CN1234924C - Cross blend resin in use for stainable in fine denier and fabrication method - Google Patents
Cross blend resin in use for stainable in fine denier and fabrication method Download PDFInfo
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- CN1234924C CN1234924C CN 200410017316 CN200410017316A CN1234924C CN 1234924 C CN1234924 C CN 1234924C CN 200410017316 CN200410017316 CN 200410017316 CN 200410017316 A CN200410017316 A CN 200410017316A CN 1234924 C CN1234924 C CN 1234924C
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Abstract
The present invention discloses resin for dying fine denier polypropylene fiber and blending and a manufacture method thereof. The resin for dying fine denier polypropylene fiber and blending comprises polypropylene resin and nanometer or/and submicron order rare earth particles. The resin contains 95 to 99q% of polypropylene and 1 to 5q% of rare earth particles. The rheological property of the modified polypropylene resin which is used in the present invention and is blended with submicron level and nanometer level rare earth particles is good, and the rare earth particles are evenly dispersed in the polypropylene. The size of nanometer level rare earth is evenly below 100 nm, and the monofilament finess of the fiber made by spinning is 0.3 to 1.2 fente. Intensity and toughness are obviously improved, and the resin can be dyed to a deep color by dispersion dye with a conventional method. Dye-uptake rate increases 30%. Dyeing performance is obviously improved, and the fiber has special functions of fluorescence, static electricity resistance, etc. because every rare earth elements has a specific electron layer structure to further enlarge the application field of polypropylene fiber.
Description
Technical field
The present invention relates to make the blending resin and the blend method thereof of dyeable polypropylene.
Background technology
The fiber that is made by plain polypropylene fails to obtain to use widely at garment industry because of bad performances such as stainability, hygroscopicity are relatively poor as taking fibrous material.In recent years, because with the thin dawn of special processing method production and the development of super fine denier (filament number is less than 1 dtex) polypropylene fibre, give the significant saturating wet perspiration discharging performance of polypropylene fabric and be widely used in underclothes, as high-grade sweater, underwear and spring and autumn clothing lining.
According to ZL 92,1,08576.1 report, controllable rheology acrylic resin and CDPET blending and modifyings such as (can dye, easily dye polyester) with the sex change of molecular-weight adjusting control polymer streams make its prepared fiber have the disperse dyes stainability.The polypropylene modified fiber filament number that makes is 0.3～1.2 dtex, thereby makes fabric have good wicking effect, wet perspire thoroughly, can be used as top grade and takes fibrous material.But the dyeing of the fiber of this invention manufacturing can only dye in dark partially, can not dye darkly, and with polypropene blended CDPET be organic matter, do not relate to inorganic matter.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of dyeable fine-denier polypropylene with blending resin and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
The said dyeable fine-denier polypropylene of the present invention comprises acrylic resin and nanometer with the component of blending resin or/and submicron order rare earth particle, and its mass percent is:
Polypropylene 95～99%, rare earth particle 1～5%
Nanometer is or/and the content of submicron order rare earth particle can not be too high, too highly will cause difficulty in spinning, can not be low excessively, and it is not obvious to cross low effect.
Said nanometer is or/and submicron order rare earth particle grain size is 20～900nm;
Said rare earth comprises cerium oxide and/or yittrium oxide;
Adopt conventional method, dyeable fine-denier polypropylene of the present invention can be made polypropylene modified fiber with blending resin, filament number is 0.3～1.2 dtex, and available disperse dyeing can be dyed to dark color.The fabric that is used to prepare not only has good wicking effect, wet perspire and stainability thoroughly, but also has fluorescence and antistatic etc. functional.
Because the rare earth particle is inorganic matter, less with polyacrylic compatibility, dyeable fine-denier polypropylene of the present invention can not adopt conventional method to be prepared with blending resin, after must handling earlier to the rare earth particle again with polypropene blended.Therefore, method of the present invention comprises the steps:
The rare earth particle is added nitric acid and hydrogen peroxide, stir to clarify, with ethanol is solvent, with polyvinylpyrrolidone with 1: 5～9 mass ratio under 50～90 ℃, reacted 2～60 minutes, will make rare earth organic complex again, then that above-mentioned complex compound and polypropylene is mixed, adopt conventional method, in melt blending in double screw extruder, and the granulation of system band.Blending extrudant is observed under ESEM, and the rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of rare earth particle is less than 0.9 micron;
Said rare earth particle is preferably submicron order, and promptly its particle diameter is 0.1～0.9um;
The weight ratio of rare earth particle and nitric acid and hydrogen peroxide is:
Rare earth particle: nitric acid: hydrogen peroxide=1: 1～20: 1～40;
The present invention is with rare earth particle and the complexing of polyvinylpyrrolidone hydridization, thereby the complex compound that makes is because organic existence has good compatibility with polypropylene;
Or comprise the steps:
With rare earth particle and silane coupler in organic solvent, temperature is to carry out surface treatment under 50～90 ℃ the condition, it can be disperseed in polypropylene equably, rare earth particle after will handling then and polypropylene are mixed, adopt conventional method, melt blending and the granulation of system band in double screw extruder.Blending extrudant is observed under ESEM, and the nano rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of nano rare earth particle is less than 100 nanometers.
Said rare earth particle is preferably nanoscale, and promptly its particle diameter is 20～100nm;
Said organic solvent comprises a kind of in ethanol, ethylene glycol, the cyclohexane;
Said silane coupler comprises the titanate esters of C5～C20, as metatitanic acid monooctyl ester etc.
The mass percent of its prescription is: nano rare earth particle 90～99.5%, finishing agent 0.5～10%.
With above-mentioned polypropylene modification resin slicer melt spinning, 800～3500 meters/minute spin under the speed, stretch 3～5 times between room temperature to 120 ℃, can make the fiber that filament number is 0.3～1.2 dtex, adopt dyer artistic skill commonly used to dye with DISPERSE DYES, but also have fluorescence and antistatic etc. functional to dark color.
The advantage of invention is very significant, compares prior art, and the present invention is good with the rheological characteristic of submicron order and nano-scale rare earth particle blended and modified polypropylene resin, rare earth particle being uniformly dispersed in polypropylene, and the nano-scale rare earth size is all below 100nm.Fibre single thread fiber number by its spinning is 0.3～1.2 dtex, intensity and toughness are improved significantly, adopt conventional method dyeing can dye with DISPERSE DYES to dark color, dye-uptake has improved 30%, because the particular electrical sublayer structure that rare earth element had, not only make its dyeability obtain obvious must the raising, and can make fiber have fluorescence and special function such as antistatic, further enlarged the Application Areas of polypropylene fibre.
Description of drawings
The stereoscan photograph of the blend sample that Fig. 1 makes for example 1, as can be seen from the figure, the size of rare earth particle is below 0.9um.
The stereoscan photograph of the blend sample that Fig. 2 makes for example 2, as can be seen from the figure, the size of rare earth particle is below 0.5um.
The stereoscan photograph of the blend sample that Fig. 3 makes for example 3, as can be seen from the figure, the size of rare earth particle is below 100nm.
The stereoscan photograph of the blend sample that Fig. 4 makes for example 4, as can be seen from the figure, the size of rare earth particle is below 100nm.
The stereoscan photograph of the blend sample that Fig. 5 makes for example 5, as can be seen from the figure, the size of rare earth particle is below 90nm.
The stereoscan photograph of the blend sample that Fig. 6 makes for example 6, as can be seen from the figure, the size of rare earth particle is below 90nm.
The specific embodiment
Embodiment 1
2.5 gram submicron order rare earth particles are added 15ml nitric acid and 30ml hydrogen peroxide, stir to clarify, with ethanol is solvent, reacted in 10 minutes with mass ratio stirring under 70 ℃ of 10: 90 with polyvinylpyrrolidone, to make rare earth organic complex again, with mass ratio 5: 95 with above-mentioned complex compound and polypropylene mixed after, under 220 ℃ in double screw extruder melt blending, and system band granulation.Blending extrudant is observed under ESEM, and the rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of rare earth particle is less than 0.9 micron.As Fig. 1.
Embodiment 2
2.5 gram submicron order rare earth particles adding 15ml nitric acid and 30ml hydrogen peroxide are stirred to clarify, with ethanol is solvent, reacted in 10 minutes with mass ratio stirring under 70 ℃ of 7: 93 with polyvinylpyrrolidone, to make rare earth organic complex again, with mass ratio 3: 97 with above-mentioned complex compound and polypropylene mixed after, under 220 ℃ in double screw extruder melt blending, and system band granulation.Blending extrudant is observed under ESEM, and the rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of rare earth particle is less than 0.5 micron.As Fig. 2.
Embodiment 3
2.5 gram submicron order rare earth particles adding 15ml nitric acid and 30ml hydrogen peroxide are stirred to clarify, with ethanol is solvent, reacted in 10 minutes with the stirring under 70 ℃ of 3: 97 mass ratio of polyvinylpyrrolidone, to make rare earth organic complex again, with mass ratio 1: 99 with above-mentioned complex compound and polypropylene mixed after, under 220 ℃ in double screw extruder melt blending, and system band granulation.Blending extrudant is observed under ESEM, and the rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of rare earth particle is less than 100 nanometers.As Fig. 3.
Embodiment 4
Is 8: 92 with nano rare earth particle and silane coupler (trimethoxy silane) at mass ratio, absolute ethyl alcohol is a solvent, temperature is to carry out surface treatment under the condition about 78 ℃, nano rare earth particle after will handling then is mixed with 5: 95 mass ratio and polypropylene, melt blending and the granulation of system band in double screw extruder under 220 ℃.Blending extrudant is observed under ESEM, and the nano rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of nano rare earth particle is less than 100 nanometers.As Fig. 4.
Embodiment 5
Is 8: 92 with nano rare earth particle and titanate coupling agent (butyl titanate) at mass ratio, absolute ethyl alcohol is a solvent, temperature is to carry out surface treatment under the condition about 78 ℃, nano rare earth particle after will handling then is mixed with 3: 97 mass ratio and polypropylene, melt blending and the granulation of system band in double screw extruder under 220 ℃.Blending extrudant is observed under ESEM, and the nano rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of nano rare earth particle is less than 90 nanometers.As Fig. 5.
Embodiment 6
Is 3: 97 with nano rare earth particle and titanate coupling agent (butyl titanate) at mass ratio, absolute ethyl alcohol is a solvent, temperature is to carry out surface treatment under the condition about 78 ℃, nano rare earth particle after will handling then is mixed with 1: 99 mass ratio and polypropylene, melt blending and the granulation of system band in double screw extruder under 220 ℃.Blending extrudant is observed under ESEM, and the nano rare earth particle is uniformly dispersed in polypropylene, and the maximum particle diameter of nano rare earth particle is less than 90 nanometers.As Fig. 6.
Embodiment 7
Adopt the preparation of product fiber of embodiment 1, its filament number was 1 dawn, and fracture strength is 3cn/dex.Adopt DISPERSE DYES under 120 ℃ temperature, 60min dyes on high temperature-pressure dyeing machine.Dyeing and finishing technology according to the salty edge of gold is learned the method for experimentally measuring dye-uptake, measures its dye-uptake on spectrophotometer, and dye-uptake has improved 30%.
Claims (4)
1. a dyeable fine-denier polypropylene blending resin is characterized in that, or/and submicron order rare earth particle is formed, its mass percent is by acrylic resin and nanometer:
Polypropylene 95～99%, rare earth particle 1～5%;
Said nanometer is or/and submicron order rare earth particle grain size is 20～900nm;
Said rare earth is cerium oxide and/or yittrium oxide;
Said cerium oxide or yttria particles are cerium oxide or the yttria particles with the complexing of polyvinylpyrrolidone hydridization, or through coupling agent surface-treated cerium oxide or yttria particles.
2. dyeable fine-denier polypropylene according to claim 1 is characterized in that comprising the steps: with the preparation method of blending resin
The rare earth particle is added nitric acid and hydrogen peroxide, is solvent with ethanol, with polyvinylpyrrolidone with 1: 5～9 mass ratio under 50～90 ℃, reacted 2～60 minutes, and made rare earth organic complex, then that above-mentioned complex compound and polypropylene is mixed, adopt conventional method, extrude blend, granulation.
3. method according to claim 2 is characterized in that, said rare earth particle is a submicron order, and promptly its particle diameter is 0.1～0.9um.
4. method according to claim 2 is characterized in that, the weight ratio of rare earth particle and nitric acid and hydrogen peroxide is:
Rare earth particle: nitric acid: hydrogen peroxide=1: 1～20: 1～40.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017316 CN1234924C (en) | 2004-03-30 | 2004-03-30 | Cross blend resin in use for stainable in fine denier and fabrication method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017316 CN1234924C (en) | 2004-03-30 | 2004-03-30 | Cross blend resin in use for stainable in fine denier and fabrication method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1563528A CN1563528A (en) | 2005-01-12 |
| CN1234924C true CN1234924C (en) | 2006-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410017316 Expired - Fee Related CN1234924C (en) | 2004-03-30 | 2004-03-30 | Cross blend resin in use for stainable in fine denier and fabrication method |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390335C (en) * | 2005-03-10 | 2008-05-28 | 中国科学院化学研究所 | Polymer compounding fiber composed by surface-modified, inorganic filler and polymer |
| CN100360737C (en) * | 2006-02-13 | 2008-01-09 | 上海金霞化纤有限公司 | Dyeing method of ion exchanging dyeable fine denier poly propylene fiber |
| CN100414039C (en) * | 2006-02-13 | 2008-08-27 | 上海金霞化纤有限公司 | Method for dyeing rare-earth modified polyolefine and polypropylene blended thin Denier yarns |
| CN101922060B (en) * | 2010-09-01 | 2012-07-04 | 青岛大学 | Method for preparing rare earth fluorescence micro/nano fibers |
| CN102691127B (en) * | 2012-06-08 | 2014-04-02 | 上海大学 | Ionic nano particle blending modified dyeable fine-denier polypropylene and preparation method thereof |
| 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 |
| CN108796656A (en) * | 2018-07-06 | 2018-11-13 | 上海曙雀贸易有限公司 | A kind of high-performance of dopen Nano yttrium oxide is anti-fake, can trace to the source yarn |
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