CN1818203A - Method for dyeing rare-earth modified polyolefine and polypropylene blended thin Denier yarns - Google Patents
Method for dyeing rare-earth modified polyolefine and polypropylene blended thin Denier yarns Download PDFInfo
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Abstract
A dyeing method including such steps as pre-dyeing treatment with lotion and calcined soda, high temperature dyeing with mixture of disperse dyes and acetic acid, and post treatment by cleaning loose colour. We screen for red, yellow and blue colors that fit for disperse dyes by comparing building up properties, light fastness, rubbing fastness and washing fastness of disperse dyes. This method can increase dye-uptake rate, color brightness, evenness degree and color fastness.
Description
Technical field
The present invention relates to the colouring method of fine-denier polypropylene, be specifically related to contain the colouring method of the fine-denier polypropylene of rare earth material in-situ polymerization improved polyalkene and polypropene blended resins.
Background technology
Polypropylene fibre is because raw material sources are abundant, makes simply, cheap, thereby development is quite rapid, has a lot of good characteristics, has obtained application widely in industry and daily life.Because the succeeding in developing of fine denier polypropylene fibers, it is found that fine denier polypropylene fibers has unique hydrophobic wet effect of leading, the underwear of making dress is smooth, comfortable.But the nonpolar structure of polypropylene fibre, there is not the polar group that can combine in its molecule with any dye molecule, and the degree of crystallinity of polypropylene fibre is very high, structure is tight, the inner essential hole of dye diffusion that lacks, hydrophobicity is very remarkable, thereby dye molecule can only spread or be penetrated into the unformed area of fiber molecule, and can not enter the crystalline region.Therefore, general at present dyestuff commonly used can not make dyeing polypropylene fibers (comprising DISPERSE DYES).As taking textile material, the colouring problem of polypropylene fibre is that polypropylene fibre further develops middle urgent problem.
People are carrying out number of research projects around the colouring problem that how to solve polypropylene fibre aspect dyeing, block copolymerization and grafting, copolymerization and modification polypropylene fibre, low molecular compound (metallic compound) modified polypropylene fiber and the high polymer blended and modified polypropylene fiber of unmodified polypropylene fiber.Wherein, the high polymer blending and modifying should be the effective way that improves polypropylene fibre stainability energy.Patent CN1339623A discloses a kind of preparation of resin specially for dyable fine denier polypropylene fibre, (the TPO derivative of the polyolefine material and 0～3% (by weight) of the polypropylene material of) spinned fine count fiber, 2～20% (by weight) carries out binary or the modification of ternary melt blending under 200～280 ℃ temperature by weight, and the finished product that makes can spin the fine-denier polypropylene of available common disperse dye dyeable with 77～98%.But because the TPO material and the TPO derivative polarity that add are lower, and the affinity between DISPERSE DYES a little less than, thereby soaping fastness is not ideal enough in the actual dyeing, in particularly dying when dark.
DISPERSE DYES is that molecule is smaller, and not with the dyestuff of water soluble group, chromatogram is complete on the structure, now is widely used in dying synthetic fiber such as polyester and acetate fiber.Patent CA1264443A is based on obtaining best Color, the DISPERSE DYES of fastness that selective aggregation is good, good (rub resistance, water-fastly wash, sun-resistant etc.) and high K/S value, and these DISPERSE DYES are combined, make it to play a role with its Cmax before fading the dyestuff friction occurring.It is said that this patent can under atmospheric pressure make polypropylene fibre dye reliably, and the fiber of dyeing shows good fastness.But since blending and modifying after the polypropylene fibre internal structure and and DISPERSE DYES between the effect mechanism variation has taken place, some variations also will take place in the DISPERSE DYES of mentioning in the redness of mentioning in this Patent right requirement, yellow and the blue primaries family.
Adopt the rare earth material in-situ hybridization of surface modification to participate in polyolefinic polymerization, be a kind of fine denier dyeable polypropylene fibre that industrial prospect is arranged very much then with polypropene blended preparation fine denier dyeable polypropylene fibre blending resin, both can realize the even dispersion of inorganic nano-particle in high polymer in this resin, keep the nano-meter characteristic of particle simultaneously again.And for this novel fine denier dyeable polypropylene fibre, still there is not well-content colouring method at present, need screen DISPERSE DYES again according to the aggregation of dyestuff, fastness (rub resistance, water-fastly wash, sun-resistant etc.) and K/S value, colouring method is analyzed and studied, to realize the suitability for industrialized production of this fine denier dyeable polypropylene fibre.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of colouring method that contains rare earth material improved polyalkene and polypropene blended fine-denier polypropylene, to satisfy need of industrial production.
Said rare earth material improved polyalkene and the polypropene blended fine-denier polypropylene of containing, be to contain the improved polyalkene of rare earth material and the resin of polypropene blended acquisition, through melt spinning, stretching, the filament number that is obtained is the fiber of 0.9～2dtex, wherein, the weight content that contains the rare earth material improved polyalkene is 2～8%, the polypropylene weight content is 92～98%, contain in the rare earth material improved polyalkene, the rare earth material weight content is 7.5～12.5%, and the improved polyalkene weight content is 87.5～92.5%;
The said rare earth material modified poly preparation of polyolefins method that contains comprises the steps:
At 70～75 ℃, with Na
2S
2O
3Add the aqueous solution that contains dispersant, add mixture then through nano rare earth particle, initator and the modified olefin monomer of finishing, 70～80 ℃ were reacted 50～70 minutes down, were warming up to 81～85 ℃ of reactions 80～100 minutes, continued to be warming up to 86～90 ℃ of reactions 80～100 minutes, be warming up to 91～96 ℃ at last, particle sclerosis 100～140 minutes, the hybrid particle of acquisition slaking, washing, oven dry obtains to contain the rare earth material improved polyalkene;
And then mix with polypropylene, melt blending is extruded, and obtain to contain rare earth material modified poly polyolefin and become fiberized resin with polypropene blended fine count fiber special use, through melt spinning, stretching, the fiber that obtains, filament number is 0.9～2dtex;
To contain rare earth material improved polyalkene and polypropene blended fine-denier polypropylene gross weight, the weight that contains the rare earth material improved polyalkene is 2～8%, and polyacrylic weight is 92～98%;
Said dispersant is selected from a kind of in polyvinyl alcohol, polyacrylic acid, poly-methyl acrylate or maleic anhydride one styrol copolymer, contains in the aqueous solution of dispersant, and the content of dispersant is 0.01～0.04 grams per milliliter;
Na
2S
2O
3Addition be 0.0005～0.001 grams per milliliter aqueous solution;
The addition of the nano rare earth particle of process finishing is 0.03～0.05 grams per milliliter aqueous solution;
The addition of initator is 0.002～0.006 grams per milliliter aqueous solution;
The addition of modified olefin monomer is 0.3～0.5 grams per milliliter aqueous solution;
Said initator is selected from dibenzoyl peroxide (BPO), azodiisobutyronitrile (AIBN), potassium peroxydisulfate (K
2S
2O
8) or the peroxycarbonates class in a kind of;
Said improved polyalkene prepares according to (original position) suspension polymerization basic skills, as " Blends of Polypropylene and Modified Polystyrene for Dyeable Fibers " document disclosed methods such as Huang Xin, be a kind of polyolefin that contains the benzene ring structure unit, general structure is:
Formula 1
In the formula, preferred R is selected from H or CH
3In a kind of; M=1,2,3 or 4, n=180～720;
Said nano rare earth particle through finishing can adopt precious letter of seat etc., and " stearic acid is to CeO
2The Study on surface-modification of nano particle " disclosed method is prepared, and is a kind of nano rare earth particle that adopts coupling agent or surfactant processing;
Said rare earth is selected from cerium oxide, yittrium oxide or urania; The average grain diameter of nano rare earth particle is 50～100 nanometers;
The said colouring method that contains rare earth material polyolefin and polypropene blended fine denier dyeable polypropylene fibre of the present invention comprises the steps:
(1) contains the rare earth material improved polyalkene and polypropene blended fine-denier polypropylene places dye bath with said, according to bath raio is 1: after the weight ratio of 15-30 adds water, add the detergent that deoils of blend fine denier dyeable polypropylene fibre weight 1.0-3.0%, the soda ash of 0.5-3.0%, be warmed up to 70-85 ℃, insulation 20-40min;
(2) add DISPERSE DYES and acetic acid, 10-20min turns round after being warmed up to 50-60 ℃ with the speed of 2～4 ℃/min;
The addition of DISPERSE DYES determines that according to the color matching needs in blend fine denier dyeable polypropylene fibre weight, preferred addition is greater than 0 to 5%, and the acetic acid addition is the 0.5-2.0% of blend fine denier dyeable polypropylene fibre weight;
(3) speed with 1～2 ℃/min is warmed up to 90～120 ℃, dye shallow in during look, temperature is 90-100 ℃, when dark, temperature is 100-120 ℃, running 30-60min in dying;
(4) discharge water the clear water washing after dropping to 80～90 ℃ with the speed of 2～4 ℃/min;
Further, dye the back fine-denier polypropylene and will handle the removal loose colour, for tinctorial pattern product in shallow, by bath raio 1: 15-30 adds water, adds the soaping agent of blend fine denier dyeable polypropylene fibre weight 0-1.0%, is warmed up to the 50-70 ℃ of 20～40min that turns round, and clear water washs; For middle dark sample, by bath raio 1: 15-30 adds water, adds the soaping agent of blend fine denier dyeable polypropylene fibre weight 1.0-3.0%, is warmed up to 60-90 ℃ of running 20～40min, the clear water washing;
Term " look in shallow ", " middle dark color " all have clear and definite definition in Chen Guanlong " standards for dyeing degree of depth colour atla " document.
Said soaping agent is selected from polyacrylic acid sodium salt or modified phosphate, can adopt the commercially available prod, as the soap flakes of the refreshing High Seience Technology Co., Ltd. of the clean that in Beijing, Shandong generation dragon chemical industry Co., Ltd and vapour Bagong department;
The said detergent that deoils is selected from fatty alcohol-polyoxyethylene ether, polyoxyethylene phenolic ether or alkylphenol polyoxyethylene, can adopt the commercially available prod, be the deoil product of yarn agent LD-22 of special efficacy as clean your the refreshing High Seience Technology Co., Ltd. in Beijing and the Shandong generation dragon chemical industry Co., Ltd trade mark;
Adopt said method, the DISPERSE DYES dye-uptake is greatly improved, and the colour brightness of coloured fibre, the uniformity and COLOR FASTNESS are good.
The present invention requires aggregation, fastness (rub resistance, water-fastly wash, sun-resistant etc.) and the K/S value according to dyestuff that commercially available DISPERSE DYES is screened, and finds out redness, yellow and the blue primaries family of DISPERSE DYES.Adopt selected one or more admixture of disperse dyes and dyeing course of the present invention, not only the DISPERSE DYES dye-uptake can be greatly improved, and bright color after being dyed degree, the uniformity and COLOR FASTNESS are all better.
The specific embodiment
Embodiment 1
Contain the preparation of rare earth material improved polyalkene and polypropene blended fine denier dyeable polypropylene fibre
In the 250ml there-necked flask, add 100ml absolute ethyl alcohol, 10 gram Y
2O
3Nano-powder and with respect to Y
2O
3The titanate coupling agent of the C15 of nano-powder quality 8%.Then will be at the Y of 100 ℃ of following dry 2h
2O
3Nano particle adds in the flask gradually, and 25 ℃ of sonic oscillations also stir 30min simultaneously.After vibration finishes, heated constant temperature backflow 4h in 80 ℃ cleansing bath tub.
Y with the above-mentioned finishing of 6 grams
2O
3After the ultrasonic dispersion of mixing suspension of nano particle together with 0.7 gram dibenzoyl peroxide (BPO) and 80 gram modified olefin monomers, add 4 grams and be dissolved with polyethylene of dispersing agent alcohol (PVA) and 0.2 gram Na
2S
2O
3250 ml deionized water in, at 75 ℃ of reaction 1h, be warming up to 80 ℃ of reaction 1.5h, be warming up to 90 ℃ of reaction 1.5h, be warming up to 95 ℃, particle sclerosis 2h.
The general structure of said improved polyalkene is suc as formula 1, and wherein, R is H, m=1, n=360.
Above-mentioned hybrid modification polyolefin additive that will make at last and polypropylene with 6: 94 mass ratio in 220 ℃ of melt blendings in double screw extruder, granulation.
Through 250 ℃ of melt spinnings,,, can obtain the fiber that filament number is 1dtex in 3 times of 80 ℃ of stretchings 1000 meters/minute spin under the speed.
Embodiment 2
The fiber of raw material: embodiment 1
With following method fiber sample is dyed light red.
Whole dyeing course comprises and dyes pre-treatment successively, dyes, dyes post-treating and other steps.Dye in the pre-treatment process, the fine-denier polypropylene that makes is added water by bath raio at 1: 20 after, add the special efficacy yarn agent LD-22 that deoils, addition is 3.0% of a fine-denier polypropylene weight, soda ash 3.0% is warmed up to 85 ℃, insulation 40min.After will dying fiber after the pre-treatment and adding water at 1: 20 with bath raio, add the disperse red E-4B (disperse red 60) of fine-denier polypropylene weight 0.1%, the acetic acid addition is 0.7% of a fine-denier polypropylene weight.15min turns round after being warmed up to 50 ℃ with 3 ℃/min.Be warmed up to definite temperature with 1.5 ℃/min subsequently, the temperature of dying shallow middle look is 100 ℃.After running 40min, discharge water after dropping to 90 ℃ with 3 ℃/min, clear water is washed 2 times.Dye the back fine-denier polypropylene and will dye post processing removal loose colour, for tinctorial pattern product in shallow, add water at 1: 30 by bath raio, be warmed up to 60 ℃ of running 30min, clear water is washed 2 times afterwards, and final drying is dyed fiber.Adopt the method for Xu Muqing " printing and dyeing examination chemical examination " document, GB/T 3920-1997, GB/T3921.1～5-1997, GB/T 3922-1995 and GB/T 8424.1～3-2001 document specifies to detect, its result is as follows:
| The dyestuff dye-uptake | Colour brightness | The color and luster uniformity | Crock fastness | Soaping fastness | Perspiration fastness | |||
| Do | Wet | The former state variable color | Calico staining | The former state variable color | Calico staining | |||
| 90％ | Bright in colour | Color and luster is even | 4-5 | 4-5 | 3-4 | 4-5 | 3-4 | 4 |
Embodiment 3
Adopt the identical method of embodiment 1, preparation cerium oxide improved polyalkene and polypropene blended fine denier dyeable polypropylene fibre, cerium oxide improved polyalkene and polyacrylic weight ratio are 6: 94, filament number is 2dtex, with following method fiber sample is dyed blueness.
Whole dyeing course comprises and dyes pre-treatment successively, dyes, dyes post-treating and other steps.Dye in the pre-treatment process, the fine-denier polypropylene that makes is added water by bath raio at 1: 20 after, the special efficacy yarn agent LD-22 that deoils, addition is 2.0%, soda ash 1.5% is warmed up to 75 ℃, insulation 30min.After will dying fiber after the pre-treatment and adding water at 1: 20 with bath raio, add Terasil Navy Blue GRL-C (Disperse Blue-79) 1%, the acetic acid addition is 1.0%.15min turns round after being warmed up to 50 ℃ with 3 ℃/min.Be warmed up to definite temperature with 1.5 ℃/min subsequently, the temperature of dying shallow middle look is 100 ℃.After running 60min, discharge water after dropping to 90 ℃ with 3 ℃/min, clear water is washed 2 times.Dye the back fine-denier polypropylene and will dye post processing removal loose colour, add water at 1: 30 by bath raio, add soap flakes 0.5%, be warmed up to 60 ℃ of running 30min, clear water is washed 3 times afterwards, and final drying is dyed fiber.Adopt the method for Xu Muqing " printing and dyeing examination chemical examination " document, GB/T3920-1997, GB/T 3921.1～5-1997, GB/T 3922-1995 and GB/T 8424.1～3-2001 document specifies to detect, its result is as follows:
| The dyestuff dye-uptake | Colour brightness | The color and luster uniformity | Crock fastness | Soaping fastness | Perspiration fastness | |||
| Do | Wet | The former state variable color | Calico staining | The former state variable color | Calico staining | |||
| 85％ | Bright in colour | Color and luster is even | 4 | 4 | 4 | 4 | 4 | 4 |
Embodiment 4
The fiber of raw material: embodiment 1, filament number are 2dtex, with following method with the fiber sample red colouration.
Whole dyeing course comprises and dyes pre-treatment successively, dyes, dyes post-treating and other steps.Dye in the pre-treatment process, the fine-denier polypropylene that makes is added water by bath raio at 1: 20 after, the special efficacy yarn agent LD-22 that deoils, addition is 1.0%, soda ash 1.0% is warmed up to 75 ℃, insulation 30min.After will dying fiber after the pre-treatment and adding water at 1: 20 with bath raio, add disperse red E-4B (disperse red 60) 2.5%, the acetic acid addition is 2.0%.15min turns round after being warmed up to 50 ℃ with 3 ℃/min.Be warmed up to definite temperature with 1.5 ℃/min subsequently, the temperature of dying shallow middle look is 100 ℃.After running 60min, discharge water after dropping to 90 ℃ with 3 ℃/min, clear water is washed 2 times.Dye the back fine-denier polypropylene and will dye post processing removal loose colour, for tinctorial pattern product in shallow, add water at 1: 30 by bath raio, add soap flakes 1.5%, be warmed up to 60 ℃ of running 30min, clear water is washed 4 times afterwards, and final drying is dyed fiber.Adopt the method for Xu Muqing " printing and dyeing examination chemical examination " document, GB/T 3920-1997, GB/T 3921.1～5-1997, GB/T 3922-1995 and GB/T 8424.1～3-2001 document specifies to detect, its result is as follows:
| The dyestuff dye-uptake | Colour brightness | The color and luster uniformity | Crock fastness | Soaping fastness | Perspiration fastness | |||
| Do | Wet | The former state variable color | Calico staining | The former state variable color | Calico staining | |||
| 80％ | Bright in colour | Color and luster is even | 4 | 3-4 | 4 | 3-4 | 4 | 4 |
Embodiment 5
The fiber of raw material: embodiment 3, filament number are 2dtex, with following method with the fiber sample yellow colouration.
Whole dyeing course comprises and dyes pre-treatment successively, dyes, dyes post-treating and other steps.Dye in the pre-treatment process, the fine-denier polypropylene that makes is added water by bath raio at 1: 20 after, the special efficacy yarn agent LD-22 that deoils, addition is 1.0%, soda ash 0.5% is warmed up to 75 ℃, insulation 30min.After will dying fiber after the pre-treatment and adding water at 1: 20, add and disperse golden yellow E-3RL (disperse yellow 23) 4.5% with bath raio, disperse red E-4B (disperse red 60) 0.5%, the acetic acid addition is 2.0%.15min turns round after being warmed up to 50 ℃ with 3 ℃/min.Be warmed up to 120 ℃ with 1.5 ℃/min subsequently.After running 60min, discharge water after dropping to 90 ℃ with 3 ℃/min, clear water is washed 2 times.Dye the back fine-denier polypropylene and will dye post processing removal loose colour, for tinctorial pattern product in shallow, add water at 1: 30 by bath raio, add soap flakes 3.0%, be warmed up to 70 ℃ of running 30min, clear water is washed 5 times afterwards, and final drying is dyed fiber.Adopt the method for Xu Muqing " printing and dyeing examination chemical examination " document, GB/T 3920-1997, GB/T 3921.1～5-1997, GB/T 3922-1995 and GB/T8424.1～3-2001 document specifies to detect, its result is as follows:
。
| The dyestuff dye-uptake | Colour brightness | The color and luster uniformity | Crock fastness | Soaping fastness | Perspiration fastness | |||
| Do | Wet | The former state variable color | Calico staining | The former state variable color | Calico staining | |||
| 65％ | Bright in colour | Color and luster is even | 3-4 | 3 | 4 | 3 | 4 | 3-4 |
Claims (7)
1. a colouring method that contains rare earth material improved polyalkene and polypropene blended fine-denier polypropylene is characterized in that, comprises the steps:
(1) will contain the rare earth material improved polyalkene and polypropene blended fine-denier polypropylene places dye bath, according to bath raio is 1: after the weight ratio of 15-30 adds water, add the detergent that deoils of blend fine-denier polypropylene weight 1.0-3.0%, the soda ash of 0.5-3.0%, be warmed up to 70-85 ℃, insulation 20-40min;
(2) add DISPERSE DYES and acetic acid, 10-20min turns round after being warmed up to 50-60 ℃ with the speed of 2～4 ℃/min;
The addition of DISPERSE DYES determines that according to the color matching needs acetic acid addition is the 0.5-2.0% of blend fine-denier polypropylene weight;
(3) speed with 1～2 ℃/min is warmed up to 90～120 ℃, running 30-60min;
(4) discharge water the clear water washing after dropping to 80～90 ℃ with the speed of 2～4 ℃/min.
2. method according to claim 1 is characterized in that, in blend fine-denier polypropylene weight, the addition of DISPERSE DYES is greater than 0 to 5%.
3. method according to claim 1 is characterized in that, step (3) dye shallow in during look, temperature is 90-100 ℃.
4. method according to claim 1 is characterized in that, when dark, temperature was 100-120 ℃ during step (3) was dyed.
5. method according to claim 1 is characterized in that, dyes the back fine-denier polypropylene and handles the removal loose colour.
6. according to each described method of claim 1～5, it is characterized in that, said rare earth material improved polyalkene and the polypropene blended fine-denier polypropylene of containing, be to contain the improved polyalkene of rare earth material and the resin of polypropene blended acquisition, through melt spinning, stretch, the filament number that is obtained is the fiber of 0.9～2dtex, wherein, the weight content that contains the rare earth material improved polyalkene is 2～8%, the polypropylene weight content is 92～98%, contain in the rare earth material improved polyalkene, the rare earth material weight content is 7.5～12.5%, and the improved polyalkene weight content is 87.5～92.5%; The general structure of said improved polyalkene is:
Formula 1
In the formula, R is selected from H or CH
3In a kind of; M=1,2,3 or 4, n=180～720.
7. method according to claim 6 is characterized in that said rare earth is selected from cerium oxide, yittrium oxide or urania.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469628A (en) * | 2013-09-16 | 2013-12-25 | 上海大学 | Method for dyeing polyether type high-hydrophilicity polyester fiber |
| CN106868886A (en) * | 2016-12-22 | 2017-06-20 | 马鞍山市鑫程纳米新材料科技有限公司 | A kind of acrylic resin non-woven fabrics painting methods |
| CN107268102A (en) * | 2017-08-01 | 2017-10-20 | 合肥梵清电子商务有限公司 | A kind of manufacturing process of fine-denier polypropylene chopped fiber |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5468259A (en) * | 1992-12-07 | 1995-11-21 | Sheth; Paresh J. | Dyeable polyolefin compositions and dyeing polyolefin compositions |
| US5447539A (en) * | 1994-02-10 | 1995-09-05 | Dke Incorporated | Method of dyeing polypropylene fiber with more than one color |
| AU690997B2 (en) * | 1994-06-07 | 1998-05-07 | Equistar Chemicals, Lp | Dyeable polyolefin compositions and method |
| CN1114727C (en) * | 2000-08-23 | 2003-07-16 | 东华大学 | Preparation of resin specially for dyable fine denier polypropylene fibre |
| JP2002080608A (en) * | 2000-09-06 | 2002-03-19 | Kenji Murakami | Method for dyeing polyolefin resin |
| CN1234924C (en) * | 2004-03-30 | 2006-01-04 | 东华大学 | Cross blend resin in use for stainable in fine denier and fabrication method |
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2006
- 2006-02-13 CN CNB2006100238439A patent/CN100414039C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469628A (en) * | 2013-09-16 | 2013-12-25 | 上海大学 | Method for dyeing polyether type high-hydrophilicity polyester fiber |
| CN106868886A (en) * | 2016-12-22 | 2017-06-20 | 马鞍山市鑫程纳米新材料科技有限公司 | A kind of acrylic resin non-woven fabrics painting methods |
| CN107268102A (en) * | 2017-08-01 | 2017-10-20 | 合肥梵清电子商务有限公司 | A kind of manufacturing process of fine-denier polypropylene chopped fiber |
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