CN102675628A - High-speed spinning bright nylon 6 slice and manufacturing method thereof - Google Patents
High-speed spinning bright nylon 6 slice and manufacturing method thereof Download PDFInfo
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- CN102675628A CN102675628A CN2012101234159A CN201210123415A CN102675628A CN 102675628 A CN102675628 A CN 102675628A CN 2012101234159 A CN2012101234159 A CN 2012101234159A CN 201210123415 A CN201210123415 A CN 201210123415A CN 102675628 A CN102675628 A CN 102675628A
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Abstract
The invention relates to a high-speed spinning bright nylon 6 slice and a manufacturing method thereof, belongs to the field of polymer synthesis and modification and is particularly suitable for spinning a nylon 6 bright yarn at a high speed. The invention aims to research and develop a slice which contains no delustering agent and can be used for spinning the nylon yarn with a special-shaped section at a high speed. The high-speed spinning bright nylon 6 slice has excellent spinnability, can also reach the satisfactory full-package rate at a high speed and is particularly suitable for spinning the bright nylon 6 yarn at a high speed. The high-speed spinning bright nylon 6 slice is generated by polymerizing the following components in percentage by weight: 105-115 percent of caprolactam, 0.001-0.1 percent of surface treatment barium sulfate, 0.2-2 percent of molecular weight regulator and 0.05-0.5 percent of light stabilizer. Through the bright nylon 6 slice, the spinning defect of the existing bright nylon 6 slice is overcome; and the bright nylon 6 slice has excellent spinnability, can also reach the satisfactory full-package rate at a high speed and is particularly suitable for spinning the bright yarn at a high speed.
Description
Technical field
The nylon 6 that the present invention relates to a kind of high speed spinning has light section and method of manufacture thereof, belongs to the synthetic and modification field of polymkeric substance, is specially adapted to high-speed spinning nylon 6 bright yarns.
Background technology
One of them trend of chemical fibre textile technical development improves constantly spinning speed exactly.The melt of the important kind nylon 6 fiber of chemical fibre spins speed from beginning PM hundreds of rice, has developed into several kms of PM.The conspicuous benefit of high speed spinning is significantly to enhance productivity, and reduces unit cost, and the fiber of its production to have a physical stability qualitative higher, be fit to add the advantage of aftertreatments such as bullet, thereby extensively adopted.Nylon 6 high speed spinnings require highly to spinning material section, and viscosity, moisture content, oligomer, and inorganic additives content, homogeneity, dispersiveness and some other factors all can influence the process of spinning and the character of fiber.
Be to improve the spinning speed of nylon 6, Chinese patent CN93108287.0 has proposed a kind of high-speed spinning filament yarn based on polycaprolactam and preparation method thereof, its relative viscosity RV is 2.0-3.0, and at least a di-carboxylic acid exists and is prepared from down.Add di-carboxylic acid and stablize the nylon 6 slice that melt quality is produced suitable high-speed spinning, but in fact only just be prone to realize in this quadrat method industry at the matting agent TO2 that is added with certain limit.The half delustring section of adding a small amount of matting agent is a nylon raw fiber the most widely; Realized stable high speed spinning the earliest, the full-dull section of adding a large amount of matting agents then is to have realized also that after having solved a large amount of matting agent dispersion problems higher stable spins speed.Non-additive then still not ideal enough when having light section to be used for high-speed spinning.
Transparent nylon silk with special crosssection can present glittering gloss and be called as bright yarn through light refraction, can produce various linings with unique flash of light color and luster.At present the bright yarn of the nylon nylon that does not contain matting agent commonly used has light section spinning to form, and does not have the light section that has of matting agent can be in the lower spinning under the speed of spinning, but not ideal enough when being used for high-speed spinning.Major cause is the transparent effect that reaches good for asking, and has light section can not add TiO2, so the silk face is very smooth during spinning; Just many with the Silk Road and mutual contact area; And add that mostly bright yarn is shaped filaments, also more like the contact area of the more common cylindrical wire of trilobal cross, trilateral, so frictional force is higher; The electrostatic interaction of supervening simultaneously all produces negative influence to spinning, is prone to produce lousiness, fracture of wire.Therefore conventional have the light section to spin shaped filaments, the particularly shaped filaments at thin dawn can only to take the lower speed of spinning, the requirement that does not reach high speed spinning.
A way that can solve the frictional force problem is the most current present matting agents such as interpolation titanium oxide; The matting agent particle can produce projection on the surface; Reduce frictional force and then can carry out the high speed spinning, thereby half matt nylon chip spinning velocity-stabilization of high-speed spinning level can reach more than the 4500m/min.But for the bright yarn of glittering style, this type of has the additive of photoextinction obviously can not to add titanium oxide etc., even if the titanium oxide of trace also can produce negative influence to the glittering gloss of silk.
Chinese patent CN200810025150.2, the patent of " a kind of special-shaped monofilament section and working method thereof " by name has been described a kind of nylon 6 special-shaped monofilament sections and working method thereof.Specifically, be section and the working method thereof that is used for producing special-shaped monofilament.It is to process special-shaped monofilament section with raw materials such as hexanolactam, permanent white, phenylformic acid and vaal waters through polymerization.Use this special-shaped monofilament section, spinning quality is better.But should specially invent the section of being produced mainly is to be used for the section of monofilament abnormity.
Summary of the invention
A kind of high speed spinning that the present invention proposes light nylon 6 slice and method of manufacture thereof arranged, its objective is a kind of section that can be used for high-speed spinning special crosssection nylon wire of not having matting agent of development.It possesses excellent spinning property, is also reaching gratifying full-rolling rate down high-speed, and what be specially adapted to high-speed spinning has 6 of light nylon.
A kind of high speed spinning the light nylon 6 slice arranged, generate by following component polymerization:
Hexanolactam, permanent white, molecular weight regulator and photostabilizer; Its weight percent is:
Hexanolactam 105 ~ 115%,
Surface treatment permanent white 0.001 ~ 0.1%,
Molecular weight regulator 0.2 ~ 2%,
Photostabilizer 0.05 ~ 0.5%.
Above-mentioned a kind of high speed spinning the light nylon 6 slice arranged; Be that said molecular weight regulator is C2 ~ C18 straight chained alkyl or C4 ~ C8 naphthenic base, C6 ~ C24 aromatic dicarboxylic acid, any one in C4 ~ C20 straight chained alkyl, C4 ~ C8 naphthenic base, the C6 ~ C24 aromatic diamine.
Above-mentioned a kind of high speed spinning the light nylon 6 slice arranged, be that said photostabilizer is a 4-carboxyl-2,2,6,6 ,-tetramethyl piperidine or 4-are amino-2,2,6,6 ,-tetramethyl piperidine.
Above-mentioned a kind of high speed spinning the light nylon 6 slice arranged, be that the surface treatment agent of described permanent white is: a kind of in silane coupling agent or tensio-active agent, titanate coupling agent, the aluminate coupling agent.
The particle size range of the permanent white powder of described surface treatment permanent white is 0.1 ~ 0.6um.
A kind of method of manufacture that the light nylon 6 slice is arranged of high speed spinning comprises that the following step gathers:
One, the preparation of permanent white dispersion liquid
(1), selects surface treatment permanent white for use
Can on market, select surface-treated permanent white for use; The permanent white surface treatment agent can be any one in silane coupling agent or tensio-active agent, titanate coupling agent, the aluminate coupling agent, and raw material can be the form of pressed powder, slurry, aqueous suspensions.The particle size range of permanent white powder is 0.1 ~ 0.6um;
The permanent white specific refractory power is 1.64, and close with the nylon 6 fiber specific refractory power (vertical 1.58, horizontal 1.53) are very little to the gloss effect, under certain addition, transparency is not almost influenced.And process white has the microballoon shape, can form spot-like projections on the nylon 6 fiber surface, and then reduce the contact area of nylon 6 fiber, and the power of reducing friction reduces electrostatic effect;
Surface treated permanent white, surface treatment can improve the dispersiveness of permanent white in solution, reduce its reunion, and particle diameter is too thin, then are difficult for disperseing, even disperseed, its specific surface area is big, the easy reunion, generate the macrobead particle.The permanent white mass content is 10 ~ 1000PPM in the finished product, preferred 50 ~ 500PPM.Addition is crossed conference transparency is exerted an influence, and influences the gloss of spun silk, and the silk surface does not have enough projections during the too small then spinning of addition, does not have the effect of reducing friction;
(2), preparation permanent white dispersion liquid
The component of surface treated permanent white, liquid hexanolactam and water is by the proportional arrangement of 1 ~ 20:1 ~ 100:1 ~ 100; Then; Put into whipping device to the component that configures, stirred 0.5 ~ 10 hour down, be mixed with 5% ~ 20% (in the permanent white quality) permanent white dispersion liquid at 20 ~ 95 ℃; Then use the wet grinding machine to disperse when using pressed powder, to open reunion;
(3), obtain barium sulfate suspension
The permanent white dispersion liquid was through 12 ~ 48 hours precipitated and separateds, and it is subsequent use to get the upper strata stable suspension;
Two, preparation molecular-weight adjusting agent dispersing liquid
Molecular weight regulator is dissolved in 100 ~ 50% molten caprolactam or caprolactam water solution, and it is 2% ~ 50% molecular-weight adjusting agent dispersing liquid that dispersed with stirring is processed weight fraction.
Adopt the molecular weight regulator of bimolecular group: C2 ~ C18 straight chained alkyl or C4 ~ C8 naphthenic base, C6 ~ C24 aromatic dicarboxylic acid; A kind of in C4 ~ C20 straight chained alkyl, C4 ~ C8 naphthenic base or the C6 ~ C24 aromatic diamine; Preferred C6 ~ C24 aromatic dicarboxylic acid, the molecular weight regulator of bimolecular group help the stable of melt viscosity;
Three, preparation photostabilizer dispersion liquid
Photostabilizer is dissolved in 50 ~ 0% the caprolactam water solution or water, it is 2% ~ 50% photostabilizer dispersion liquid that dispersed with stirring is processed weight fraction;
Preferred photostabilizer is a 4-carboxyl-2,2,6,6 ,-tetramethyl piperidine, 4-amino-2,2,6,6 ,-tetramethyl piperidine.Described photostabilizer is colourless, and is good with the hexanolactam consistency, have the stable molecule structure, have can with the organism of nylon reactive group;
When being arranged, also brought light nylon 6 slice bleach ultraviolet ray can directly inject nylon inside; Caused double matt nylon variation of light stability phase that light nylon 6 is arranged; And the titanium oxide that contains in half matt nylon ability usable reflection and absorption ultraviolet ray; Reduce action of ultraviolet ray, thereby have light nylon 6 slice photostability than common half delustring section higher requirement to be arranged, the content of said photostabilizer in the light nylon 6 slice is finally arranged is 0.05% ~ 0.5%;
Four, obtain the light nylon 6 slice through successive polymerization, pelletizing, extraction, drying
(1), polyreaction generates polymkeric substance
Hexanolactam or caprolactam water solution; Static mixer is passed through with permanent white dispersion liquid, molecular-weight adjusting agent dispersing liquid, photostabilizer dispersion liquid through metering in the metering back; Join again in prepolymerization tower or the polymerization tower; Through ring-opening polymerization, polymerization temperature is controlled at 240 ~ 280 ℃, generates viscosity and reaches 2.0 ~ 3.0 (98% sulfuric acid) polymkeric substance;
(2), polymer processing is a particle
Plate pumps polymkeric substance through the Cast Strip through Melt Pump, through being sliced into particle;
(3), extraction
Particle with 100 ~ 120 ℃ of extractions, is reduced to extractable matter below 0.5% in pure water;
(4), dried particles obtains finished product
Particle after the extraction feeds 110 ~ 150 ℃ of nitrogen dryings, below the moisture drying to 0.05%, promptly gets the particle that the light nylon 6 slice is arranged that is applicable to high-speed spinning.
Spun the light nylon chips though batchwise polymerization also can be used to produce height, the continuous production device can keep stable processing condition can keep the homogeneity of product, reduces the intermittently problems such as batch difference of device, is preferable methods of the present invention.
Method manufacturing of the present invention the defective that the light nylon 6 slice has overcome has the spinning of light nylon chips now arranged, it possesses excellent spinning property, also reaches gratifying full-rolling rate down high-speed, is specially adapted to the high-speed spinning bright yarn.
Embodiment
Embodiment one
This example has each composition weight of the used raw material of light nylon 6 slice to be:
Hexanolactam 2200 kg
Permanent white powder 1 kg that silane coupling agent is handled
Molecular weight regulator phthalic acid 5 kg
Photostabilizer 4-amino-2,2,6,6 ,-tetramethyl piperidine 2 kg
This component can have light nylon 6 slice 2000kg
One, the preparation of permanent white dispersion liquid
Permanent white powder, pure water and the hexanolactam of selecting for use silane coupling agent 3-aminopropyltriethoxywerene werene to handle are prepared burden in the ratio of 5:90:5; With permanent white powder 1kg; Be equipped with pure water 18kg and hexanolactam 1kg and mix, stir the dispersion liquid of processing permanent white, disperse pump to disperse through multistage shearing again; Precipitate 24 hours, get upper strata suspension-s.
Two, preparation molecular-weight adjusting agent dispersing liquid
Get molecular weight regulator phthalic acid (being the C8 aromatic dicarboxylic acid) 5kg and be dissolved in the 95kg75% caprolactam water solution, be mixed with the dispersion liquid that contains terephthalic acid 5%.
Three, preparation photostabilizer dispersion liquid
Get photostabilizer 4-amino-2,2,6,6 ,-tetramethyl piperidine 2kg is dissolved in the 8kg25% caprolactam water solution, is mixed with to contain 4-amino-2,2,6,6, the dispersion liquid of-tetramethyl piperidine 20%.
Four, obtained the light nylon 6 slice through successive polymerization, pelletizing, extraction, drying
(1), polyreaction generates polymkeric substance
The caprolactam melted into a liquid state at 21.5kg / h of flow rate, flow rate of 0.2kg / h barium sulfate dispersion flow of 1.0kg / h flow rate of terephthalic acid solution and 0.1kg / h of 4 - amino -2 2,2,6,6, - tetramethylpiperidine was mixed into the polymer Fu.Controlling the polymerization Fu temperature from top to bottom, respectively 270 ℃, 260 ℃, 250 ℃.The residence time is 12 hours, aggregates into polymer melt.
(2), polymer processing is a particle
The plate melt pumps polymkeric substance through the Cast Strip, after water-cooled, gets into dicing machine again and is cut to Ф 2*2.5 cylinder shape particle.
(3), extraction
Add extraction tower to particle with transferpump, 110 ℃ of extraction water temperature, the residence time is 12 hours.
(4), dried particles obtains finished product
Particle adds in the drying tower, feeds nitrogen, and the nitrogen inlet temperature is 105 ℃, dew point-20 ℃, the residence time is 24 hours, dry back nitrogen cool off nylon 6 slice.
Comparative Examples one; Routine has light nylon 6 slice (1)
Acetic acid and water are mixed with solution by 10:90.Velocity and flow rate of liquid caprolactam to 22.2kg / h and 0.4kg / h? Acetic acid mixture into the polymerization Fu.Controlling the polymerization Fu temperature from top to bottom, respectively 270 ℃, 260 ℃, 250 ℃.The residence time is 12 hours, and plate pumps the melt that polymerization is accomplished through the Cast Strip with Melt Pump, after water-cooled, gets into dicing machine again and is cut to Ф 2*2.5 cylinder shape particle; Add extraction tower with transferpump again, 110 ℃ of extraction water temperature, the residence time is 12 hours; Add in the drying tower, the nitrogen inlet temperature is 105 ℃ again, dew point-20 ℃; The residence time is 24 hours, dry back nitrogen cool off nylon 6 slice (1).
Comparative Examples two: low-titania content nylon 6 slice (2)
Titanium oxide and pure water, hexanolactam are prepared burden in the ratio of 5:90:5, mix, and are mixed with the suspension-s of titanium oxide, disperse pump to disperse through multistage shearing again, precipitate 24 hours, get upper strata suspension-s.Acetic acid and water are mixed with solution by 10:90.Liquid caprolactam to 22.2kg / h flow rate, flow 0.2kg / h suspension of titanium dioxide, and 0.4kg / h acetic acid was mixed into the polymer Fu.Controlling the polymerization Fu temperature from top to bottom, respectively 270 ℃, 260 ℃, 250 ℃.The residence time is 12 hours, and plate pumps the melt that polymerization is accomplished through the Cast Strip with Melt Pump, after water-cooled, gets into dicing machine again and is cut to Ф 2*2.5 cylinder shape particle; Add extraction tower with transferpump again, 110 ℃ of extraction water temperature, the residence time is 12 hours; Add in the drying tower, the nitrogen inlet temperature is 105 ℃ again, dew point-20 ℃; The residence time is 24 hours, dry back nitrogen cool off nylon 6 slice.
6 sections (3) of Comparative Examples three conventional half matt nylons
Titanium oxide and pure water, hexanolactam are prepared burden in the ratio of 20:75:5, mix, and are mixed with the suspension-s of permanent white, disperse pump to disperse through multistage shearing again, precipitate 24 hours, get upper strata suspension-s.Acetic acid and water are mixed with solution by 10:90.Liquid caprolactam (what is meant) (caprolactam melt to a liquid state) to 22.2kg / h flow rate and flow 0.3kg / h suspension of titanium dioxide, and 0.4kg / h acetic acid was mixed into the polymer Fu.Controlling the polymerization Fu temperature from top to bottom, respectively 270 ℃, 260 ℃, 250 ℃.The residence time is 12 hours, and plate pumps the melt that polymerization is accomplished through the Cast Strip with Melt Pump, after water-cooled, gets into dicing machine again and is cut to Ф 2*2.5 cylinder shape particle; Add extraction tower with transferpump again, 110 ℃ of extraction water temperature, the residence time is 12 hours; Add in the drying tower, the nitrogen inlet temperature is 105 ℃ again, dew point-20 ℃; The residence time is 24 hours, dry back nitrogen cool off nylon 6 slice.
Embodiment, Comparative Examples high rapid-result FDY on same spinning machinery, the relatively full circle rate in 5 day time
From last table contrast, visible, product high-speed spinning speed full-rolling rate (%) of the present invention and silk reflecting feel are superior to the product of Comparative Examples.
Claims (6)
1. a high speed spinning has a light nylon 6 slice, is generated by following component polymerization:
Hexanolactam, permanent white, molecular weight regulator and photostabilizer; Its weight percent is:
Hexanolactam 105 ~ 110%,
Surface treatment permanent white 0.001 ~ 0.1%,
Molecular weight regulator 0.2 ~ 2%,
Photostabilizer 0.05 ~ 0.5%,
Each weight percentages of components sum is one of percentage hundred.
2. a kind of high speed spinning according to claim 1 has a light nylon 6 slice, it is characterized in that said molecular weight regulator is any one in C2 ~ C18 straight chained alkyl or C4 ~ C8 naphthenic base, C6 ~ C24 aromatic dicarboxylic acid, C4 ~ C20 straight chained alkyl, C4 ~ C8 naphthenic base, the C6 ~ C24 aromatic diamine.
3. a kind of high speed spinning according to claim 1 has a light nylon 6 slice, it is characterized in that described photostabilizer is a 4-carboxyl-2,2,6,6, and-tetramethyl piperidine or 4-are amino-2,2,6,6 ,-tetramethyl piperidine.
4. a kind of high speed spinning according to claim 1 has a light nylon 6 slice, and the surface treatment agent that it is characterized in that described surface treatment permanent white is a kind of in silane coupling agent or tensio-active agent, titanate coupling agent, the aluminate coupling agent.
5. a kind of high speed spinning according to claim 4 has a light nylon 6 slice, and the particle size range that it is characterized in that the permanent white powder of said surface treatment permanent white is 0.1 ~ 0.6um.
According to claim 1 or 2,3,4 described a kind of high speed spinnings the light nylon 6 slice arranged, its method of manufacture comprises that the following step gathers:
One, the preparation of permanent white dispersion liquid
(1), selects surface treatment permanent white for use
Can on market, select surface-treated permanent white for use; The permanent white surface treatment agent can be any one in silane coupling agent, tensio-active agent or titanate coupling agent, the aluminate coupling agent, and raw material can be the form of pressed powder, slurry, aqueous suspensions;
(2), preparation permanent white dispersion liquid
The component of surface treated permanent white, liquid hexanolactam and water is by the proportional arrangement of 1 ~ 20:1 ~ 100:1 ~ 100; Then; Put into whipping device to the component that configures, stirred 0.5 ~ 10 hour down, be mixed with 5% ~ 20% (in the permanent white quality) permanent white dispersion liquid at 20 ~ 95 ℃; Then use the wet grinding machine to disperse when using pressed powder, to open reunion;
(3), obtain barium sulfate suspension
The permanent white dispersion liquid was through 12 ~ 48 hours precipitated and separateds, and it is subsequent use to get the upper strata stable suspension;
Two, preparation molecular-weight adjusting agent dispersing liquid
Molecular weight regulator is dissolved in 100 ~ 50% molten caprolactam or caprolactam water solution, and it is 2% ~ 50% molecular-weight adjusting agent dispersing liquid that dispersed with stirring is processed weight fraction;
Three, preparation photostabilizer dispersion liquid
Photostabilizer is dissolved in 50 ~ 0% the caprolactam water solution or water, it is 2% ~ 50% photostabilizer dispersion liquid that dispersed with stirring is processed weight fraction;
Four, obtain the light nylon 6 slice through successive polymerization, pelletizing, extraction, drying
(1), polyreaction generates polymkeric substance
Hexanolactam or caprolactam water solution; Static mixer is passed through with permanent white dispersion liquid, molecular-weight adjusting agent dispersing liquid, photostabilizer dispersion liquid through metering in the metering back; Join again in prepolymerization tower or the polymerization tower; Through ring-opening polymerization, polymerization temperature is controlled at 240 ~ 280 ℃, generates viscosity and reaches 2.0 ~ 3.0 (98% sulfuric acid) polymkeric substance;
(2), polymer processing is a particle
Plate pumps polymkeric substance through the Cast Strip through Melt Pump, through being sliced into particle;
(3), extraction
Particle with 100 ~ 120 ℃ of extractions, is reduced to extractable matter below 0.5% in pure water;
(4), dried particles obtains finished product
Particle after the extraction feeds 110 ~ 150 ℃ of nitrogen dryings, below the moisture drying to 0.05%, promptly gets the particle that the light nylon 6 slice is arranged that is applicable to high-speed spinning.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754663A (en) * | 2018-06-06 | 2018-11-06 | 温州大学 | A kind of nylon 6 slice of high speed spinning and preparation method thereof |
| CN111979591A (en) * | 2020-07-30 | 2020-11-24 | 神马实业股份有限公司 | High-strength high-heat-resistance fine single-fiber nylon 66 fiber and preparation method thereof |
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| CN111979591A (en) * | 2020-07-30 | 2020-11-24 | 神马实业股份有限公司 | High-strength high-heat-resistance fine single-fiber nylon 66 fiber and preparation method thereof |
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Inventor after: Liang Weidong Inventor after: Mao Xinhua Inventor after: Jian Jinchi Inventor after: Shi Yujun Inventor after: Zhang Yitang Inventor after: Chen Jizong Inventor before: Liang Weidong Inventor before: Mao Xinhua Inventor before: Jian Jinchi Inventor before: Shi Yujun Inventor before: Zhang Yitang Inventor before: Zhan Jizhong |
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Application publication date: 20120919 |