone class pigment, nitrogen methyne class pigment, nitro and nitrous base class pigment, condensed ring ketone pigment, pyrazolo quinolinones pigment, pyroles pigment or the indoline-like pigment.
3. Lyocell fiber original liquid coloring as claimed in claim 1 is with ultra-fine coating dispersible pigment color paste, and it is characterized in that: described polymerizable dispersion agent can be an anionic dispersing agents: allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ammonium sulfate (ANPS), allyloxy hydroxypropyl azochlorosulfonate acid sodium (AHPS), hydroxyethyl methacrylate propyl sulfonic acid sodium (HMPS); Or cation dispersing agent: one or more in methylacryoyloxyethyl hexadecyldimethyl benzyl ammonium brometo de amonio (DMHB), methacrylate based quaternary ammonium salt (PMQ), the methacrylate based bi-quaternary ammonium salt (PDQ).
4. Lyocell fiber original liquid coloring as claimed in claim 1 is with ultra-fine coating dispersible pigment color paste; it is characterized in that: described anion surfactant can be a metal carboxylate: N-acyl amino hydrochlorate, Lei Mibang-A or alcohol ether carboxylate; Sulfonates: Sodium dodecylbenzene sulfonate, dispersing agent C NF, sulfonated AOS; sulfuric ester salt: ether alcohol sulfate (AES), secondary alkyl sulfate (Teep01) or Sodium Lauryl Sulphate BP/USP, a kind of in the sodium lignosulfonate.
5. Lyocell fiber original liquid coloring as claimed in claim 1 is with ultra-fine coating dispersible pigment color paste, and it is characterized in that: described comonomer can be one or both in (methyl) methyl acrylate, (methyl) butyl acrylate, vinylformic acid bay alcohol ester, (methyl) vinylformic acid, vinyl cyanide, vinylbenzene, n-methylolacrylamide, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, glycidyl acrylate, methacrylic acid urea groups ester, the diacetone-acryloamide(DAA).
6. Lyocell fiber original liquid coloring as claimed in claim 1 is with ultra-fine coating dispersible pigment color paste, it is characterized in that: described initiator is an oil-soluble initiator, can be azo-initiator, a kind of as in Diisopropyl azodicarboxylate, azo dicyclohexyl formonitrile HCN, 2,2'-Azobis(2,4-dimethylvaleronitrile), 2,2'-Azobis(2,4-dimethylvaleronitrile), the azo-bis-iso-dimethyl.
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Cited By (8)
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| CN102585554A (en) * | 2011-12-29 | 2012-07-18 | 苏州世名科技股份有限公司 | Preparation method for ultrathin pigment paste used for coloring viscose filament fiber dope |
| CN102926224A (en) * | 2012-11-27 | 2013-02-13 | 江南大学 | Preparation method of pigment ink for inkjet printing of non-adhesive textile |
| CN103710772A (en) * | 2013-12-30 | 2014-04-09 | 苏州世名科技股份有限公司 | Superfine carbon black water-based color paste for coloring fiber stock solution |
| CN106118131A (en) * | 2016-06-23 | 2016-11-16 | 苏州世名科技股份有限公司 | A kind of it is coated with AZOpigments continuous preparation method in branch's serpentine pipe |
| CN106245136A (en) * | 2016-08-17 | 2016-12-21 | 东华大学 | A kind of coloured superhigh molecular weight polyethylene fibers and preparation method thereof |
| CN107653704A (en) * | 2017-08-08 | 2018-02-02 | 江苏丽王科技股份有限公司 | A kind of fiber stoste mill base and preparation method thereof |
| CN109295517A (en) * | 2018-08-26 | 2019-02-01 | 上海金慈实业有限公司 | A kind of dope dyeing superelevation strength noctilucence silk and preparation method thereof |
| CN109385136A (en) * | 2018-09-21 | 2019-02-26 | 楼乐超 | A kind of preparation process of magnetic Nano ink |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102585554A (en) * | 2011-12-29 | 2012-07-18 | 苏州世名科技股份有限公司 | Preparation method for ultrathin pigment paste used for coloring viscose filament fiber dope |
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| CN103710772A (en) * | 2013-12-30 | 2014-04-09 | 苏州世名科技股份有限公司 | Superfine carbon black water-based color paste for coloring fiber stock solution |
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| CN106245136A (en) * | 2016-08-17 | 2016-12-21 | 东华大学 | A kind of coloured superhigh molecular weight polyethylene fibers and preparation method thereof |
| CN107653704A (en) * | 2017-08-08 | 2018-02-02 | 江苏丽王科技股份有限公司 | A kind of fiber stoste mill base and preparation method thereof |
| CN107653704B (en) * | 2017-08-08 | 2020-12-15 | 江苏丽王科技股份有限公司 | Fiber stock solution color paste and preparation method thereof |
| CN109295517A (en) * | 2018-08-26 | 2019-02-01 | 上海金慈实业有限公司 | A kind of dope dyeing superelevation strength noctilucence silk and preparation method thereof |
| CN109385136A (en) * | 2018-09-21 | 2019-02-26 | 楼乐超 | A kind of preparation process of magnetic Nano ink |
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Application publication date: 20110720 |