CN101857981B - Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group - Google Patents

Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group Download PDF

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CN101857981B
CN101857981B CN201010151762A CN201010151762A CN101857981B CN 101857981 B CN101857981 B CN 101857981B CN 201010151762 A CN201010151762 A CN 201010151762A CN 201010151762 A CN201010151762 A CN 201010151762A CN 101857981 B CN101857981 B CN 101857981B
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polylactic acid
spinning
melt
flange
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CN101857981A (en
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程贤生
谈杰
李涛
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Anhui Han Lian color textile Limited by Share Ltd
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ANHUI HESHENG NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a process for producing nanometer bamboo carbon fiber by adopting a polylactic acid group. In the process, the nanometer bamboo carbon fiber is produced from polylactic acid as a carrier and nanometer bamboo carbon powder by a dry spinning technology. The nanometer bamboo carbon fiber produced by the invention has the advantages of greenness, environmental protection, easy recovery and degradation, low carbon emission during production, simple production process, easy operation and low cost.

Description

Adopt the process of polylactic acid based production nanometer bamboo carbon fiber
Technical field
The present invention relates to the process of suitability for industrialized production nanometer bamboo carbon fiber, specifically is the process that adopts polylactic acid based production nanometer bamboo carbon fiber.
Background technology
In modern society, research and produce ecological with the healthy functional textile that is beneficial to man and become a kind of trend.Bamboo charcoal is a kind of new function material, has the environment-friendly materials of excellent performance, has the good reputation of " black diamond ", is described as " the new bodyguard of the environmental protection of 21 century " in the world, is the brand-new developing direction that bamboo timber resource effectively utilizes.Bamboo-carbon fibre is to select nano bamboo powder (bamboo charcoal micropowder) for use, and it is added in section or the spinning solution again through the approximate spun fibre new species of conventional spinning technique through special process.
Bamboo-carbon fibre and the fabric of processing thereof have function and effects such as absorbing and deodorizing, antibacterial mildew-resistant, emission far infrared, anion.According to surveying and determination, there are micropore, mesopore and macropore in bamboo-carbon fibre inside, and specific area is big.1cm 3The specific area of bamboo charcoal can reach 350m 2, make the bamboo charcoal textiles can adsorb multiple pernicious gas, eliminate body odor and airborne peculiar smell.Bamboo-carbon fibre can continue to discharge anion, through detecting, when measuring distance 1cm, discharges 2000/cm of anion 3, during measuring distance 2cm, discharge 1600/cm of anion 3Bamboo-carbon fibre can absorb and the far infrared that radiates 4-14 μ m again, and the growth of the far infrared of this section wavelength and biology has utmost point confidential relation, so be called " fertility light " or " growth light " again.Far infrared is absorbed by the body easily, can increase the microvascular blood circulation of human body surface, and the effect that have heat accumulation thermal, enhances metabolism there is obvious effect for prevention and treatment of arthritis, insomnia etc.Except that above premium properties, bamboo-carbon fibre also has characteristics such as environmental protection, electrostatic screen, antibacterial and mouldproof, and grey, the black of the nature that all has of bamboo-carbon fibre, do not need to make it dyeing, does not contain the harmful substance of chemical dye, so environment protection health.
2003, egression chemical fibre group in Xinxiang, Henan successfully developed bamboo-carbon viscose fibre.The fragrant charcoal nanoscale of the bamboo micro mist that this fiber adopts the hill mao bamboon of China's south high-quality to process is a raw material, is added in the viscose glue, is made through special process.In the same year, Shanghai Hualy Superfines Science and Technology Co.,Ltd. of East China University of Science has released a bamboo-carbon fibre new varieties.This fiber is to process at the ultra-fine bamboo charcoal additive that fiber surface is coated a kind of pure natural.Since 2004, the Taiwan is also reported successively has New-type bamboo charcoal fibre to come out.Weaving center, Taiwan utilizes nanometer technology with bamboo charcoal micropowderization, incorporates bamboo charcoal in the polyester fiber equably through the melt spinning program, thereby processes bamboo-carbon fibre.2005, Japanese natural science magazine reported that Japan produces 500 purpose bamboo-carbon fibres, and its processing method is that bamboo charcoal is processed as the first step, then bamboo fibre is elongated and with weave ins such as chemical fibre, cotton thread.2006, the great strong color polyester in Shangyu, Zhejiang Co., Ltd successfully developed the multifunction environment-protection type bamboo-carbon fibre.The processing of this bamboo-carbon fibre is after pure oxygen high temperature intercepts the novel technique processing with nitrogen through moment the above bamboo of life in 5 years; Pass through physical method; Make its particle diameter reach micron order; Polyester modified section after handling through the particular polymeric technology is fused among the spinning melt then, processes bamboo-carbon fibre through spinning again.
PLA (being called for short PLA) is to be the resulting high molecular polymer of main raw material polymerization with lactic acid.And the raw material of lactic acid is the material of all carbohydrate enrichments, and for example corn, potato and organic waste etc. can constantly be regenerated, therefore inexhaustible.Acid fiber by polylactic is the tencel cellulose fiber that the polylactic resin section is processed through the melting spinning.It is the environmentally friendly regenerated celulose fibre of a kind of intrinsic antibiotic property of not adding all harmful chemicals and anti-flammability, weather fastness.Detect according to the charcoal discharge capacity, the regenerated celulose fibre viscose that adopts traditional viscose process production is 14680CO 2Kg/t, to represent the polyester of synthetic fiber be 6443 CO 2Kg/t, and acid fiber by polylactic 3650 CO only 2Kg/t, its carrying capacity of environment characteristic is remarkable.
Discuss according to the front, can know that traditional bamboo-carbon fibre produces used carrier and be mainly viscose glue and two kinds of polyester, its charcoal discharge capacity occupies high, and the oil product resource is nervous, is difficult for degrading.The acid fiber by polylactic recyclable regenerative, aboundresources, intrinsic antibiotic property and characteristics such as anti-flammability, weather, environment protection health.
Summary of the invention
The invention provides a kind of process that adopts polylactic acid based production nanometer bamboo carbon fiber; Be that the employing PLA is a carrier; Add the bamboo charcoal nano powder, utilize the dry spinning technology to produce environmental protection, be prone to the nanometer bamboo carbon fiber process that reclaims, is prone to degraded, produces low charcoal discharging.
The technical scheme of invention is down:
Adopt the process of polylactic acid based production nanometer bamboo carbon fiber, may further comprise the steps:
(1), with polylactic acid slice and bamboo charcoal nano powder by the mass percent of 95-97%:3-5% mix mixed material; Mixed material carries out the heating, vacuum drying; Dry process conditions are: descended predrying 100-140 minute at 103-107 ℃, be warmed up to 118-122 ℃ of dry 6.5-7.5 hour then;
(2), dried mixed material is transported in six casees screw extruders carries out heating and melting through one to six the casees successively and get melt; One to six casees temperature is set to respectively successively: 158-162 ℃, 180-190 ℃, 170-180 ℃, 165-175 ℃, 165-175 ℃, 170-180 ℃; Then melt Conveying is got in the filament spinning component flange and continue heating at 170-180 ℃; With the melt that continues to obtain after the heating carry out spinning, wire vent gets long filament, spinning temperature is 170-180 ℃;
(3), with long filament through cooling forming; The long filament of moulding through seal wire, oil, doff; Long filament behind the doff stretches drawing of fiber 3.5-4 times that obtains long filament through boundling immersion oil, 55-65 ℃ following water-bath drawing-off, physics then; Silk is wide through regulating then, coiling, HEAT SETTING, cooling, cut-out, packing, finished product.
The molecular weight of described polylactic acid slice is 33.5 ten thousand, and fusing point is 155-165 ℃, and degree of crystallinity is 74-78%, and glass transition temperature is 58-59 ℃, and the L-content of isomer of section molecule is more than 99%; The particle diameter of described bamboo charcoal nano powder is 90-100nm, and the screening particle diameter is the 15000-18000 order.
Described spinning, wire vent are to be spinning after 165-175 ℃ filter is conveyed into manifold with melt through temperature, are that compression pump, the frequency of 10-20Mpa is the measuring pump of 40-50HZ through excess pressure then, supply with spinning pack uniformly, by nozzle ejection silk; Described cooling forming adopts low temperature ring blowing carrying out cooling forming, and temperature 19-21 ℃, wind speed are 0.22-0.27m/s; The finish addition of described boundling immersion oil is 5-7kg/T; It is to carry out the physics stretching through deflector roll and take up roll that described physics stretches, and the deflector roll frequency is 20-30HZ, and the take up roll frequency is 20-25HZ; Described adjusting silk is wide to be with the wide silk ribbon of furnishing 100mm on tension bracket of the long filament after the drawing-off; Described coiling is to reel with 800-1200m/min speed; Described HEAT SETTING is that the silk after reeling is come on the lax heat setting machine, utilizes vapours to carry out dryness finalization through baking oven 1 and 2 pairs of long filaments of baking oven successively, and the temperature of baking oven 1 is 75-85 ℃, and the temperature of baking oven 2 is 80-90 ℃; Described cut-out is to cut off through cutting machine with the speed of 90-110m/min.
Six casees screw extruders of the present invention are to be produced by Anhui Nanao Carpet Co., Ltd., and model is JLG120.
Polylactic acid slice of the present invention is to be produced with victory Science and Technology Ltd. by Anhui; Described bamboo charcoal nano powder is commercially available by Shanghai Keruisen Environmental Protection Technology Co., Ltd..
The present invention has following advantage:
1, raw material sources are wide, and PLA belongs to regenerated celulose fibre, are regenerated resources, and the production process greenization does not have the oilization of genus;
2, the PLA energy consumption is low, and the charcoal discharge capacity is merely 3650 CO 2Kg/t, less than 1/3 of viscose glue, 1/2 of about polyester, its carrying capacity of environment characteristic is remarkable;
3, biological degradability is good, and is free from environmental pollution, and can reclaim granulation again after the bamboo charcoal nano powder of the present invention use, realizes reclaiming spinning 2 times, economizes on resources;
4, the fiber of bamboo charcoal nano and the fabric processed thereof have function and effects such as absorbing and deodorizing, antibacterial mildew-resistant, emission far infrared, anion, belong to green functional property new material.
Description of drawings
Fig. 1 doesProcess chart of the present invention.
The specific embodiment
Adopt the process of polylactic acid based production nanometer bamboo carbon fiber, comprise following processing step:
(1), the apolegamy of raw material:
The polylactic acid slice that the present invention uses is come Anhui and is won Science and Technology Ltd.'s self-control, and molecular weight is 33.5 ten thousand, 162 ℃ of fusing points, and degree of crystallinity is about 76%, 58.5 ℃ of glass transition temperatures, the L-content of isomer of section molecule is more than 99%; The bamboo charcoal nano powder is commercially available black 18000 orders of Shanghai Keruisen Environmental Protection Technology Co., Ltd., the specification of 100nm; The mass ratio of polylactic acid slice and bamboo charcoal nano powder is among the present invention: polylactic acid slice 95%, bamboo charcoal nano powder 5%.
(2), raw materials mix oven dry:
The ratio that polylactic acid slice and bamboo charcoal nano powder gather (1) according to the step is mixed, render to vacuum drier then and carry out heat drying.Dry technology does, predrying temperature is 106 ℃, and be 2.5 hours drying time; Stretch temperature then to 120 ℃, dry 7 hours.Dried polylactic acid slice moisture content remains on below the 30ppm.
(3), melt spinning:
The mixed material that is gathered (2) middle drying the step is transported to and carries out heating and melting in six casees screw extruders, and the temperature of the temperature of control from one to six each case is respectively: 160 ℃, 185 ℃, 175 ℃, 170 ℃, 170 ℃, 175 ℃.Raw materials melt through after the screw extruder heating becomes melt, and melt Conveying is got in the filament spinning component flange (flange divides three zones: big flange, flange 1, flange 2) continue heating again, be that the melt melted by heating is more even.Its control temperature is: 175 ℃.Get into manifold (temperature is 175 ℃) through the melt Conveying behind the flange assembly through filter (temperature is 172 ℃) and carry out spinning.Melt gets into manifold after excess pressure pump (pressure is 17Mpa), measuring pump (frequency is 45HZ) are supplied with spinning pack uniformly, by nozzle ejection silk.
(4), cold and hot moulding:
By the long filament of spinneret ejection, adopt the blowing of low temperature ring to cool off (20 ℃ of temperature, wind speed are 0.25m/s) moulding.When the long filament of moulding passes through the deflector roll seal wire, utilize deflector roll to oil, give a silk doff then.Long filament behind the doff is again through creel boundling (30) immersion oil, through water-bath, oil bath two procedures, through deflector roll and take up roll with 3.6 times of tensile fibers.Wherein bath temperature is: 604 ℃, the finish addition is 6kg/T, deflector roll frequency: 25HZ, take up roll frequency: 25HZ.With the silk wide silk ribbon of furnishing 100mm on tension bracket after the drawing-off, reel with 1000m/min speed.The silk of reeling is come on the lax heat setting machine, utilize vapours let the long filament dryness finalization through baking oven 1 and 2 (temperature is respectively 80 ℃, 85 ℃).After baking oven 3 coolings, cut off through cutting machine with the speed of 100m/min, wind send packing again.

Claims (1)

1. adopt the process of polylactic acid based production nanometer bamboo carbon fiber, it is characterized in that: may further comprise the steps:
(1), raw materials mix oven dry:
Polylactic acid slice and bamboo charcoal nano powder are mixed by 95%: 5% mass percent, render to vacuum drier then and carry out heat drying, dry technology is: predrying temperature is 106 ℃, and be 2.5 hours drying time; Be warmed up to 120 ℃ then, dry 7 hours; Dried polylactic acid slice moisture content remains on below the 30ppm;
Wherein, the molecular weight of polylactic acid slice is 33.5 ten thousand, 162 ℃ of fusing points, and degree of crystallinity 76%, 58.5 ℃ of glass transition temperatures, the L-content of isomer of section molecule is more than 99%; The particle diameter of bamboo charcoal nano powder is 100nm, and the screening particle diameter is 18000 orders;
(2), melt spinning:
The mixed material that is gathered (1) middle drying the step is transported to and carries out heating and melting in six casees screw extruders, and the temperature of the temperature of control from one to six each case is respectively: 160 ℃, 185 ℃, 175 ℃, 170 ℃, 170 ℃, 175 ℃;
Raw materials melt through after the screw extruder heating becomes melt, melt Conveying is got into continue heating in the filament spinning component flange again, and flange is divided into big flange, flange 1 and 2 three zones of flange, and its control temperature is 175 ℃;
Get into manifold through the melt Conveying behind the flange assembly through filter and carry out spinning, filter temperature is 172 ℃, and condition of spinning manifold temperature is 175 ℃;
Melt gets into manifold after excess pressure pump, measuring pump are supplied with spinning pack uniformly, and by nozzle ejection silk, compression pump pressure is 17Mpa, and the measuring pump frequency is 45HZ;
(3), cold and hot moulding:
By the long filament of spinneret ejection, adopt the blowing of low temperature ring to carry out cooling forming, temperature is 20 ℃, wind speed is 0.25m/s;
When the long filament of moulding passes through the deflector roll seal wire, utilize deflector roll to oil, give a silk doff then;
Long filament behind the doff is again through 30 immersion oil of creel boundling, and through water-bath, oil bath two procedures, with 3.6 times of tensile fibers, wherein bath temperature is 604 ℃ through deflector roll and take up roll, and the finish addition is 6kg/T, and the deflector roll frequency is 25HZ, and the take up roll frequency is 25HZ;
With the silk wide silk ribbon of furnishing 100mm on tension bracket after the drawing-off, reel with 1000m/min speed;
The silk of reeling is come on the lax heat setting machine, utilize vapours to let long filament dryness finalization, baking oven 1 and 2 temperature be respectively 80 ℃, 85 ℃ through baking oven 1 and 2;
After after baking oven 3 coolings, cut off through cutting machine with the speed of 100m/min, wind send packing.
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CN105463589B (en) * 2016-01-11 2018-02-16 河南省龙都生物科技有限公司 Bamboo charcoal particles of polylactic acid spinning technique
CN105504236B (en) * 2016-01-11 2018-06-26 河南省龙都生物科技有限公司 Polylactic acid bamboo charcoal is sliced production technology
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CN105671648B (en) * 2016-01-11 2018-03-23 河南省龙都生物科技有限公司 Bamboo charcoal micropowder polylactic acid slice produces fibre technology
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