WO2022099979A1 - Method for preparing flame-retardant colored functional environmentally friendly fibers - Google Patents
Method for preparing flame-retardant colored functional environmentally friendly fibers Download PDFInfo
- Publication number
- WO2022099979A1 WO2022099979A1 PCT/CN2021/084434 CN2021084434W WO2022099979A1 WO 2022099979 A1 WO2022099979 A1 WO 2022099979A1 CN 2021084434 W CN2021084434 W CN 2021084434W WO 2022099979 A1 WO2022099979 A1 WO 2022099979A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- retardant
- flame
- polylactic acid
- environmentally friendly
- calcium carbonate
- Prior art date
Links
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000003063 flame retardant Substances 0.000 title claims abstract description 106
- 239000000835 fiber Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 79
- 239000004626 polylactic acid Substances 0.000 claims abstract description 79
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 73
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 40
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000007909 melt granulation Methods 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 10
- 230000003179 granulation Effects 0.000 claims abstract description 10
- 238000009987 spinning Methods 0.000 claims abstract description 10
- 238000001125 extrusion Methods 0.000 claims abstract description 9
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 33
- 238000004040 coloring Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 22
- 230000007613 environmental effect Effects 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000003086 colorant Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 8
- 239000012943 hotmelt Substances 0.000 claims description 7
- REJHVSOVQBJEBF-OWOJBTEDSA-N 5-azaniumyl-2-[(e)-2-(4-azaniumyl-2-sulfonatophenyl)ethenyl]benzenesulfonate Chemical compound OS(=O)(=O)C1=CC(N)=CC=C1\C=C\C1=CC=C(N)C=C1S(O)(=O)=O REJHVSOVQBJEBF-OWOJBTEDSA-N 0.000 claims description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- HONMCSLFRKBQHG-UHFFFAOYSA-N 1,3-diamino-1,3-diphenylurea Chemical compound C=1C=CC=CC=1N(N)C(=O)N(N)C1=CC=CC=C1 HONMCSLFRKBQHG-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 229920000728 polyester Polymers 0.000 abstract description 9
- 239000000049 pigment Substances 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000011550 stock solution Substances 0.000 abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 42
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 22
- 239000000920 calcium hydroxide Substances 0.000 description 22
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 15
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 12
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 12
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical class [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002131 composite material Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000001523 electrospinning Methods 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 235000014655 lactic acid Nutrition 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000000859 sublimation Methods 0.000 description 6
- 230000008022 sublimation Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000005292 vacuum distillation Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- QRTXZGIQTYDABO-UHFFFAOYSA-N carbanolate Chemical compound CNC(=O)OC1=CC(C)=C(C)C=C1Cl QRTXZGIQTYDABO-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- -1 compound antimony trioxide Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000009973 dope dyeing Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000002473 artificial blood Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Definitions
- the invention belongs to the field of fibers, and in particular relates to a preparation method of a flame-retardant coloring functional environment-friendly fiber.
- Polyester fiber is a synthetic fiber obtained by spinning polyester obtained by polycondensation of organic dibasic acid and dihydric alcohol. Polyester fiber is mainly used for clothing and interior decoration. Chemical fiber blending; filaments can be processed into elastic yarns, tire cords, industrial ropes, transmission belts, filter cloths and fishing nets, etc., and can also be used as electrical insulating materials and artificial blood vessels.
- Polyester fibers have been widely used because of their high strength and good elasticity. However, because they are flammable substances, their application in many fields is limited. Therefore, the research on flame retardant copolyester fibers has received extensive attention. And has successfully obtained industrial production. Fiber dope dyeing technology is a commonly used method for preparing colored fibers in the industry. Because it does not produce waste water and causes water pollution problems, and its products are bright in color, uniform in color, and not easy to fade, it has been widely valued by the industry. However, the flame retardant polyester fiber produced by the dope dyeing technology has poor flame retardant effect, and there is no technical improvement based on this technology.
- the present invention provides a method for preparing flame-retardant colored functional environmental protection fibers, which solves the problem of poor flame-retardant effect of the existing flame-retardant polyester fibers, and utilizes the melt granulation of polylactic acid powder
- the flame retardant is intrusively mixed to achieve the improvement of the flame retardant properties of the polylactic acid powder, thereby improving the overall performance.
- the technical scheme of the present invention is:
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and after drying, extrude and granulate through a screw extruder to obtain a raw liquid coloring flame retardant polylactic acid masterbatch;
- Step 2 spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber.
- the mass proportion of polylactic acid powder is 65-82%
- the mass proportion of environmental protection pigment is 5-15%
- the mass proportion of flame retardant is 65-82%. 12-15%
- the mass proportion of nano calcium carbonate is 3-5%.
- the environment-friendly color material adopts one of diaminostilbene disulfonic acid, 4.4-diaminodiphenylurea, and diaminoheterocycle.
- the flame retardant adopts antimony trioxide or magnesium hydroxide.
- the flame retardant adopts activated alumina composite antimony trioxide
- the preparation method of the activated alumina composite antimony trioxide includes the following steps: step i, adding antimony trichloride and aluminum trichloride into Stir evenly in dehydrated ethanol until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 3-5:2, and the ratio of the antimony trichloride in dehydrated ethanol is 3-5:2.
- the concentration is 100-150g/L, and the stirring speed is 1000-2000r/min; in step ii, saturated ammonia water is passed into the dissolved alcohol solution until the precipitation no longer forms, then filtered and washed with distilled water to obtain a precipitate, which is dried at a constant temperature Dry to obtain activated alumina composite antimony trioxide, wherein, the feeding amount of saturated ammonia water is 5-10mL/min, The time is 60-120min, and the temperature of constant temperature drying is 200-250°C.
- the nano calcium carbonate adopts light nano calcium carbonate.
- nano-calcium titanate is coated with light-weight nano-calcium carbonate.
- the preparation method of the coated light-weight nano-calcium carbonate comprises the following steps:
- step a calcium hydroxide powder and n-butyl titanate are blended and added to absolute ethanol, and then left to dry to obtain coated calcium hydroxide powder;
- the amount of n-butyl titanate added is hydrogen 10-20% of the mass of calcium oxide, the mass of the anhydrous ethanol is 150-200% of the mass of n-butyl titanate, and the temperature for standing and drying is 80-100 °C;
- the diameter is 10-20 ⁇ m;
- step b the coated calcium hydroxide powder and polyvinylpyrrolidone are stirred and mixed to form a blend, and then electrospinned to form a monofilament, and the monofilament is placed in a sealed environment for 30-50 minutes to obtain a prefabricated filament; the The amount of polyvinylpyrrolidone added is 150-200% of the quality of the coated calcium hydroxide, the temperature of electrospinning is 135-145°C, the pressure of the closed environment is 0.3-0.5MPa, and the temperature is 100-110°C.
- the airtight environment is composed of ether vapor and water vapor, and the volume ratio of ether vapor to water vapor is 10:0.3-0.8;
- step c the prefabricated filaments are placed in absolute ethanol for microwave reaction for 30-50 min, and after filtration, the coated light nano-calcium carbonate is obtained; the concentration of the prefabricated filaments in absolute ethanol is 100-200 g/L, The power of the microwave reaction is 200-400W, and the temperature is 10-20°C;
- step d the filtered waste liquid is distilled under reduced pressure to obtain polyvinylpyrrolidone and dehydrated alcohol.
- the temperature of the vacuum distillation is 80-90° C., and the pressure is 70-80% of the standard atmospheric pressure.
- step b absolute ethanol is recovered for step a and step c.
- the extrusion granulation adopts a hot melt granulation method, and the temperature is 160-170°C.
- the mass ratio of the raw liquid and the flame-retardant polylactic acid masterbatch is 13-15%, and the mass ratio of the polylactic acid chips is 85-87%.
- the drawing force is 0.5-0.9 MPa.
- the present invention has the following advantages:
- the present invention solves the problem of poor flame retardant effect of existing flame retardant polyester fibers, and uses the melt granulation method of polylactic acid powder to mix the flame retardant in an intrusive manner, so as to improve the flame retardant properties of polylactic acid powder. , so as to improve the overall performance.
- the present invention uses antimony trioxide as a flame retardant, which forms a stable molten state after combustion, and forms a surface protective film to isolate the air at the initial stage of combustion. The area of the protective liquid film.
- the present invention uses light calcium carbonate as a filler to form a stable microporous system and improve stability.
- calcium carbonate is given good weather resistance and antibacterial properties, while reducing the effect of titanium dioxide on organic compounds. Molecular degradation effects.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65%, the mass proportion of environmental protection pigment is 15%, the mass proportion of flame retardant is 15%, and the mass proportion of nano calcium carbonate is 5%.
- the environmentally friendly color material adopts diaminostilbene disulfonic acid; the flame retardant adopts antimony trioxide; the nano calcium carbonate adopts light nano calcium carbonate; the extrusion granulation adopts hot melting Granulation method, the temperature is 160 °C;
- Step 2 spinning and drawing the raw solution colored flame retardant polylactic acid masterbatch and the polylactic acid chips to obtain the raw solution colored flame retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 87%; the tensile force of the drawing is 0.5MPa.
- the prepared filaments limiting oxygen index 30%, strength 3.7cN/dtex, color fastness to washing 5, sublimation fastness 5.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 82%, the mass proportion of environmental protection pigment is 5%, the mass proportion of flame retardant is 10%, and the mass proportion of nano calcium carbonate is 3%.
- the environmentally friendly color material adopts 4.4-diaminodiphenylurea;
- the flame retardant adopts magnesium hydroxide;
- the nano calcium carbonate adopts light nano calcium carbonate;
- the extrusion granulation adopts hot melt granulation method , the temperature is 170°C;
- Step 2 spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 85%; the tensile force of the drawing is 0.9MPa.
- the prepared filaments limiting oxygen index 32%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 73%, the mass proportion of environmental protection pigment is 10%, the mass proportion of flame retardant is 13%, and the mass proportion of nano calcium carbonate is 4%.
- the environmentally friendly colorant adopts one of diaminostilbene disulfonic acid, 4.4-diaminodiphenylurea, and diaminoheterocycle;
- the flame retardant adopts antimony trioxide or magnesium hydroxide ;
- Described nano calcium carbonate adopts light nano calcium carbonate;
- Described extrusion granulation adopts hot melt granulation method, and the temperature is 165 °C;
- Step 2 spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 86%; the tensile force of the drawing is 0.7MPa.
- the prepared filaments limiting oxygen index 31%, strength 3.8cN/dtex, color fastness to washing 5, sublimation fastness 5.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65%, the mass proportion of environmental protection pigment is 15%, the mass proportion of flame retardant is 15%, and the mass proportion of nano calcium carbonate is 5%.
- the environment-friendly color material adopts diaminostilbene disulfonic acid; the flame retardant adopts activated alumina compound antimony trioxide, and its preparation method includes the following steps: step i, mixing antimony trichloride and trioxide
- step i mixing antimony trichloride and trioxide
- the aluminum chloride is added to 1 L of anhydrous ethanol and stirred evenly until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 3:2, and the antimony trichloride in anhydrous
- the concentration in the ethanol is 100 g/L, and the stirring speed is 1000 r/min; in step ii, saturated ammonia water is passed into the dissolved alcohol solution until the precipitation no longer forms, then filtered and washed with distilled water to obtain a precipitate, which is dried at a constant temperature
- Activated alumina composite antimony trioxide is obtained, wherein the feeding amount of
- Step 2 spinning and drawing the raw solution colored flame retardant polylactic acid masterbatch and the polylactic acid chips to obtain the raw solution colored flame retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 87%; the tensile force of the drawing is 0.5MPa.
- the prepared fiber yarn limiting oxygen index 33%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 82%, the mass proportion of environmental protection pigment is 5%, the mass proportion of flame retardant is 10%, and the mass proportion of nano calcium carbonate is 3%.
- the environmentally friendly colorant adopts 4.4-diaminodiphenylurea
- the flame retardant adopts activated alumina composite antimony trioxide
- the preparation method of the activated alumina composite antimony trioxide comprises the following steps: step i, adding antimony trichloride and aluminum trichloride to 1 L of dehydrated alcohol and stirring, until completely dissolved, to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 5:2, and The concentration of the antimony trichloride in absolute ethanol is 150 g/L, and the stirring speed is 2000 r/min; step ii, the saturated ammonia water is passed into the dissolved alcohol solution until the precipitation is no longer formed, then filtered and washed with distilled water , obtain the precipitate, obtain the activated alumina composite antimony trioxide through constant temperature drying, wherein, the feeding amount of saturated ammonia water is 5mL/min, The time is 120min, and
- step c put the prefabricated filaments into 1 L of absolute ethanol for microwave reaction for 50 min, and after filtration, obtain coated light-weight nano-calcium carbonate; the concentration of the prefabricated filaments in absolute ethanol is 200 g/L, and the microwave reaction
- the power is 400W, and the temperature is 20 ° C; step d, the filtered waste liquid is vacuum distilled to obtain polyvinylpyrrolidone and anhydrous ethanol, the temperature of the vacuum distillation is
- Step 2 spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 85%; the tensile force of the drawing is 0.9MPa.
- the prepared filaments limiting oxygen index 35%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
- a preparation method of flame-retardant coloring functional environmental protection fiber comprising the following steps:
- Step 1 Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 73%, the mass proportion of environmental protection pigment is 10%, the mass proportion of flame retardant is 13%, and the mass proportion of nano calcium carbonate is 4%.
- the environment-friendly coloring material adopts diamino heterocycles; the flame retardant adopts activated alumina compound antimony trioxide, and the preparation method thereof includes the following steps: Step i, combining antimony trichloride and aluminum trichloride with Add it to 1 L of absolute ethanol and stir until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 2:1, and the ratio of the antimony trichloride in the absolute ethanol is 2:1.
- step ii saturated ammonia water is passed into the dissolved alcohol solution until the precipitation is no longer formed, then filtered and washed with distilled water to obtain the precipitate, which is dried at a constant temperature to obtain active oxidation Aluminum composite antimony trioxide, wherein, the feeding amount of saturated ammonia water is 8mL/min, The time is 90min, and the temperature of constant temperature drying is 230°C; the nano-calcium carbonate adopts coated light-weight nano-calcium carbonate, and the preparation method includes the following steps: step a, 100 g of calcium hydroxide powder is mixed with n-butyl titanate The ester is blended and added to absolute ethanol, and then left to dry to obtain coated calcium hydroxide powder; the amount of n-butyl titanate added is 15% of the mass of calcium hydroxide, and the mass of the absolute ethanol is 15%.
- step b the coating calcium hydroxide powder is stirred and mixed with polyvinylpyrrolidone to form The blend material is then electrospun to form monofilaments, and the monofilaments are placed in a sealed environment for 40 minutes to obtain prefabricated filaments; the amount of polyvinylpyrrolidone added is 180% of the quality of the coated calcium hydroxide, and the electrospinning
- the temperature of the silk is 140°C
- the pressure of the airtight environment is 0.4MPa
- the temperature is 105°C
- the airtight environment is composed of ether steam and water vapor
- the volume ratio of ether steam and water vapor is 10:0.5
- Step c put the prefabricated filaments into 1 L of absolute ethanol for microwave reaction for 40 min, and after filtration, obtain coated light nano-calcium carbonate; the concentration of the pre
- Step 2 spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber;
- the mass ratio of the lactic acid slices is 86%; the tensile force of the drawing is 0.7MPa.
- the prepared filaments limiting oxygen index 35%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
- the present invention has the following advantages:
- the present invention solves the problem of poor flame retardant effect of existing flame retardant polyester fibers, and uses the melt granulation method of polylactic acid powder to mix the flame retardant in an intrusive manner, so as to improve the flame retardant properties of polylactic acid powder. , so as to improve the overall performance.
- the present invention uses antimony trioxide as a flame retardant, which forms a stable molten state after combustion, and forms a surface protective film to isolate the air at the initial stage of combustion. The area of the protective liquid film.
- the present invention uses light calcium carbonate as a filler to form a stable microporous system and improve stability.
- calcium carbonate is given good weather resistance and antibacterial properties, while reducing the effect of titanium dioxide on organic compounds. Molecular degradation effects.
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Abstract
A method for preparing flame-retardant colored functional environmentally friendly fibers. The method comprises the following steps: step 1. uniformly mixing a polylactic acid powder, an environmentally friendly pigment, a flame retardant, and nano calcium carbonate, drying the mixture, and carrying out extrusion granulation by means of a screw extruder to obtain a stock solution colored flame-retardant polylactic acid master batch; and step 2. subjecting the stock solution colored flame-retardant polylactic acid master batch and polylactic acid slices to spinning and drawing to obtain stock solution colored flame-retardant polylactic acid fibers. The problem of existing flame-retardant polyester fibers having a poor flame-retardant effect is solved, and by intrusively mixing the flame retardant by means of the melt granulation of the polylactic acid powder, the flame-retardant properties of the polylactic acid powder are improved, and the overall performance is thus improved.
Description
本发明属于纤维领域,具体涉及一种阻燃着色功能性环保纤维的制备方法。The invention belongs to the field of fibers, and in particular relates to a preparation method of a flame-retardant coloring functional environment-friendly fiber.
聚酯纤维由有机二元酸和二元醇缩聚而成的聚酯经纺丝所得的合成纤维，聚酯纤维主要用于衣着和室内装饰，短纤维可以纯纺，也可与天然纤维及其他化学纤维混纺；长丝可加工制得弹力丝，也可制轮胎帘子线、工业绳索、传动带、滤布及渔网等，还可用作电绝缘材料以及制备人造血管等。Polyester fiber is a synthetic fiber obtained by spinning polyester obtained by polycondensation of organic dibasic acid and dihydric alcohol. Polyester fiber is mainly used for clothing and interior decoration. Chemical fiber blending; filaments can be processed into elastic yarns, tire cords, industrial ropes, transmission belts, filter cloths and fishing nets, etc., and can also be used as electrical insulating materials and artificial blood vessels.
聚酯纤维因其强度高、弹性好等优点而得到了广泛的应用，但由于属于易燃性物质，使其在很多领域的应用受限制，因此阻燃共聚酯纤维的研究得到广泛关注，并已成功获得工业化生产。纤维原液着色技术是工业界常用的制备有色纤维的方法，由于不会产生废水而造成水污染问题，且其产品颜色鲜艳、色泽均匀、不易褪色，因此得到工业界的广泛重视。但是，采用原液着色技术生产的阻燃聚酯纤维阻燃效果不佳，且目前还未有在该技术基础上的技术改进。Polyester fibers have been widely used because of their high strength and good elasticity. However, because they are flammable substances, their application in many fields is limited. Therefore, the research on flame retardant copolyester fibers has received extensive attention. And has successfully obtained industrial production. Fiber dope dyeing technology is a commonly used method for preparing colored fibers in the industry. Because it does not produce waste water and causes water pollution problems, and its products are bright in color, uniform in color, and not easy to fade, it has been widely valued by the industry. However, the flame retardant polyester fiber produced by the dope dyeing technology has poor flame retardant effect, and there is no technical improvement based on this technology.
针对现有技术中的问题，本发明提供一种阻燃着色功能性环保纤维的制备方法，解决了现有阻燃聚酯纤维阻燃效果不佳的问题，利用聚乳酸粉体的熔融造粒方式将阻燃剂进行侵入式混合，实现聚乳酸粉体的阻燃特性提升，从而达到提升整体性能的提升。In view of the problems in the prior art, the present invention provides a method for preparing flame-retardant colored functional environmental protection fibers, which solves the problem of poor flame-retardant effect of the existing flame-retardant polyester fibers, and utilizes the melt granulation of polylactic acid powder The flame retardant is intrusively mixed to achieve the improvement of the flame retardant properties of the polylactic acid powder, thereby improving the overall performance.
为实现以上技术目的，本发明的技术方案是：For realizing the above technical purpose, the technical scheme of the present invention is:
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and after drying, extrude and granulate through a screw extruder to obtain a raw liquid coloring flame retardant polylactic acid masterbatch;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber.
进一步的，所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为65-82%，环保色料的质量占比为5-15%，阻燃剂的质量占比为12-15%，纳米碳酸钙的质量占比为3-5%。Further, in the raw liquid coloring flame retardant polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65-82%, the mass proportion of environmental protection pigment is 5-15%, and the mass proportion of flame retardant is 65-82%. 12-15%, the mass proportion of nano calcium carbonate is 3-5%.
所述环保色料采用二氨基二苯乙烯二磺酸类、4.4-二氨基二苯脲类、二氨基杂环类中的一种。The environment-friendly color material adopts one of diaminostilbene disulfonic acid, 4.4-diaminodiphenylurea, and diaminoheterocycle.
所述阻燃剂采用三氧化二锑或氢氧化镁。The flame retardant adopts antimony trioxide or magnesium hydroxide.
进一步的，所述阻燃剂采用活性氧化铝复合三氧化二锑，所述活性氧化铝复合三氧化二锑的制备方法，包括如下步骤：步骤i，将三氯化锑和三氯化铝加入至无水乙醇中搅拌均匀，直至完全溶解，得到溶解醇液，其中三氯化锑和三氯化铝的质量比为3-5:2，且所述三氯化锑在无水乙醇中的浓度为100-150g/L，搅拌速度为1000-2000r/min；步骤ii，将饱和氨水通入至溶解醇液中直至沉淀不再形成，然后过滤并采用蒸馏水洗涤，得到沉淀物，经恒温烘干得到活性氧化铝复合三氧化锑，其中，饱和氨水的通入量为5-10mL/min,
时间为60-120min，恒温烘干的温度为200-250℃。Further, the flame retardant adopts activated alumina composite antimony trioxide, and the preparation method of the activated alumina composite antimony trioxide includes the following steps: step i, adding antimony trichloride and aluminum trichloride into Stir evenly in dehydrated ethanol until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 3-5:2, and the ratio of the antimony trichloride in dehydrated ethanol is 3-5:2. The concentration is 100-150g/L, and the stirring speed is 1000-2000r/min; in step ii, saturated ammonia water is passed into the dissolved alcohol solution until the precipitation no longer forms, then filtered and washed with distilled water to obtain a precipitate, which is dried at a constant temperature Dry to obtain activated alumina composite antimony trioxide, wherein, the feeding amount of saturated ammonia water is 5-10mL/min,
The time is 60-120min, and the temperature of constant temperature drying is 200-250℃.
所述纳米碳酸钙采用轻质纳米碳酸钙。The nano calcium carbonate adopts light nano calcium carbonate.
再进一步的，所述纳米钛酸钙采用镀膜轻质纳米碳酸钙。Still further, the nano-calcium titanate is coated with light-weight nano-calcium carbonate.
所述镀膜轻质纳米碳酸钙的制备方法，包括如下步骤：The preparation method of the coated light-weight nano-calcium carbonate comprises the following steps:
步骤a，将氢氧化钙粉体与钛酸正丁酯共混加入至无水乙醇中，然后静置烘干，得到镀膜氢氧化钙粉体；所述钛酸正丁酯的加入量是氢氧化钙质量的10-20%，所述无水乙醇的质量是钛酸正丁酯 质量的150-200%，静置烘干的温度为80-100℃；所述氢氧化钙粉体的粒径为10-20μm；In step a, calcium hydroxide powder and n-butyl titanate are blended and added to absolute ethanol, and then left to dry to obtain coated calcium hydroxide powder; the amount of n-butyl titanate added is hydrogen 10-20% of the mass of calcium oxide, the mass of the anhydrous ethanol is 150-200% of the mass of n-butyl titanate, and the temperature for standing and drying is 80-100 °C; The diameter is 10-20μm;
步骤b，镀膜氢氧化钙粉料与聚乙烯吡咯烷酮搅拌混合形成共混料，然后静电纺丝形成单丝，并将单丝放置在密封环境中静置30-50min，得到预制纤维丝；所述聚乙烯吡咯烷酮的加入量是镀膜氢氧化钙质量的150-200%，静电纺丝的温度为135-145℃，所述密闭环境的压力为0.3-0.5MPa，温度为100-110℃，所述密闭环境由***蒸汽和水蒸气组成，且***蒸汽与水蒸气的体积比为10:0.3-0.8；In step b, the coated calcium hydroxide powder and polyvinylpyrrolidone are stirred and mixed to form a blend, and then electrospinned to form a monofilament, and the monofilament is placed in a sealed environment for 30-50 minutes to obtain a prefabricated filament; the The amount of polyvinylpyrrolidone added is 150-200% of the quality of the coated calcium hydroxide, the temperature of electrospinning is 135-145°C, the pressure of the closed environment is 0.3-0.5MPa, and the temperature is 100-110°C. The airtight environment is composed of ether vapor and water vapor, and the volume ratio of ether vapor to water vapor is 10:0.3-0.8;
步骤c，将预制纤维丝放入无水乙醇中微波反应30-50min，过滤后，得到镀膜轻质纳米碳酸钙；所述预制纤维丝在无水乙醇中的的浓度为100-200g/L，所述微波反应的功率为200-400W，温度为10-20℃；In step c, the prefabricated filaments are placed in absolute ethanol for microwave reaction for 30-50 min, and after filtration, the coated light nano-calcium carbonate is obtained; the concentration of the prefabricated filaments in absolute ethanol is 100-200 g/L, The power of the microwave reaction is 200-400W, and the temperature is 10-20°C;
步骤d，将过滤后的废液减压蒸馏，得到聚乙烯吡咯烷酮和无水乙醇，减压蒸馏的温度为80-90℃，压力为标准大气压的70-80%，所述聚乙烯吡咯烷酮回收用于步骤b，无水乙醇回收用于步骤a和步骤c。In step d, the filtered waste liquid is distilled under reduced pressure to obtain polyvinylpyrrolidone and dehydrated alcohol. The temperature of the vacuum distillation is 80-90° C., and the pressure is 70-80% of the standard atmospheric pressure. In step b, absolute ethanol is recovered for step a and step c.
进一步的，所述挤出造粒采用热熔造粒法，温度为160-170℃。Further, the extrusion granulation adopts a hot melt granulation method, and the temperature is 160-170°C.
进一步的，所述原液货色阻燃聚乳酸母料的质量占比为13-15%，聚乳酸切片的质量占比为85-87%。Further, the mass ratio of the raw liquid and the flame-retardant polylactic acid masterbatch is 13-15%, and the mass ratio of the polylactic acid chips is 85-87%.
进一步的，所述牵伸的拉力为0.5-0.9MPa。Further, the drawing force is 0.5-0.9 MPa.
从以上描述可以看出，本发明具备以下优点：As can be seen from the above description, the present invention has the following advantages:
1.本发明解决了现有阻燃聚酯纤维阻燃效果不佳的问题，利用聚乳酸粉体的熔融造粒方式将阻燃剂进行侵入式混合，实现聚乳酸粉体的阻燃特性提升，从而达到提升整体性能的提升。1. The present invention solves the problem of poor flame retardant effect of existing flame retardant polyester fibers, and uses the melt granulation method of polylactic acid powder to mix the flame retardant in an intrusive manner, so as to improve the flame retardant properties of polylactic acid powder. , so as to improve the overall performance.
2.本发明采用三氧化二锑作为阻燃剂，燃烧后形成稳定的熔融状态，在初期燃烧形成表面保护膜隔绝空气，若配合氧化铝的高热传导性，形成三氧化二锑热量均匀，提升保护液膜的面积。2. The present invention uses antimony trioxide as a flame retardant, which forms a stable molten state after combustion, and forms a surface protective film to isolate the air at the initial stage of combustion. The area of the protective liquid film.
3.本发明采用轻质碳酸钙作为填料，形成稳定的微孔体系，提升稳固性，在利用二氧化钛作为镀膜层的情况下，赋予碳酸钙良好的耐候性与抗菌性，同时减少了二氧化钛对有机分子的降解影响。3. The present invention uses light calcium carbonate as a filler to form a stable microporous system and improve stability. In the case of using titanium dioxide as a coating layer, calcium carbonate is given good weather resistance and antibacterial properties, while reducing the effect of titanium dioxide on organic compounds. Molecular degradation effects.
结合实施例详细说明本发明，但不对本发明的权利要求做任何限定。The present invention is described in detail with reference to the embodiments, but does not limit the claims of the present invention.
实施例1Example 1
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为65%，环保色料的质量占比为15%，阻燃剂的质量占比为15%，纳米碳酸钙的质量占比为5%；所述环保色料采用二氨基二苯乙烯二磺酸类；所述阻燃剂采用三氧化二锑；所述纳米碳酸钙采用轻质纳米碳酸钙；所述挤出造粒采用热熔造粒法，温度为160℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65%, the mass proportion of environmental protection pigment is 15%, the mass proportion of flame retardant is 15%, and the mass proportion of nano calcium carbonate is 5%. ; The environmentally friendly color material adopts diaminostilbene disulfonic acid; the flame retardant adopts antimony trioxide; the nano calcium carbonate adopts light nano calcium carbonate; the extrusion granulation adopts hot melting Granulation method, the temperature is 160 ℃;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为13%，聚乳酸切片的质量占比为87%；所述牵伸的拉力为0.5MPa。Step 2, spinning and drawing the raw solution colored flame retardant polylactic acid masterbatch and the polylactic acid chips to obtain the raw solution colored flame retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 87%; the tensile force of the drawing is 0.5MPa.
制备的纤维丝：极限氧指数30％，强度为 3.7cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared filaments: limiting oxygen index 30%, strength 3.7cN/dtex, color fastness to washing 5, sublimation fastness 5.
实施例2Example 2
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为82%，环保色料的质量占比为5%，阻燃剂的质量占比为10%，纳米碳酸钙的质量占比为3%；所述环保色料采用4.4-二氨基二苯脲类；所述阻燃剂采用氢氧化镁；所述纳米碳酸钙采用轻质纳米碳酸钙；所述挤出造粒采用热熔造粒法，温度为170℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 82%, the mass proportion of environmental protection pigment is 5%, the mass proportion of flame retardant is 10%, and the mass proportion of nano calcium carbonate is 3%. ; The environmentally friendly color material adopts 4.4-diaminodiphenylurea; the flame retardant adopts magnesium hydroxide; the nano calcium carbonate adopts light nano calcium carbonate; the extrusion granulation adopts hot melt granulation method , the temperature is 170℃;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为15%，聚乳酸切片的质量占比为85%；所述牵伸的拉力为0.9MPa。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 85%; the tensile force of the drawing is 0.9MPa.
制备的纤维丝：极限氧指数32％，强度为 3.9cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared filaments: limiting oxygen index 32%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
实施例3Example 3
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为73%，环保色料的质量占比为10%，阻燃剂的质量占比为13%，纳米碳酸钙的质量占比为4%；所述环保色料采用二氨基二苯乙烯二磺酸类、4.4-二氨基二苯脲类、二氨基杂环类中的一种；所述阻燃剂采用三氧化二锑或氢氧化镁；所述纳米碳酸钙采用轻质纳米碳酸钙；所述挤出造粒采用热熔造粒法，温度为165℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 73%, the mass proportion of environmental protection pigment is 10%, the mass proportion of flame retardant is 13%, and the mass proportion of nano calcium carbonate is 4%. ; The environmentally friendly colorant adopts one of diaminostilbene disulfonic acid, 4.4-diaminodiphenylurea, and diaminoheterocycle; the flame retardant adopts antimony trioxide or magnesium hydroxide ; Described nano calcium carbonate adopts light nano calcium carbonate; Described extrusion granulation adopts hot melt granulation method, and the temperature is 165 ℃;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为14%，聚乳酸切片的质量占比为86%；所述牵伸的拉力为0.7MPa。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 86%; the tensile force of the drawing is 0.7MPa.
制备的纤维丝：极限氧指数31％，强度为 3.8cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared filaments: limiting oxygen index 31%, strength 3.8cN/dtex, color fastness to washing 5, sublimation fastness 5.
实施例4Example 4
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为65%，环保色料的质量占比为15%，阻燃剂的质量占比为15%，纳米碳酸钙的质量占比为5%；所述环保色料采用二氨基二苯乙烯二磺酸类；所述阻燃剂采用活性氧化铝复合三氧化二锑，其制备方法，包括如下步骤：步骤i，将三氯化锑和三氯化铝加入至无水乙醇1L中搅拌均匀，直至完全溶解，得到溶解醇液，其中三氯化锑和三氯化铝的质量比为3:2，且所述三氯化锑在无水乙醇中的浓度为100g/L，搅拌速度为1000r/min；步骤ii，将饱和氨水通入至溶解醇液中直至沉淀不再形成，然后过滤并采用蒸馏水洗涤，得到沉淀物，经恒温烘干得到活性氧化铝复合三氧化锑，其中，饱和氨水的通入量为5mL/min,时间为60min，恒温烘干的温度为200℃；所述纳米碳酸钙采用采用镀膜轻质纳米碳酸钙，其镀膜轻质纳米碳酸钙的制备方法，包括如下步骤：步骤a，将氢氧化钙粉体100g与钛酸正丁酯共混加入至无水乙醇中，然后静置烘干，得到镀膜氢氧化钙粉体；所述钛酸正丁酯的加入量是氢氧化钙质量的10%，所述无水乙醇的质量是钛酸正丁酯 质量的150%，静置烘干的温度为80℃；所述氢氧化钙粉体的粒径为10μm；步骤b，镀膜氢氧化钙粉料与聚乙烯吡咯烷酮搅拌混合形成共混料，然后静电纺丝形成单丝，并将单丝放置在密封环境中静置30min，得到预制纤维丝；所述聚乙烯吡咯烷酮的加入量是镀膜氢氧化钙质量的150%，静电纺丝的温度为135℃，所述密闭环境的压力为0.3MPa，温度为100℃，所述密闭环境由***蒸汽和水蒸气组成，且***蒸汽与水蒸气的体积比为10:0.3；步骤c，将预制纤维丝放入无水乙醇1L中微波反应30min，过滤后，得到镀膜轻质纳米碳酸钙；所述预制纤维丝在无水乙醇中的的浓度为100g/L，所述微波反应的功率为200W，温度为10℃；步骤d，将过滤后的废液减压蒸馏，得到聚乙烯吡咯烷酮和无水乙醇，减压蒸馏的温度为80℃，压力为标准大气压的70%，所述聚乙烯吡咯烷酮回收用于步骤b，无水乙醇回收用于步骤a和步骤c；所述挤出造粒采用热熔造粒法，温度为160℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65%, the mass proportion of environmental protection pigment is 15%, the mass proportion of flame retardant is 15%, and the mass proportion of nano calcium carbonate is 5%. The environment-friendly color material adopts diaminostilbene disulfonic acid; the flame retardant adopts activated alumina compound antimony trioxide, and its preparation method includes the following steps: step i, mixing antimony trichloride and trioxide The aluminum chloride is added to 1 L of anhydrous ethanol and stirred evenly until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 3:2, and the antimony trichloride in anhydrous The concentration in the ethanol is 100 g/L, and the stirring speed is 1000 r/min; in step ii, saturated ammonia water is passed into the dissolved alcohol solution until the precipitation no longer forms, then filtered and washed with distilled water to obtain a precipitate, which is dried at a constant temperature Activated alumina composite antimony trioxide is obtained, wherein the feeding amount of saturated ammonia water is 5mL/min, the time is 60min, and the temperature of constant temperature drying is 200°C; The preparation method of coated light nano-calcium carbonate includes the following steps: step a, blending 100 g of calcium hydroxide powder with n-butyl titanate into absolute ethanol, and then standing to dry to obtain coated calcium hydroxide powder; the amount of n-butyl titanate added is 10% of the mass of calcium hydroxide, the quality of the dehydrated alcohol is 150% of the mass of n-butyl titanate, and the temperature for standing and drying is 80°C; The particle size of the calcium hydroxide powder is 10 μm; in step b, the coating calcium hydroxide powder is stirred and mixed with polyvinylpyrrolidone to form a blend, and then electrospinning to form a monofilament, and the monofilament is placed in a sealed environment Let stand for 30min to obtain prefabricated filaments; the amount of polyvinylpyrrolidone added is 150% of the quality of the coated calcium hydroxide, the temperature of electrospinning is 135°C, the pressure of the closed environment is 0.3MPa, and the temperature is 100°C , the airtight environment is composed of ether vapor and water vapor, and the volume ratio of ether vapor and water vapor is 10:0.3; step c, the prefabricated filaments are placed in 1 L of absolute ethanol for microwave reaction for 30min, and after filtration, a coating is obtained Light nano calcium carbonate; the concentration of the prefabricated filaments in absolute ethanol is 100g/L, the power of the microwave reaction is 200W, and the temperature is 10°C; step d, the filtered waste liquid is vacuum distilled , obtain polyvinylpyrrolidone and absolute ethanol, the temperature of vacuum distillation is 80 ℃, the pressure is 70% of standard atmospheric pressure, described polyvinylpyrrolidone is recovered for step b, and absolute ethanol is recovered for step a and step c; The extrusion granulation adopts the hot melt granulation method, and the temperature is 160°C;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为13%，聚乳酸切片的质量占比为87%；所述牵伸的拉力为0.5MPa。Step 2, spinning and drawing the raw solution colored flame retardant polylactic acid masterbatch and the polylactic acid chips to obtain the raw solution colored flame retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 87%; the tensile force of the drawing is 0.5MPa.
制备的纤维丝：极限氧指数33％，强度为 3.9cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared fiber yarn: limiting oxygen index 33%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
实施例5Example 5
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为82%，环保色料的质量占比为5%，阻燃剂的质量占比为10%，纳米碳酸钙的质量占比为3%；所述环保色料采用4.4-二氨基二苯脲类；所述阻燃剂采用活性氧化铝复合三氧化二锑，所述活性氧化铝复合三氧化二锑的制备方法，包括如下步骤：步骤i，将三氯化锑和三氯化铝加入至无水乙醇1L中搅拌均匀，直至完全溶解，得到溶解醇液，其中三氯化锑和三氯化铝的质量比为5:2，且所述三氯化锑在无水乙醇中的浓度为150g/L，搅拌速度为2000r/min；步骤ii，将饱和氨水通入至溶解醇液中直至沉淀不再形成，然后过滤并采用蒸馏水洗涤，得到沉淀物，经恒温烘干得到活性氧化铝复合三氧化锑，其中，饱和氨水的通入量为5mL/min,
时间为120min，恒温烘干的温度为250℃；所述纳米碳酸钙采用镀膜轻质纳米碳酸钙，其制备方法，包括如下步骤：步骤a，将氢氧化钙粉体100g与钛酸正丁酯共混加入至无水乙醇中，然后静置烘干，得到镀膜氢氧化钙粉体；所述钛酸正丁酯的加入量是氢氧化钙质量的20%，所述无水乙醇的质量是钛酸正丁酯 质量的200%，静置烘干的温度为100℃；所述氢氧化钙粉体的粒径为20μm；步骤b，镀膜氢氧化钙粉料与聚乙烯吡咯烷酮搅拌混合形成共混料，然后静电纺丝形成单丝，并将单丝放置在密封环境中静置50min，得到预制纤维丝；所述聚乙烯吡咯烷酮的加入量是镀膜氢氧化钙质量的200%，静电纺丝的温度为145℃，所述密闭环境的压力为0.5MPa，温度为110℃，所述密闭环境由***蒸汽和水蒸气组成，且***蒸汽与水蒸气的体积比为10:0.3-0.8；步骤c，将预制纤维丝放入无水乙醇1L中微波反应50min，过滤后，得到镀膜轻质纳米碳酸钙；所述预制纤维丝在无水乙醇中的的浓度为200g/L，所述微波反应的功率为400W，温度为20℃；步骤d，将过滤后的废液减压蒸馏，得到聚乙烯吡咯烷酮和无水乙醇，减压蒸馏的温度为90℃，压力为标准大气压的80%，所述聚乙烯吡咯烷酮回收用于步骤b，无水乙醇回收用于步骤a和步骤c；所述挤出造粒采用热熔造粒法，温度为170℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 82%, the mass proportion of environmental protection pigment is 5%, the mass proportion of flame retardant is 10%, and the mass proportion of nano calcium carbonate is 3%. ; The environmentally friendly colorant adopts 4.4-diaminodiphenylurea; the flame retardant adopts activated alumina composite antimony trioxide, and the preparation method of the activated alumina composite antimony trioxide comprises the following steps: step i, adding antimony trichloride and aluminum trichloride to 1 L of dehydrated alcohol and stirring, until completely dissolved, to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 5:2, and The concentration of the antimony trichloride in absolute ethanol is 150 g/L, and the stirring speed is 2000 r/min; step ii, the saturated ammonia water is passed into the dissolved alcohol solution until the precipitation is no longer formed, then filtered and washed with distilled water , obtain the precipitate, obtain the activated alumina composite antimony trioxide through constant temperature drying, wherein, the feeding amount of saturated ammonia water is 5mL/min,
The time is 120min, and the temperature of constant temperature drying is 250°C; the nano-calcium carbonate is made of coated light-weight nano-calcium carbonate, and the preparation method includes the following steps: step a, 100 g of calcium hydroxide powder and n-butyl titanate are mixed The blend is added into absolute ethanol, and then left to dry to obtain coated calcium hydroxide powder; the addition amount of the n-butyl titanate is 20% of the calcium hydroxide quality, and the quality of the absolute ethanol is 200% of the mass of n-butyl titanate, and the temperature for standing and drying is 100°C; the particle size of the calcium hydroxide powder is 20 μm; in step b, the coating calcium hydroxide powder is stirred and mixed with polyvinylpyrrolidone to form a co-polymer. Mixing materials, and then electrospinning to form monofilaments, and placing the monofilaments in a sealed environment for 50 minutes to obtain prefabricated filaments; the amount of polyvinylpyrrolidone added is 200% of the quality of the coated calcium hydroxide, and electrospinning The temperature is 145 ℃, the pressure of the airtight environment is 0.5MPa, the temperature is 110 ℃, the airtight environment is composed of ether steam and water vapor, and the volume ratio of ether steam and water vapor is 10:0.3-0.8; step c, put the prefabricated filaments into 1 L of absolute ethanol for microwave reaction for 50 min, and after filtration, obtain coated light-weight nano-calcium carbonate; the concentration of the prefabricated filaments in absolute ethanol is 200 g/L, and the microwave reaction The power is 400W, and the temperature is 20 ° C; step d, the filtered waste liquid is vacuum distilled to obtain polyvinylpyrrolidone and anhydrous ethanol, the temperature of the vacuum distillation is 90 ° C, and the pressure is 80% of the standard atmospheric pressure, so the The polyvinylpyrrolidone is recovered for step b, and the anhydrous ethanol is recovered for step a and step c; the extrusion granulation adopts a hot melt granulation method, and the temperature is 170 ° C;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为15%，聚乳酸切片的质量占比为85%；所述牵伸的拉力为0.9MPa。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 85%; the tensile force of the drawing is 0.9MPa.
制备的纤维丝：极限氧指数35％，强度为 3.9cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared filaments: limiting oxygen index 35%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
实施例6Example 6
一种阻燃着色功能性环保纤维的制备方法，包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, comprising the following steps:
步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为73%，环保色料的质量占比为10%，阻燃剂的质量占比为13%，纳米碳酸钙的质量占比为4%；所述环保色料采用二氨基杂环类；所述阻燃剂采用活性氧化铝复合三氧化二锑，且其制备方法，包括如下步骤：步骤i，将三氯化锑和三氯化铝加入至无水乙醇1L中搅拌均匀，直至完全溶解，得到溶解醇液，其中三氯化锑和三氯化铝的质量比为2:1，且所述三氯化锑在无水乙醇中的浓度为1350g/L，搅拌速度为1500r/min；步骤ii，将饱和氨水通入至溶解醇液中直至沉淀不再形成，然后过滤并采用蒸馏水洗涤，得到沉淀物，经恒温烘干得到活性氧化铝复合三氧化锑，其中，饱和氨水的通入量为8mL/min,
时间为90min，恒温烘干的温度为230℃；所述纳米碳酸钙采用镀膜轻质纳米碳酸钙，且其制备方法，包括如下步骤：步骤a，将氢氧化钙粉体100g与钛酸正丁酯共混加入至无水乙醇中，然后静置烘干，得到镀膜氢氧化钙粉体；所述钛酸正丁酯的加入量是氢氧化钙质量的15%，所述无水乙醇的质量是钛酸正丁酯 质量的180%，静置烘干的温度为90℃；所述氢氧化钙粉体的粒径为15μm；步骤b，镀膜氢氧化钙粉料与聚乙烯吡咯烷酮搅拌混合形成共混料，然后静电纺丝形成单丝，并将单丝放置在密封环境中静置40min，得到预制纤维丝；所述聚乙烯吡咯烷酮的加入量是镀膜氢氧化钙质量的180%，静电纺丝的温度为140℃，所述密闭环境的压力为0.4MPa，温度为105℃，所述密闭环境由***蒸汽和水蒸气组成，且***蒸汽与水蒸气的体积比为10:0.5；步骤c，将预制纤维丝放入无水乙醇1L中微波反应40min，过滤后，得到镀膜轻质纳米碳酸钙；所述预制纤维丝在无水乙醇中的的浓度为150g/L，所述微波反应的功率为300W，温度为15℃；步骤d，将过滤后的废液减压蒸馏，得到聚乙烯吡咯烷酮和无水乙醇，减压蒸馏的温度为85℃，压力为标准大气压的75%，所述聚乙烯吡咯烷酮回收用于步骤b，无水乙醇回收用于步骤a和步骤c；所述挤出造粒采用热熔造粒法，温度为165℃；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and extrude and granulate through a screw extruder after drying to obtain a raw liquid coloring flame retardant polylactic acid masterbatch; the raw liquid coloring and flame retardant polylactic acid masterbatch; In the polylactic acid masterbatch, the mass proportion of polylactic acid powder is 73%, the mass proportion of environmental protection pigment is 10%, the mass proportion of flame retardant is 13%, and the mass proportion of nano calcium carbonate is 4%. The environment-friendly coloring material adopts diamino heterocycles; the flame retardant adopts activated alumina compound antimony trioxide, and the preparation method thereof includes the following steps: Step i, combining antimony trichloride and aluminum trichloride with Add it to 1 L of absolute ethanol and stir until it is completely dissolved to obtain a dissolved alcohol solution, wherein the mass ratio of antimony trichloride and aluminum trichloride is 2:1, and the ratio of the antimony trichloride in the absolute ethanol is 2:1. The concentration is 1350g/L, and the stirring speed is 1500r/min; in step ii, saturated ammonia water is passed into the dissolved alcohol solution until the precipitation is no longer formed, then filtered and washed with distilled water to obtain the precipitate, which is dried at a constant temperature to obtain active oxidation Aluminum composite antimony trioxide, wherein, the feeding amount of saturated ammonia water is 8mL/min,
The time is 90min, and the temperature of constant temperature drying is 230°C; the nano-calcium carbonate adopts coated light-weight nano-calcium carbonate, and the preparation method includes the following steps: step a, 100 g of calcium hydroxide powder is mixed with n-butyl titanate The ester is blended and added to absolute ethanol, and then left to dry to obtain coated calcium hydroxide powder; the amount of n-butyl titanate added is 15% of the mass of calcium hydroxide, and the mass of the absolute ethanol is 15%. It is 180% of the mass of n-butyl titanate, and the temperature for standing and drying is 90°C; the particle size of the calcium hydroxide powder is 15 μm; in step b, the coating calcium hydroxide powder is stirred and mixed with polyvinylpyrrolidone to form The blend material is then electrospun to form monofilaments, and the monofilaments are placed in a sealed environment for 40 minutes to obtain prefabricated filaments; the amount of polyvinylpyrrolidone added is 180% of the quality of the coated calcium hydroxide, and the electrospinning The temperature of the silk is 140°C, the pressure of the airtight environment is 0.4MPa, the temperature is 105°C, the airtight environment is composed of ether steam and water vapor, and the volume ratio of ether steam and water vapor is 10:0.5; Step c , put the prefabricated filaments into 1 L of absolute ethanol for microwave reaction for 40 min, and after filtration, obtain coated light nano-calcium carbonate; the concentration of the prefabricated filaments in absolute ethanol is 150 g/L, and the microwave reaction The power is 300W and the temperature is 15°C; in step d, the filtered waste liquid is subjected to vacuum distillation to obtain polyvinylpyrrolidone and absolute ethanol, the temperature of the vacuum distillation is 85°C, and the pressure is 75% of the standard atmospheric pressure. Polyvinylpyrrolidone is recovered for step b, and absolute ethanol is recovered for step a and step c; the extrusion granulation adopts hot melt granulation method, and the temperature is 165°C;
步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维；所述原液货色阻燃聚乳酸母料的质量占比为14%，聚乳酸切片的质量占比为86%；所述牵伸的拉力为0.7MPa。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber; The mass ratio of the lactic acid slices is 86%; the tensile force of the drawing is 0.7MPa.
制备的纤维丝：极限氧指数35％，强度为 3.9cN/dtex,耐洗色牢度5级，升华牢度5级。The prepared filaments: limiting oxygen index 35%, strength 3.9cN/dtex, color fastness to washing 5, sublimation fastness 5.
综上所述，本发明具有以下优点：To sum up, the present invention has the following advantages:
1.本发明解决了现有阻燃聚酯纤维阻燃效果不佳的问题，利用聚乳酸粉体的熔融造粒方式将阻燃剂进行侵入式混合，实现聚乳酸粉体的阻燃特性提升，从而达到提升整体性能的提升。1. The present invention solves the problem of poor flame retardant effect of existing flame retardant polyester fibers, and uses the melt granulation method of polylactic acid powder to mix the flame retardant in an intrusive manner, so as to improve the flame retardant properties of polylactic acid powder. , so as to improve the overall performance.
2.本发明采用三氧化二锑作为阻燃剂，燃烧后形成稳定的熔融状态，在初期燃烧形成表面保护膜隔绝空气，若配合氧化铝的高热传导性，形成三氧化二锑热量均匀，提升保护液膜的面积。2. The present invention uses antimony trioxide as a flame retardant, which forms a stable molten state after combustion, and forms a surface protective film to isolate the air at the initial stage of combustion. The area of the protective liquid film.
3.本发明采用轻质碳酸钙作为填料，形成稳定的微孔体系，提升稳固性，在利用二氧化钛作为镀膜层的情况下，赋予碳酸钙良好的耐候性与抗菌性，同时减少了二氧化钛对有机分子的降解影响。3. The present invention uses light calcium carbonate as a filler to form a stable microporous system and improve stability. In the case of using titanium dioxide as a coating layer, calcium carbonate is given good weather resistance and antibacterial properties, while reducing the effect of titanium dioxide on organic compounds. Molecular degradation effects.
可以理解的是，以上关于本发明的具体描述，仅用于说明本发明而并非受限于本发明实施例所描述的技术方案。本领域的普通技术人员应当理解，仍然可以对本发明进行修改或等同替换，以达到相同的技术效果；只要满足使用需要，都在本发明的保护范围之内。It can be understood that the above specific description of the present invention is only used to illustrate the present invention and is not limited to the technical solutions described in the embodiments of the present invention. Those of ordinary skill in the art should understand that the present invention can still be modified or equivalently replaced to achieve the same technical effect; as long as it meets the needs of use, it is within the protection scope of the present invention.
Claims (10)
- 一种阻燃着色功能性环保纤维的制备方法，其特征在于：包括如下步骤：A preparation method of flame-retardant coloring functional environmental protection fiber, which is characterized in that: comprising the following steps:步骤1：将聚乳酸粉体、环保色料、阻燃剂和纳米碳酸钙混合均匀，干燥后经螺杆挤出机挤出造粒得到原液着色阻燃聚乳酸母粒；Step 1: Mix the polylactic acid powder, the environmentally friendly colorant, the flame retardant and the nano calcium carbonate uniformly, and after drying, extrude and granulate through a screw extruder to obtain a raw liquid coloring flame retardant polylactic acid masterbatch;步骤2，将原液着色阻燃聚乳酸母粒与聚乳酸切片进行纺丝和牵伸得到原液着色阻燃聚乳酸纤维。Step 2, spinning and drawing the dope-colored flame-retardant polylactic acid masterbatch and the polylactic acid chips to obtain the dope-colored flame-retardant polylactic acid fiber.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述原液着色阻燃聚乳酸母料中，聚乳酸粉体的质量占比为65-82%，环保色料的质量占比为5-15%，阻燃剂的质量占比为12-15%，纳米碳酸钙的质量占比为3-5%。The method for preparing flame-retardant coloring functional environmentally friendly fibers according to claim 1, characterized in that: in the raw solution coloring flame-retardant polylactic acid masterbatch, the mass proportion of polylactic acid powder is 65-82%, and the environmental protection color is 65-82%. The mass ratio of the material is 5-15%, the mass ratio of the flame retardant is 12-15%, and the mass ratio of the nano calcium carbonate is 3-5%.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述环保色料采用二氨基二苯乙烯二磺酸类、4.4-二氨基二苯脲类、二氨基杂环类中的一种。The preparation method of flame-retardant coloring functional environmental protection fiber according to claim 1, characterized in that: the environmental protection color material adopts diaminostilbene disulfonic acid, 4.4-diaminodiphenylurea, diaminodiphenylurea, etc. One of the ring classes.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述阻燃剂采用三氧化二锑或氢氧化镁。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 1, wherein the flame retardant is antimony trioxide or magnesium hydroxide.
- 根据权利要求4所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述阻燃剂采用活性氧化铝复合三氧化二锑。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 4, wherein the flame retardant adopts activated alumina compounded with antimony trioxide.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述纳米碳酸钙采用轻质纳米碳酸钙。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 1, wherein the nano-calcium carbonate is light nano-calcium carbonate.
- 根据权利要求6所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述纳米钛酸钙采用镀膜轻质纳米碳酸钙。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 6, wherein the nano-calcium titanate is coated with light-weight nano-calcium carbonate.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述挤出造粒采用热熔造粒法，温度为160-170℃。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 1, wherein the extrusion granulation adopts a hot-melt granulation method, and the temperature is 160-170°C.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述原液货色阻燃聚乳酸母料的质量占比为13-15%，聚乳酸切片的质量占比为85-87%。The method for preparing flame-retardant colored functional environmentally friendly fibers according to claim 1, characterized in that: the mass ratio of the raw solution or the flame-retardant polylactic acid masterbatch is 13-15%, and the mass ratio of the polylactic acid chips is 85-87%.
- 根据权利要求1所述的阻燃着色功能性环保纤维的制备方法，其特征在于：所述牵伸的拉力为0.5-0.9MPa。The method for preparing flame-retardant coloring functional environmentally friendly fibers according to claim 1, wherein the drawing force is 0.5-0.9 MPa.
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