CN102585554A - Preparation method for ultrathin pigment paste used for coloring viscose filament fiber dope - Google Patents
Preparation method for ultrathin pigment paste used for coloring viscose filament fiber dope Download PDFInfo
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- CN102585554A CN102585554A CN2011104483163A CN201110448316A CN102585554A CN 102585554 A CN102585554 A CN 102585554A CN 2011104483163 A CN2011104483163 A CN 2011104483163A CN 201110448316 A CN201110448316 A CN 201110448316A CN 102585554 A CN102585554 A CN 102585554A
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Abstract
The invention discloses a preparation method for ultrathin pigment paste used for coloring viscose filament fiber dope. The preparation method comprises the following steps of: grinding and dispersing a polymerizable dispersant serving as a main assistant, a pigment and deionized water to obtain an ultrathin pigment water-based dispersion; after dropwise adding comonomers into the dispersion and continuing grinding and dispersing for a period of time, performing irradiation polymerization by using cobalt 60-gamma rays to polymerize the polymerizable dispersant with monomers; and coating the copolymer to the surface of the pigment. The ultrathin pigment paste used for coloring the viscose filament fiber dope prepared by the method is small in particle size, high in stability and free of precipitation after long-time storage; and the spinning dope is high in spinnability, small in color difference and high in color fastness.
Description
Technical field
The present invention relates to a kind of preparation method of dispersible pigment color paste, relate in particular to the preparation method of a kind of viscose rayon filament yarn fiber original liquid coloring, belong to field of fine chemical with the superfine pigment mill base.
Background technology
The viscose fiber original liquid coloring is to be evenly dispersed in mill base in the viscose fiber spinning solution, forms colored gluey thread through spinning nozzle, with the acid bath reaction, generates viscose tinting threads then.The original liquid coloring viscose fiber is compared with traditional genonema, has reduced painted technical process, practices thrift cost, has reduced environmental pollution, has promoted the energy-saving and emission-reduction of dyeing; And original liquid coloring viscose fiber aberration is little, and circulation ratio is preferably arranged.In process of production, the mill base of adding has tangible influence to the spinning property of spinning solution, the Difference Control and the colour fastness of look silk.
The mill base of domestic production at present; Mainly being suitable for the viscose staple fibre original liquid coloring, and can not being used for the original liquid coloring of viscose rayon filament yarn, mainly is because these performance mill bases are unstable; Granules of pigments is bigger; Strainability is poor, and variable color takes place in the spinning process easily, and granules of pigments is prone to stick to places such as pipeline, spinning nozzle and causes spinning property poor.Publication number is that the Chinese patent of CN101736429A discloses a kind of preparation method who adopts dispersion agent to grind the black color paste of carbon dust production viscose tinting threads; Publication number is the working method that the Chinese patent of CN1563527 discloses a kind of coloured viscose fiber; Specific practice is for to be made into pasty state with vat dyes with basic soln; The powder that takes a policy again reaction generates the leuco vat dye salts solution; In the viscose ripening process, add dye liquor and be mixed and made into painted viscose glue with it, spinning then, coloured viscose fiber is processed in concise and oven dry.But; The mill base that is used for the viscose rayon filament yarn fiber sprinning has higher requirement; Grain diameter must be less than 1 micron, and stability in storage requires high, requires can not stick to places such as pipeline, spinning nozzle because of granules of pigments in the mill base simultaneously and causes the spinning property variation; Spun long filament requires to have lower aberration and higher colour fastness, and present viscose fiber original liquid coloring is difficult to satisfy so harsh requirement with the superfine pigment mill base.
Summary of the invention
In order to overcome the deficiency that exists in the above-mentioned prior art; The invention provides the preparation method of a kind of viscose rayon filament yarn fiber original liquid coloring with the superfine pigment mill base; The superfine pigment mill base that is used for viscose rayon filament yarn fiber original liquid coloring that this method is prepared can overcome the conventional pigment mill base and exist particle big, and size-grade distribution is uneven; Filterableness is poor, with and flocculation be prone to take place in rayon spinning liquid and return problems such as thick.
The present invention for the technical scheme that solves its technical problem and adopt is:
The present invention is tinting material with pigment, adopts polymerizable dispersion agent and double bond containing comonomer to prepare the viscose rayon filament yarn original liquid coloring through mini-emulsion polymerization and high-energy radiation technology and uses the superfine pigment mill base.
A kind of viscose rayon filament yarn fiber original liquid coloring may further comprise the steps with the preparation method of superfine pigment mill base:
(1) places sand mill to grind 3～6 hours pigment, polymerizable dispersion agent and deionized water, make the superfine pigment aqueous based dispersions with the speed of 1800～3000r/min;
(2) in (1), drip comonomer in the gained superfine pigment aqueous based dispersions, under grinding rate described in (1), continue then to grind 1～1.5 hour, get dispersion liquid;
(3) gained dispersion liquid in (2) is transferred in the reactor drum, under continuous condition of stirring, adopted cobalt 60-gamma-rays that said dispersion liquid is carried out radiopolymerization, radiation agent consumption is 2～600,000 Curie, and radiated time is 30～120 minutes;
(4) dispersion liquid after radiotreatment in (3) is taken out,, promptly get viscose rayon filament yarn fiber original liquid coloring and use the superfine pigment mill base with the filtering with microporous membrane of 500nm;
Said pigment accounts for 8～20wt.% of whole mill base system total mass, and the mass ratio of said polymerizable dispersion agent and pigment is 6～20: 100, and the mass ratio of said comonomer and pigment is 2～5: 100, and surplus is a deionized water.
Said pigment is a kind of in carbon black, azo class pigment, phthalocyanine pigment, quinacridone pigments, thioindigo class pigment, triarylmethane compound pigment, anthraquinone pigment 、 dioxazines pigment and the quinophthalone class pigment, like C.I. Pigment Yellow 73 93, C.I. pigment blue 60 and C.I. pigment Violet 23 etc.
Said polymerizable dispersion agent is at least a in allyloxy Nonylphenoxy propyl alcohol T 46155 ammonium sulfate (ANPS), allyloxy hydroxypropyl azochlorosulfonate acid sodium (AHPS), hydroxyethyl methacrylate propyl sulfonic acid sodium (HMPS), methylacryoyloxyethyl hexadecyldimethyl benzyl ammonium brometo de amonio (DMHB), methacrylate based quaternary ammonium salt (PMQ) and the methacrylate based bi-quaternary ammonium salt (PDQ).
Said comonomer is at least a in vinylformic acid, methylacrylic acid, methyl acrylate, TEB 3K, Bing Xisuandingzhi, NSC 20956, vinylbenzene, vinylformic acid bay alcohol ester, vinyl cyanide, NMA, Hydroxyethyl acrylate, Rocryl 400, Propylene glycol monoacrylate, Rocryl 410, methylacrylic acid urea groups ester and the glycidyl acrylate.
Useful technique effect of the present invention is: the present invention is tinting material with pigment; Adopt polymerizable dispersion agent and double bond containing comonomer to prepare the viscose rayon filament yarn original liquid coloring and use the superfine pigment mill base through mini-emulsion polymerization and high-energy radiation technology; This mill base granules of pigments particle diameter is little and stability in storage is high; Standing storage does not have deposition, is easy to preserve; The particle diameter and the adhesive power of pigment particles are little, and the spinning property of spinning solution is high; Look silk front and back aberration is little in the spinning process; The colour fastness of look silk is good.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed description, but the invention is not restricted to the following example.
Embodiment 1
Get carbon black 20kg, polymerizable dispersant A HPS 1.2kg, deionized water 178.8kg; Place sand mill to grind 3 hours, make black superfine pigment water-base disperse system, continue to grind 1.5 hours to drip styrene 0.6kg wherein then with 1800r/min speed; Transfer in the reactor drum; Adopt the radiation of cobalt 60-gamma-rays, about 300,000 Curie of radiation agent consumption, radiated time 30 minutes; Take out material and use the filtering with microporous membrane of 500nm then, can obtain the long fine original liquid coloring of viscose glue with black superfine pigment mill base.
Embodiment 2
Get C.I. Pigment Yellow 73 93 powder 30kg, polymerizable dispersion agent HMPS 3kg, deionized water 167kg; Place sand mill to grind 4 hours, make yellow superfine pigment water-base disperse system, continue to grind 1.3 hours to dropwise addition of acrylic acid glycidyl ester 1.2kg wherein then with 2000r/min speed; Transfer in the reactor drum; Adopt the radiation of cobalt 60-gamma-rays, about 600,000 Curie of radiation agent consumption, radiated time 120 minutes; With the filtering with microporous membrane of 500nm, can obtain the long fine original liquid coloring of viscose glue with yellow superfine pigment mill base.
Embodiment 3
Get C.I. pigment blue 60 powder 40kg, polymerizable dispersion agent DMHB8kg, deionized water 152kg; Place sand mill to grind 5 hours, make blue superfine pigment water-base disperse system, then to wherein dripping TEB 3K 1.5kg with 2500r/min speed; Vinylformic acid bay alcohol ester 0.5kg continues to grind 1.2 hours, transfers in the reactor drum; Adopt the radiation of cobalt 60-gamma-rays, about 20,000 Curie of radiation agent consumption, radiated time 30 minutes; With the filtering with microporous membrane of 500nm, can obtain the long fine original liquid coloring of viscose glue with blue superfine pigment mill base.
Embodiment 4
Get C.I. pigment Violet 23 powder 16kg, polymerizable dispersant A NPS 1.28kg, deionized water 182.72kg; Place sand mill to grind 6 hours, make purple superfine pigment water-base disperse system, then to wherein dripping Rocryl 400 0.32kg with 3000r/min speed; Continue to grind 1 hour, transfer in the reactor drum, adopt the radiation of cobalt 60-gamma-rays; About 300,000 Curie of radiation agent consumption; Radiated time 60 minutes with the filtering with microporous membrane of 500nm, can obtain the long fine original liquid coloring of viscose glue with purple superfine pigment mill base.
The long fine original liquid coloring of the viscose glue of embodiment 1～4 preparation is used the superfine pigment mill base, by following method mill base performance and effect is tested:
(1) size distribution test
The size distribution of testing above-mentioned dispersible pigment color paste with the Zetasizer Nano Zs90 type nano particle size and the zeta potential instrument of Britain Ma Erwen Instr Ltd.; In the test result; D50 representes 50% through particle diameter, promptly surveys in the particle minimum grain size that 50% particle can both pass through, in like manner; D90, D99, D100 represent the minimum grain size that 90%, 99%, 100% particle can both pass through respectively, can describe the size distribution of dispersible pigment color paste with D50, D90, D99, D100.
(2) stable storing property testing
Airtight placement is after 90 days down at 25 ℃ with dispersible pigment color paste, and visual observations has or not the situation that obvious pigment deposition, flocculation etc. have a strong impact on stability that occurs.
(3) spinning property test
After superfine pigment mill base and the 100kg viscose fiber stoste of getting 3kg embodiment 1～4 preparation respectively mixes, carry out spinning with the spinning nozzle in 0.08 millimeter in 30 holes, spinning speed is 50m/min; 45 ℃ of control acid bath solidification liquid temperature, 60 ℃ of washing temperature, preparation viscose rayon filament yarn; Wherein, Acid bath solidification liquid composition is: 120g/L sulfuric acid, 250g/L sodium sulfate, 15g/L zinc sulfate.Continuous spinning 24 hours is observed the situation of stopping up spinning top that has or not.
(4) chromatism test
Objective ranking method and the GB/T 8424.3-2001 textile color stability test aberration of testing relative whiteness according to standard GB/T 8424.2-2001 textile color stability calculate; In the spinning property test process, get the viscose rayon filament yarn test aberration that spinning began 0.5 hour and prepared in 24 hours respectively.
(5) colour fastness test
The viscose rayon filament yarn for preparing in the spinning property test process is carried out the colour fastness test, and the colour fastness to washing test is tested according to GB/T 3921-2008 textile color stability test fastness to soaping standard; The colour fastness to perspiration test is tested according to GB/T 3922-1995 textiles colour fastness to perspiration TP.
According to above-mentioned testing method the viscose rayon filament yarn of embodiment 1～4 superfine pigment mill base and preparation thereof is tested, test result is as shown in table 1.
Table 1 embodiment 1～4 gained superfine pigment mill base test result
Claims (4)
1. a viscose rayon filament yarn fiber original liquid coloring is characterized in that: may further comprise the steps with the preparation method of superfine pigment mill base:
(1) places sand mill to grind 3～6 hours pigment, polymerizable dispersion agent and deionized water, make the superfine pigment aqueous based dispersions with the speed of 1800～3000r/min;
(2) in (1), drip comonomer in the gained superfine pigment aqueous based dispersions, under grinding rate described in (1), continue then to grind 1～1.5 hour, get dispersion liquid;
(3) gained dispersion liquid in (2) is transferred in the reactor drum, under continuous condition of stirring, adopted cobalt 60-gamma-rays that said dispersion liquid is carried out radiopolymerization, radiation agent consumption is 2～600,000 Curie, and radiated time is 30～120 minutes;
(4) dispersion liquid after radiotreatment in (3) is taken out,, promptly get viscose rayon filament yarn fiber original liquid coloring and use the superfine pigment mill base with the filtering with microporous membrane of 500nm;
Said pigment accounts for 8～20wt.% of whole mill base system total mass, and the mass ratio of said polymerizable dispersion agent and pigment is 6～20: 100, and the mass ratio of said comonomer and pigment is 2～5: 100, and surplus is a deionized water.
2. viscose rayon filament yarn fiber original liquid coloring according to claim 1 is characterized in that with the preparation method of superfine pigment mill base: said pigment is a kind of in carbon black, azo class pigment, phthalocyanine pigment, quinacridone pigments, thioindigo class pigment, triarylmethane compound pigment, anthraquinone pigment 、 dioxazines pigment and the quinophthalone class pigment.
3. viscose rayon filament yarn fiber original liquid coloring according to claim 1 is characterized in that with the preparation method of superfine pigment mill base: said polymerizable dispersion agent is at least a in allyloxy Nonylphenoxy propyl alcohol T 46155 ammonium sulfate, allyloxy hydroxypropyl azochlorosulfonate acid sodium, hydroxyethyl methacrylate propyl sulfonic acid sodium, methylacryoyloxyethyl hexadecyldimethyl benzyl ammonium brometo de amonio, methacrylate based quaternary ammonium salt and the methacrylate based bi-quaternary ammonium salt.
4. viscose rayon filament yarn fiber original liquid coloring according to claim 1 is characterized in that with the preparation method of superfine pigment mill base: said comonomer is at least a in vinylformic acid, methylacrylic acid, methyl acrylate, TEB 3K, Bing Xisuandingzhi, NSC 20956, vinylbenzene, vinylformic acid bay alcohol ester, vinyl cyanide, NMA, Hydroxyethyl acrylate, Rocryl 400, Propylene glycol monoacrylate, Rocryl 410, methylacrylic acid urea groups ester and the glycidyl acrylate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105086518A (en) * | 2015-07-27 | 2015-11-25 | 安徽明珠颜料科技有限公司 | Black iron oxide pigment containing bamboo charcoal powder and preparation method thereof |
| CN105111794A (en) * | 2015-07-27 | 2015-12-02 | 安徽明珠颜料科技有限公司 | Black iron oxide pigment containing tourmalinite powder and preparation method thereof |
| CN105131653A (en) * | 2015-07-25 | 2015-12-09 | 铜陵瑞莱科技有限公司 | Iron oxide black pigment used for printing ink and preparation method thereof |
| CN104327219B (en) * | 2014-08-27 | 2017-02-22 | 武汉持欣科技有限公司 | Aqueous emulsion for basic binder of adhesive for hard-bonding materials and preparation method thereof |
| CN107587204A (en) * | 2017-09-25 | 2018-01-16 | 浙江纳美新材料股份有限公司 | A kind of polyimides stoste colouring pigments dispersion and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103710772B (en) * | 2013-12-30 | 2015-09-23 | 苏州世名科技股份有限公司 | Fiber original liquid coloring superfine carbon black aqueous color paste |
| CN104327219B (en) * | 2014-08-27 | 2017-02-22 | 武汉持欣科技有限公司 | Aqueous emulsion for basic binder of adhesive for hard-bonding materials and preparation method thereof |
| CN105131653A (en) * | 2015-07-25 | 2015-12-09 | 铜陵瑞莱科技有限公司 | Iron oxide black pigment used for printing ink and preparation method thereof |
| CN105086518A (en) * | 2015-07-27 | 2015-11-25 | 安徽明珠颜料科技有限公司 | Black iron oxide pigment containing bamboo charcoal powder and preparation method thereof |
| CN105111794A (en) * | 2015-07-27 | 2015-12-02 | 安徽明珠颜料科技有限公司 | Black iron oxide pigment containing tourmalinite powder and preparation method thereof |
| CN107587204A (en) * | 2017-09-25 | 2018-01-16 | 浙江纳美新材料股份有限公司 | A kind of polyimides stoste colouring pigments dispersion and preparation method thereof |
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Application publication date: 20120718 |