CN107366039A - It is crosslinked the preparation method and product of PLLA/low molecule amount PLLA blended fiber - Google Patents

It is crosslinked the preparation method and product of PLLA/low molecule amount PLLA blended fiber Download PDF

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Publication number
CN107366039A
CN107366039A CN201710542617.XA CN201710542617A CN107366039A CN 107366039 A CN107366039 A CN 107366039A CN 201710542617 A CN201710542617 A CN 201710542617A CN 107366039 A CN107366039 A CN 107366039A
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plla
low molecule
crosslinking
molecule amount
preparation
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CN107366039B (en
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苏娟娟
韩建
朱凡
孟扬
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Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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Zhejiang Sci Tech University ZSTU
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    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent

Abstract

The present invention relates to a kind of preparation method for being crosslinked PLLA/low molecule amount PLLA blended fiber, comprise the following steps：1) HMW PLLA is subjected to electron beam irradiation crosslinking, crosslinking PLLA is made；2) PLLA will be crosslinked and low molecule amount PLLA passes through melting mixing, and extruding pelletization, obtain blend；The mass fraction that PLLA is crosslinked in the blend is 5~50%, and the mass fraction of the low molecule amount PLLA is 50~95%；3) blend is subjected to melt spinning, produces crosslinking PLLA/low molecule amount PLLA blended fiber.The invention further relates to the product that above-mentioned preparation method is prepared.The preparation method process is simple, and production technology is controllable.Prepared polylactic acid blend fiber has abundant shish kebab superlattice structures, and its crystallinity is 40~60%, and heated dry air shrinkage factor is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.

Description

It is crosslinked the preparation method of PLLA/low molecule amount PLLA blended fiber And product
Technical field
The present invention relates to the preparation field of acid fiber by polylactic, and in particular to one kind crosslinking PLLA/low molecule amount is left Revolve the preparation method and product of polylactic acid blend fiber.
Background technology
PLA (Poly Lactic Acid, PLA) is by the various reproducible natural moneys such as starch, cellulose, polysaccharide Source by hydrolysis, fermentation be made lactic acid, aggregated obtained new polyester material, be it is a kind of can be degradable it is environmentally friendly Resin.
PLA has excellent biocompatibility, good mechanical performance and physical property so that it is in packaging, biology The fields such as medical treatment, automotive electronics have a wide range of applications, and also have potential application value in chemical fibre and non-woven field.
But at this stage, because the crystallization of PLA is slow, even in spinning process under strongly tensile flow field active force, according to So it is difficult to the PLA fibers for obtaining high-crystallinity (55-60%).And heat endurance poor caused by low-crystallinity (20-30%) Have a strong impact on its performance.
Solve acid fiber by polylactic to be to improve its heat endurance using the key issue of limitation.Generally solves its heat endurance Mode can be by improving its crystallinity, as Chinese invention patent (A of CN 106366594) is open a kind of three-dimensional containing PLA The preparation method of the high-toughness polylactic acid blend of compound, this method using the dextrorotation PLA of high-optical-purity as nucleator and PLLA mixes at room temperature, obtains the high-toughness polylactic acid blend of the stereo complex containing PLA.This method is logical Raising crystallinity is crossed to improve its heat resistance, improves its heat resistance compared to by crystallinity, the change of crystal habit is to resistance to Hot improvement is more effective.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to it is left to provide a kind of crosslinking PLLA/low molecule amount The preparation method and product of polylactic acid blend fiber are revolved, this method can improve shish-kebab superlattices knot in blended fiber The content of structure, and the heated dry air shrinkage factor and boiling water shrinkage of blended fiber can be greatly lowered, acquisition being capable of extensive use High heat-resisting blended fiber.
Technical scheme provided by the present invention is：
A kind of preparation method for being crosslinked PLLA/low molecule amount PLLA blended fiber, comprises the following steps：
1) HMW PLLA is subjected to electron beam irradiation crosslinking, crosslinking PLLA is made；
2) PLLA will be crosslinked and low molecule amount PLLA passes through melting mixing, extruding pelletization, be blended Thing；The mass fraction that PLLA is crosslinked in the blend is 5~50%, the quality of the low molecule amount PLLA Fraction is 50~95%；
3) blend is subjected to melt spinning, produces crosslinking PLLA/low molecule amount PLLA blended fiber.
In above-mentioned technical proposal, by being crosslinked PLLA (hereinafter referred to as CPLLA) and low molecule amount PLLA (hereinafter referred to as LPLLA) is blended, and obtains blended fiber through melt spinning.CPLLA is by being cross-linked to form chemistry in blend Cross-linked network structure, different from the characteristic that is easy to sliding and disentanglement of the physical entanglement network under outer field action, chemical crosslinking Network structure has permanent and stability.As shown in Figure 1 in spinning process, CPLLA chemical crosslinking net under outer field action Network sweeps along LPLLA molecules deformation of chain, orientation generation shish, and may advantageously facilitate being stabilized for the shish generated, Stable shish further triggers the LPLLA short chains of surrounding unperturbed state to crystallize generation kebab, ultimately forms shish- Kebab superlattice structures, so as to obtain the polylactic acid blend fiber that heat endurance significantly improves.
Preferably, electron beam irradiation crosslinking refers in the step 1)：HMW PLLA is compressed to 0.3~ Thin plate thick 0.8mm, it is placed in carrying out electron beam irradiation crosslinking in electron accelerator, irradiation dose is 5~10KGy, is made and hands over Join PLLA.The gel content of the crosslinking PLLA is controlled 5~30%.
Further preferably, the HMW PLLA is compressed to the thin of 0.5mm thickness at 200 DEG C under the conditions of 5MPa Plate, using progress electron beam irradiation crosslinking in 1.7MeV electron accelerators.
Preferably, the mass fraction that PLLA is crosslinked in the step 2) blend is 5~15%, the low molecule The mass fraction for measuring PLLA is 85~95%.
Preferably, melting mixing uses masterbatch with low molecule amount PLLA as raw material in the step 2).
Preferably, the preparation of the masterbatch：Crosslinking PLLA and low molecule amount PLLA are dissolved in dichloro Methane, and pour into ethanol, sediment is obtained, masterbatch is obtained after drying.
Preferably, the mass ratio that PLLA and low molecule amount PLLA are crosslinked in the masterbatch is 1:0.9~ 1.1.More preferably 1:1.
Preferably, the temperature of melting mixing is 180~220 DEG C in the step 2).More preferably 200 DEG C.
Preferably, the condition of melt spinning is in the step 3)：190~250 DEG C of spinning temperature, winding speed 100~ 500m/min, 100~150 DEG C of hot gas spring temperature, draw ratio 1~5.
Preferably, the weight average molecular weight of the HMW PLLA is 5~19 × 105G/mol, low molecule amount are left The weight average molecular weight for revolving PLA is 1.5~3 × 105g/mol。
It is left-handed that the present invention also provides crosslinking PLLA/low molecule amount that a kind of preparation method described above is prepared Polylactic acid blend fiber.The blended fiber has abundant shish-kebab superlattice structures, and its crystallinity is 40~60%, Heated dry air shrinkage factor is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.
Compared with the existing technology, beneficial effects of the present invention are embodied in：
(1) preparation method process provided by the present invention is simple, and production technology is controllable.
(2) polylactic acid blend fiber fully biodegradable provided by the present invention, thus the fiber cannot be only used for work Journey field, it may also be used for medicine and hygiene fieldses.
(3) CPLLA processes have been cross-linked to form chemical crosslinking network structure in polylactic acid blend fiber provided by the present invention, Not only favourable CPLLA cross-linked network sweeps along LPLLA molecules deformation of chain, orientation generation shish, and may advantageously facilitate raw Into shish be stabilized, stable shish further triggers the LPLLA short chains of surrounding unperturbed state to crystallize generation Kebab, shish-kebab superlattice structures are ultimately formed, obtain the polylactic acid blend fiber that heat endurance significantly improves, its Crystallinity is 40~60%, and heated dry air shrinkage factor is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.
Brief description of the drawings
Fig. 1 is the schematic flow sheet that blended fiber forms shish-kebab superlattice structures in spinning process.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
It is 5 × 10 to take weight average molecular weight5G/mol HPLLA is 1.5 × 10 with weight average molecular weight5G/mol LPLLA conducts Raw material, step are as follows：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 5KGy, gel content is made For 5% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 10g and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 100m/min, 100 DEG C of hot gas spring temperature, draw ratio is in 190 DEG C of spinning temperature Melt spinning under conditions of 2 times, PLA blended fibers are made.
Specific method of testing：1) using the hot air shrinkage of single fiber thermal contraction test instrument test PLA blended fibers, survey Examination temperature is set as 140 DEG C, testing time 30min.2) boiling shrinkage of PLA blended fibers is tested under standard atmospheric conditions Rate, testing time 30min.
Percent thermal shrinkage is calculated by below equation：
In formula, L0For the initial length of fiber, L is the final lengths of the fiber after overheat contraction.
The PLA blended fibers measure its hot air shrinkage as 5.7% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 1.8%, its crystallinity is 42%, and Herman orientation index is 0.18.
Embodiment 2
It is 10 × 10 to take weight average molecular weight5G/mol HPLLA is 1.5 × 10 with weight average molecular weight5G/mol LPLLA makees It is as follows for raw material, step：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 7KGy, gel content is made For 10% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 10g and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 120m/min, 120 DEG C of hot gas spring temperature, draw ratio is in 210 DEG C of spinning temperature Melt spinning under conditions of 2.5 times, PLA blended fibers are made.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA blended fibers measure its hot air shrinkage as 4.7% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 1.2%, its crystallinity is 45%, and Herman orientation index is 0.19.
Embodiment 3
It is 10 × 10 to take weight average molecular weight5G/mol HPLLA is 1.5 × 10 with weight average molecular weight5G/mol LPLLA makees It is as follows for raw material, step：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 8KGy, gel content is made For 15% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 10g and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 240 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 200m/min, 120 DEG C of hot gas spring temperature, draw ratio is in 230 DEG C of spinning temperature Melt spinning under conditions of 3.5 times, PLA blended fibers are made.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA blended fibers measure its hot air shrinkage as 3.8% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 0.9%, its crystallinity is 49%, and Herman orientation index is 0.23.
Embodiment 4
It is 17 × 10 to take weight average molecular weight5G/mol HPLLA is 2.5 × 10 with weight average molecular weight5G/mol LPLLA makees It is as follows for raw material, step：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 8KGy, gel content is made For 15% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 10g and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 300m/min, 130 DEG C of hot gas spring temperature, draw ratio is in 230 DEG C of spinning temperature Melt spinning under conditions of 3.5 times, PLA blended fibers are made.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA blended fibers measure its hot air shrinkage as 3.4% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 0.7%, its crystallinity is 52%, and Herman orientation index is 0.24.
Embodiment 5
It is 19 × 10 to take weight average molecular weight5G/mol HPLLA is 3 × 10 with weight average molecular weight5G/mol LPLLA conducts Raw material, step are as follows：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 8KGy, gel content is made For 15% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 15g and 35g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 500m/min, 150 DEG C of hot gas spring temperature, draw ratio is in 250 DEG C of spinning temperature Melt spinning under conditions of 5 times, PLA blended fibers are made.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA blended fibers measure its hot air shrinkage as 3.2% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 0.4%, its crystallinity is 57%, and Herman orientation index is 0.29.
Embodiment 6
It is 19 × 10 to take weight average molecular weight5G/mol HPLLA is 3 × 10 with weight average molecular weight5G/mol LPLLA conducts Raw material, step are as follows：
1) HMW PLLA (HPLLA) is compressed to the thick thin plates of 0.5mm under the conditions of 200 DEG C, 5MPa, and The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerators, irradiation dose 10KGy, gel content is made For 25% crosslinking PLLA (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml dichloromethane, magnetic agitation 3h under normal temperature condition will be mixed Close solution to be poured into while stirring in 50ml absolute ethyl alcohols, obtain CPLLA/LPLLA mass ratioes as 1:1 sediment, in vacuum Masterbatch is dried to obtain in baking oven；
3) by masterbatch above-mentioned 15g and 35g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained CPLLA/LPLLA blends；
4) blend is wound into speed 500m/min, 150 DEG C of hot gas spring temperature, draw ratio is in 230 DEG C of spinning temperature Melt spinning under conditions of 5 times, PLA blended fibers are made.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA blended fibers measure its hot air shrinkage as 3.4% through single fiber thermal contraction test instrument；In normal atmosphere Under the conditions of measure its boiling water shrinkage as 0.6%, its crystallinity is 52%, and Herman orientation index is 0.26.
Comparative example 1
1) it is 2 × 10 by weight average molecular weight5G/mol LPLLA raw materials 50g is melted under the conditions of 240 DEG C by miniature extruder Melt extruding pelletization, obtain LPLLA pellets；
2) pellet is wound into speed 100m/min, 100 DEG C of hot gas spring temperature, draw ratio is in 240 DEG C of spinning temperature PLA fibers are made in melt spinning under conditions of 2.5 times.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA fibers measure its hot air shrinkage as 20% through single fiber thermal contraction test instrument；In standard atmosphere condition Under measure its boiling water shrinkage as 7.8%, its crystallinity is 27%, and Herman orientation index is 0.12.
Comparative example 2
1) it is 2 × 10 by weight average molecular weight5G/mol LPLLA raw materials 50g is melted under the conditions of 240 DEG C by miniature extruder Melt extruding pelletization, obtain LPLLA pellets；
2) pellet is wound into speed 300m/min, 120 DEG C of hot gas spring temperature, draw ratio is in 250 DEG C of spinning temperature PLA fibers are made in melt spinning under conditions of 4.5 times.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA fibers measure its hot air shrinkage as 12% through single fiber thermal contraction test instrument；In standard atmosphere condition Under measure its boiling water shrinkage as 4.5%, its crystallinity is 30%, and Herman orientation index is 0.14.
Comparative example 3
1) it is 15 × 10 by weight average molecular weight5G/mol LPLLA raw materials 50g is by miniature extruder, under the conditions of 200 DEG C Melting extrusion is granulated, and obtains LPLLA pellets；
2) pellet is wound into speed 300m/min, 130 DEG C of hot gas spring temperature, draw ratio is in 260 DEG C of spinning temperature PLA fibers are made in melt spinning under conditions of 4.5 times.
The method of testing of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
The PLA fibers measure its hot air shrinkage as 23% through single fiber thermal contraction test instrument；In standard atmosphere condition Under measure its boiling water shrinkage as 8.5%, its crystallinity is 34%, and Herman orientation index is 0.15.

Claims (9)

  1. A kind of 1. preparation method for being crosslinked PLLA/low molecule amount PLLA blended fiber, it is characterised in that including Following steps：
    1) HMW PLLA is subjected to electron beam irradiation crosslinking, crosslinking PLLA is made；
    2) PLLA will be crosslinked and low molecule amount PLLA passes through melting mixing, and extruding pelletization, obtain blend；Institute The mass fraction for stating crosslinking PLLA in blend is 5~50%, the mass fraction of the low molecule amount PLLA For 50~95%；
    3) blend is subjected to melt spinning, produces crosslinking PLLA/low molecule amount PLLA blended fiber.
  2. 2. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 1, Characterized in that, electron beam irradiation crosslinking refers in the step 1)：HMW PLLA is compressed to 0.3~ Thin plate thick 0.8mm, it is placed in carrying out electron beam irradiation crosslinking in electron accelerator, irradiation dose is 5~10KGy, is made and hands over Join PLLA.
  3. 3. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 1, Characterized in that, melting mixing uses masterbatch with low molecule amount PLLA as raw material in the step 2).
  4. 4. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 3, Characterized in that, the preparation of the masterbatch：Crosslinking PLLA and low molecule amount PLLA are dissolved in dichloromethane, And pour into ethanol, sediment is obtained, masterbatch is obtained after drying.
  5. 5. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 4, Characterized in that, the mass ratio that PLLA and low molecule amount PLLA are crosslinked in the masterbatch is 1:0.9~1.1.
  6. 6. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 1, Characterized in that, the temperature of melting mixing is 180~220 DEG C in the step 2).
  7. 7. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 1, Characterized in that, the condition of melt spinning is in the step 3)：190~250 DEG C of spinning temperature, 100~500m/ of winding speed Min, 100~150 DEG C of hot gas spring temperature, draw ratio 1~5.
  8. 8. the preparation method of crosslinking PLLA/low molecule amount PLLA blended fiber according to claim 1, Characterized in that, the weight average molecular weight of the HMW PLLA is 5~19 × 105G/mol, low molecule amount are left-handed poly- The weight average molecular weight of lactic acid is 1.5~3 × 105g/mol。
  9. 9. a kind of crosslinking PLLA that preparation method as described in claim 1~8 is any is prepared/low molecule amount is left Revolve polylactic acid blend fiber.
CN201710542617.XA 2017-07-05 2017-07-05 It is crosslinked l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method and product Active CN107366039B (en)

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