CN107366039B - It is crosslinked l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method and product - Google Patents
It is crosslinked l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method and product Download PDFInfo
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- CN107366039B CN107366039B CN201710542617.XA CN201710542617A CN107366039B CN 107366039 B CN107366039 B CN 107366039B CN 201710542617 A CN201710542617 A CN 201710542617A CN 107366039 B CN107366039 B CN 107366039B
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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 crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method, includes the following steps: that high molecular weight l-lactic acid 1) is carried out electron beam irradiation crosslinking, crosslinking l-lactic acid is made；2) l-lactic acid will be crosslinked and low molecular weight l-lactic acid passes through melting mixing, extruding pelletization obtains blend；The mass fraction that l-lactic acid is crosslinked in the blend is 5~50%, and the mass fraction of the low molecular weight l-lactic acid is 50~95%；3) blend is subjected to melt spinning to get crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber.The invention further relates to the products that above-mentioned preparation method is prepared.The preparation method has a simple process, and production technology is controllable.Prepared polylactic acid blend fiber has shish-kebab superlattice structure abundant, and crystallinity is 40~60%, and heated dry air shrinking percentage is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.
Description
Technical field
The present invention relates to the preparation fields of acid fiber by polylactic, and in particular to a kind of crosslinking l-lactic acid/low molecular weight is left
Revolve the preparation method and product of polylactic acid blend fiber.
Background technique
Polylactic acid (Poly Lactic Acid, PLA) is by the various reproducible natural moneys such as starch, cellulose, polysaccharide
Source by hydrolysis, fermenting is made lactic acid, aggregated obtained new polyester material, be it is a kind of can be degradable it is environmentally friendly
Resin.
Polylactic acid 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, since the crystallization of polylactic acid is slow, even during the spinning process under strongly tensile flow field active force, according to
So it is difficult to obtain the PLA fiber of high-crystallinity (55-60%).And thermal stability poor caused by low-crystallinity (20-30%)
Seriously affect its service performance.
Acid fiber by polylactic is solved to be to improve its thermal stability using the critical issue of limitation.Usually solve its thermal stability
Mode can be by improving its crystallinity, as Chinese invention patent (106366594 A of CN) is open a kind of three-dimensional containing polylactic acid
The preparation method of the high-toughness polylactic acid blend of compound, this method using the dextrorotation polylactic acid of high-optical-purity as nucleating agent and
L-lactic acid mixes at room temperature, obtains the high-toughness polylactic acid blend of the stereo complex containing polylactic acid.This method is logical
Raising crystallinity is crossed to improve its heat resistance, compared to its heat resistance is improved by crystallinity, the change of crystal habit is to resistance to
Hot improvement is more effective.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to which it is left to provide a kind of crosslinking l-lactic acid/low molecular weight
The preparation method and product of polylactic acid blend fiber are revolved, this method can be improved shish-kebab superlattices knot in blended fiber
The content of structure, and the heated dry air shrinking percentage and boiling water shrinkage of blended fiber can be greatly lowered, acquisition can be widely applied
High heat resistance blended fiber.
Technical solution provided by the present invention are as follows:
A kind of crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method, includes the following steps:
1) high molecular weight l-lactic acid is subjected to electron beam irradiation crosslinking, crosslinking l-lactic acid is made；
2) l-lactic acid will be crosslinked and low molecular weight l-lactic acid passes through melting mixing, extruding pelletization is blended
Object；The mass fraction that l-lactic acid is crosslinked in the blend is 5~50%, the quality of the low molecular weight l-lactic acid
Score is 50~95%；
3) blend is subjected to melt spinning to get crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber.
In above-mentioned technical proposal, by being crosslinked l-lactic acid (hereinafter referred to as CPLLA) and low molecular weight l-lactic acid
(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 during the spinning process, the chemical crosslinking net of CPLLA under outer field action
Network sweeps along LPLLA molecule deformation of chain, orientation to generate shish, and may advantageously facilitate being stabilized for the shish generated,
The short chain crystallization of LPLLA that stable shish further causes surrounding unperturbed state generates kebab, ultimately forms shish-
Kebab superlattice structure, to obtain the polylactic acid blend fiber that thermal stability significantly improves.
Preferably, electron beam irradiation crosslinking refers in the step 1): high molecular weight l-lactic acid is compressed to 0.3~
The thin plate of 0.8mm thickness is placed in progress electron beam irradiation crosslinking in electron accelerator, and irradiation dose is 5~10KGy, is made and hands over
Join l-lactic acid.The gel content of the crosslinking l-lactic acid is controlled 5~30%.
Further preferably, the high molecular weight l-lactic acid 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 accelerator.
Preferably, the mass fraction that l-lactic acid is crosslinked in the step 2) blend is 5~15%, the low molecule
The mass fraction for measuring l-lactic acid is 85~95%.
Preferably, melting mixing uses masterbatch and low molecular weight l-lactic acid as raw material in the step 2).
Preferably, crosslinking l-lactic acid and low molecular weight l-lactic acid the preparation of the masterbatch: are dissolved in dichloro
Methane, and pour into ethyl alcohol, sediment is obtained, obtains masterbatch after drying.
Preferably, be crosslinked in the masterbatch l-lactic acid and low molecular weight l-lactic acid mass ratio be 1:0.9~
1.1.Further preferably 1:1.
Preferably, the temperature of melting mixing is 180~220 DEG C in the step 2).Further preferably 200 DEG C.
Preferably, in the step 3) melt spinning condition are as follows: 190~250 DEG C of spinning temperature, winding rate 100~
500m/min, 100~150 DEG C of hot gas spring temperature, draw ratio 1~5.
Preferably, the weight average molecular weight of the high molecular weight l-lactic acid is 5~19 × 105G/mol, low molecular weight are left
The weight average molecular weight for revolving polylactic acid is 1.5~3 × 105g/mol。
The present invention also provides a kind of crosslinking l-lactic acid/low molecular weight being prepared such as above-mentioned preparation method is left-handed
Polylactic acid blend fiber.The blended fiber has shish-kebab superlattice structure abundant, and crystallinity is 40~60%,
Heated dry air shrinking percentage is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.
Compared with the existing technology, the 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 fields.
(3) CPLLA process has been cross-linked to form chemical crosslinking network structure in polylactic acid blend fiber provided by the present invention,
Not only the cross-linked network of advantageous CPLLA sweeps along LPLLA molecule deformation of chain, orientation to generate shish, but also may advantageously facilitate raw
At shish be stabilized, the short chain crystallization of LPLLA that stable shish further causes surrounding unperturbed state generates
Kebab ultimately forms shish-kebab superlattice structure, obtains the polylactic acid blend fiber that thermal stability significantly improves,
Crystallinity is 40~60%, and heated dry air shrinking percentage is 3.2~6.0%, and boiling water shrinkage is 0.4~2.0%.
Detailed description of the invention
Fig. 1 is the flow diagram that blended fiber forms shish-kebab superlattice structure during the spinning process.
Specific embodiment
Below with reference to specific embodiment, the invention will be further described.
Embodiment 1
Taking weight average molecular weight is 5 × 105The HPLLA and weight average molecular weight of g/mol is 1.5 × 105The LPLLA conduct of g/mol
Raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 5KGy
For 5% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 10g above-mentioned masterbatch and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 190 DEG C of spinning temperature, rate 100m/min is wound, 100 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 2 times.
Specific test method: 1) it using the hot air shrinkage of single fiber thermal contraction test instrument test PLA blended fiber, surveys
Examination temperature is set as 140 DEG C, testing time 30min.2) boiling shrinkage of PLA blended fiber is tested under standard atmospheric conditions
Rate, testing time 30min.
Percent thermal shrinkage is calculate by the following formula:
In formula, L0For the initial length of fiber, L is the final lengths of the fiber after overheat contraction.
It is 5.7% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 1.8%, crystallinity 42%, Herman orientation index be 0.18.
Embodiment 2
Taking weight average molecular weight is 10 × 105The HPLLA and weight average molecular weight of g/mol is 1.5 × 105The LPLLA of g/mol makees
For raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 7KGy
For 10% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 10g above-mentioned masterbatch and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 210 DEG C of spinning temperature, rate 120m/min is wound, 120 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 2.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 4.7% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 1.2%, crystallinity 45%, Herman orientation index be 0.19.
Embodiment 3
Taking weight average molecular weight is 10 × 105The HPLLA and weight average molecular weight of g/mol is 1.5 × 105The LPLLA of g/mol makees
For raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 8KGy
For 15% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 10g above-mentioned masterbatch and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 240 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 230 DEG C of spinning temperature, rate 200m/min is wound, 120 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 3.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 3.8% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 0.9%, crystallinity 49%, Herman orientation index be 0.23.
Embodiment 4
Taking weight average molecular weight is 17 × 105The HPLLA and weight average molecular weight of g/mol is 2.5 × 105The LPLLA of g/mol makees
For raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 8KGy
For 15% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 10g above-mentioned masterbatch and 40g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 230 DEG C of spinning temperature, rate 300m/min is wound, 130 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 3.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 3.4% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 0.7%, crystallinity 52%, Herman orientation index be 0.24.
Embodiment 5
Taking weight average molecular weight is 19 × 105The HPLLA and weight average molecular weight of g/mol is 3 × 105The LPLLA conduct of g/mol
Raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 8KGy
For 15% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 15g above-mentioned masterbatch and 35g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 250 DEG C of spinning temperature, rate 500m/min is wound, 150 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 3.2% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 0.4%, crystallinity 57%, Herman orientation index be 0.29.
Embodiment 6
Taking weight average molecular weight is 19 × 105The HPLLA and weight average molecular weight of g/mol is 3 × 105The LPLLA conduct of g/mol
Raw material, steps are as follows:
1) high molecular weight l-lactic acid (HPLLA) is compressed to the thin plate of 0.5mm thickness under the conditions of 200 DEG C, 5MPa, and
The thin plate is placed in progress electron beam irradiation crosslinking in 1.7MeV electron accelerator, gel content is made in irradiation dose 10KGy
For 25% crosslinking l-lactic acid (CPLLA)；
2) 10g CPLLA and 10g LPLLA are dissolved in 150ml methylene chloride, magnetic agitation 3h under normal temperature condition will be mixed
It closes solution to be poured into while stirring in 50ml dehydrated alcohol, the sediment that CPLLA/LPLLA mass ratio is 1:1 is obtained, in vacuum
Masterbatch is dried to obtain in baking oven；
3) by 15g above-mentioned masterbatch and 35g LPLLA, melting extrusion is granulated under the conditions of miniature extruder, 200 DEG C, is obtained
CPLLA/LPLLA blend；
4) by the blend in 230 DEG C of spinning temperature, rate 500m/min is wound, 150 DEG C of hot gas spring temperature, draw ratio is
PLA blended fiber is made in melt spinning under conditions of 5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 3.4% that the PLA blended fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In normal atmosphere
Under the conditions of measure its boiling water shrinkage be 0.6%, crystallinity 52%, Herman orientation index be 0.26.
Comparative example 1
It 1) is 2 × 10 by weight average molecular weight5The LPLLA raw material 50g of g/mol passes through miniature extruder, melts under the conditions of 240 DEG C
Melt extruding pelletization, obtains LPLLA pellet；
2) by the pellet in 240 DEG C of spinning temperature, rate 100m/min is wound, 100 DEG C of hot gas spring temperature, draw ratio is
PLA fiber is made in melt spinning under conditions of 2.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 20% that the PLA fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In standard atmosphere condition
Under measure its boiling water shrinkage be 7.8%, crystallinity 27%, Herman orientation index be 0.12.
Comparative example 2
It 1) is 2 × 10 by weight average molecular weight5The LPLLA raw material 50g of g/mol passes through miniature extruder, melts under the conditions of 240 DEG C
Melt extruding pelletization, obtains LPLLA pellet；
2) by the pellet in 250 DEG C of spinning temperature, rate 300m/min is wound, 120 DEG C of hot gas spring temperature, draw ratio is
PLA fiber is made in melt spinning under conditions of 4.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 12% that the PLA fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In standard atmosphere condition
Under measure its boiling water shrinkage be 4.5%, crystallinity 30%, Herman orientation index be 0.14.
Comparative example 3
It 1) is 15 × 10 by weight average molecular weight5The LPLLA raw material 50g of g/mol is by miniature extruder, under the conditions of 200 DEG C
Melting extrusion is granulated, and obtains LPLLA pellet；
2) by the pellet in 260 DEG C of spinning temperature, rate 300m/min is wound, 130 DEG C of hot gas spring temperature, draw ratio is
PLA fiber is made in melt spinning under conditions of 4.5 times.
The test method of hot air shrinkage and boiling water shrinkage such as embodiment 1 is identical.
It is 23% that the PLA fiber, which measures its hot air shrinkage through single fiber thermal contraction test instrument,；In standard atmosphere condition
Under measure its boiling water shrinkage be 8.5%, crystallinity 34%, Herman orientation index be 0.15.
Claims (7)
1. a kind of crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method, which is characterized in that including
Following steps:
1) high molecular weight l-lactic acid is subjected to electron beam irradiation crosslinking, crosslinking l-lactic acid is made；
2) l-lactic acid will be crosslinked and low molecular weight l-lactic acid passes through melting mixing, extruding pelletization obtains blend；Institute
Stating and being crosslinked the mass fraction of l-lactic acid in blend is 5~50%, the mass fraction of the low molecular weight l-lactic acid
It is 50~95%；
Melting mixing is using masterbatch and low molecular weight l-lactic acid as raw material in the step 2)；The preparation of the masterbatch:
Crosslinking l-lactic acid and low molecular weight l-lactic acid are dissolved in methylene chloride, and poured into ethyl alcohol, sediment is obtained,
Masterbatch is obtained after drying；
3) described by blend progress melt spinning to get crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber
Being crosslinked l-lactic acid/low molecular weight l-lactic acid blended fiber includes shish-kebab superlattice structure.
2. crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method according to claim 1,
It is characterized in that, electron beam irradiation crosslinking refers in the step 1): high molecular weight l-lactic acid is compressed to 0.3~
The thin plate of 0.8mm thickness is placed in progress electron beam irradiation crosslinking in electron accelerator, and irradiation dose is 5~10KGy, is made and hands over
Join l-lactic acid.
3. crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method according to claim 1,
It is characterized in that, the mass ratio for being crosslinked l-lactic acid and low molecular weight l-lactic acid in the masterbatch is 1:0.9~1.1.
4. crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method according to claim 1,
It is characterized in that, the temperature of melting mixing is 180~220 DEG C in the step 2).
5. crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method according to claim 1,
It is characterized in that, in the step 3) melt spinning condition are as follows: 190~250 DEG C of spinning temperature, wind 100~500m/ of rate
Min, 100~150 DEG C of hot gas spring temperature, draw ratio 1~5.
6. crosslinking l-lactic acid/low molecular weight l-lactic acid blended fiber preparation method according to claim 1,
It is characterized in that, the weight average molecular weight of the high molecular weight l-lactic acid is 5~19 × 105G/mol, low molecular weight are left-handed poly-
The weight average molecular weight of lactic acid is 1.5~3 × 105g/mol。
7. a kind of crosslinking l-lactic acid that the preparation method as described in claim 1~6 is any is prepared/low molecular weight is left
Revolve polylactic acid blend fiber.
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