CN111058116B - Sheath-core PLA/PHBV composite fiber and preparation method thereof - Google Patents
Sheath-core PLA/PHBV composite fiber and preparation method thereof Download PDFInfo
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- CN111058116B CN111058116B CN201911189647.2A CN201911189647A CN111058116B CN 111058116 B CN111058116 B CN 111058116B CN 201911189647 A CN201911189647 A CN 201911189647A CN 111058116 B CN111058116 B CN 111058116B
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- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- 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
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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
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Abstract
本发明公开了一种皮芯型PLA/PHBV复合纤维及其制备方法，属于高分子材料领域。本发明的皮芯型PLA/PHBV复合纤维的制备方法具体为：(1)将皮层的原料聚乳酸PLA和芯层的原料聚(3‑羟基丁酸酯‑co‑3‑羟基戊酸酯)(PHBV)分别干燥；PLA和PHBV的含水率不高于200ppm；(2)按照复合纺丝比称取步骤(1)得到的PLA和PHBV原料进行复合纺丝，经熔融纺丝、侧吹风冷却、上油、卷绕、在线拉伸、热定型制得皮芯结构PLA/PHBV复合纤维，其中，所述的纺丝过程中采用的喷丝板的孔数为24～144孔。本发明制备得到的材料的断裂强度高，能够用于医用材料、农业用纺织品、一次性用品、包装材料等领域。The invention discloses a skin-core type PLA/PHBV composite fiber and a preparation method thereof, belonging to the field of polymer materials. The preparation method of the sheath-core PLA/PHBV composite fiber of the present invention is specifically as follows: (1) the raw material of the skin layer is polylactic acid PLA and the raw material of the core layer is poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) were dried separately; the moisture content of PLA and PHBV was not higher than 200ppm; (2) the PLA and PHBV raw materials obtained in step (1) were weighed according to the composite spinning ratio for composite spinning, and then melt-spun and side-blown for cooling. , oiling, winding, on-line drawing, heat-setting to obtain PLA/PHBV composite fiber with skin-core structure, wherein the number of holes of the spinneret used in the spinning process is 24-144 holes. The material prepared by the invention has high breaking strength and can be used in the fields of medical materials, agricultural textiles, disposable products, packaging materials and the like.
Description
Technical Field
The invention relates to a sheath-core PLA/PHBV composite fiber and a preparation method thereof, belonging to the field of high polymer materials.
Background
The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) is a biological material produced by using starch as a raw material and applying a fermentation engineering technology, is a biological polyester, is produced by bacteria, can be digested by the bacteria, can be completely decomposed into carbon dioxide, water and biomass under the condition of soil or composting, can be degraded and does not pollute the environment. But it also has some inherent performance defects, one of which is that it is difficult to spin and difficult to use industrially.
Currently, hofenus et al in switzerland [ Hufenus, r.; reifler, f.a.; Maniura-Weber, k.; spierings, A.; zinn, M.Biodegradable binary Fibers from Renewable resources, Melt-Spinning of Poly (lactic acid) and Poly [ (3-hydroxybutyl) -co- (3-hydroxyvalete)].Macromol.Mater.Eng.2012,297:75-84.]The core-sheath type PLA/PHBV composite fiber is prepared by taking PHBV as a core layer raw material and polylactic acid (PLA) as a skin layer raw material through a composite spinning method, and is multifilament and the T of the PLAgThe temperature is about 60 ℃, is far higher than the room temperature, has good spinnability, is positioned on the outer layer of the fiber, and overcomes the problem of fiber adhesion in the PHBV spinning process. However, the mechanical properties of the PLA/PHBV composite fiber are completely determined by PLA, the PHBV does not play a role, namely the significance of the PHBV is lost, and the fact proves that the fiber with excellent mechanical properties can be prepared by using the PHBV as a raw material. Research shows that only orthogonal alpha-type crystals exist in the core layer PHBV in the PLA/PHBV composite fiber with the sheath-core structure, and the orientation degree of the crystals is low, which indicates that the tensile stress applied to the PHBV in the spinning process is low, and the reason why the PHBV in the composite fiber does not play a role is shown.
Therefore, how to increase the stress applied to the core layer PHBV and fully play the function of the PHBV is a key technology for spinning the substances in the industrial production.
Disclosure of Invention
In order to solve at least one of the above problems, the present invention provides a sheath-core PLA/PHBV composite fiber which has high strength, can fully exert the effect of PHBV, can be industrially produced, can produce multifilaments, and has a high yield, and a method for producing the same.
The invention provides a preparation method of sheath-core PLA/PHBV composite fiber, which comprises the following steps:
(1) respectively drying polylactic acid (PLA) serving as a raw material of a skin layer and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) serving as a raw material of a core layer; the water content of PLA and PHBV is not higher than 200 ppm;
(2) and (2) weighing the PLA and PHBV raw materials obtained in the step (1) according to a composite spinning ratio, carrying out composite spinning, and carrying out melt spinning, side-blown cooling, oiling, winding, on-line stretching and heat setting to obtain the PLA/PHBV composite fiber with the sheath-core structure, wherein the number of holes of a spinneret plate adopted in the spinning process is 24-144 holes.
In one embodiment, the skin layer raw material polylactic acid PLA is dried in a vacuum oven for 8-48 hours at the drying temperature of 50-90 ℃;
in one embodiment, the core layer raw material poly (3-hydroxybutyrate-co-3-hydroxyvalerate) PHBV is dried in a vacuum oven for 8-48 hours at the drying temperature of 50-105 ℃;
in one embodiment, the skin layer raw material is PLA with a D-LA content of 10-50 mol%; the core layer is made of PHBV with the content of 3-Hydroxyvalerate (HV) of 0-100 mol%;
in one embodiment, the skin layer raw material is PLA with a D-LA content of 12-50 mol%;
in one embodiment, the PLA has a viscosity average molecular weight of 1.0X 105～1.0×106；
In one embodiment, when the HV content is 0, the PHBV is poly (3-hydroxybutyrate) (PHB); when the HV content is 100 mol%, the PHBV is PHV;
in one embodiment, said PHBV has a viscosity average molecular weight of 5.0X 104～1.0×106；
In one embodiment, the mass ratio of the skin layer to the core layer is 10: 90-90: 10;
in one embodiment, the skin layer melt extrusion temperature is 130-200 ℃;
in one embodiment, the melt extrusion temperature of the core layer is 150 to 200 ℃;
in one embodiment, in the spinning process, the temperature of cross air blowing is 20-35 ℃, the relative humidity of cooling air is 50-80%, and the speed of the cross air blowing is 0.5-1.5 m/s; the spinning speed is 4500-6000 m/min;
in one embodiment, the winding speed of the primary yarn in the winding step is 10-100 m/min;
in one embodiment, the heating mode in the in-line stretching process is CO2A laser irradiation heating mode;
in one embodiment, the CO is2The specific parameters of the laser irradiation heating mode are as follows: the temperature of on-line stretching is 60-80 ℃, the stretching multiple is 8-20 times, and the heat setting temperature is 70-120 ℃;
in one embodiment, the CO is2The distance between the laser irradiation heating point and the guide roller on the output side is not less than 10 cm.
The second purpose of the invention is the sheath-core PLA/PHBV composite fiber obtained by the preparation method of the sheath-core PLA/PHBV composite fiber.
The third purpose of the invention is a sheath-core PLA/PHBV composite fiber.
In one embodiment, said PHBV has a viscosity average molecular weight of 5.0X 104～1.0×106；
In one embodiment, the mass ratio of the skin layer to the core layer is 10: 90-90: 10.
the fourth purpose of the invention is the application of the sheath-core PLA/PHBV composite fiber in the fields of medical materials (suture, artificial skin), agricultural textile materials (harvest cloth, seedling substrate), disposable articles (pen, wiping cloth) and packaging materials (especially food packaging).
Has the advantages that:
(1) the preparation method of the sheath-core PLA/PHBV composite fiber is simple and easy to operate, can utilize a composite spinning device to spin, and can be used for industrial production.
(2) The sheath-core PLA/PHBV composite fiber obtained by the preparation method of the sheath-core PLA/PHBV composite fiber has the sheath layer of PLA and the core layer of PHBV, which are all resource-renewable and biodegradable raw materials and are environment-friendly materials.
(3) The PLA of the skin layer of the skin-core PLA/PHBV composite fiber is PLA with the content of a D-lactic acid structural unit (D-LA) of 10-50 mol%, the glass transition temperature of the PLA is higher than room temperature, and the adhesion phenomenon caused by low glass transition temperature of the PHBV can be overcome.
(4) The sheath-core PLA/PHBV composite fiber has high breaking strength which can reach more than 6.9cN/dtex and can reach 8.8cN/dtex at most, can be used for multifilament spinning, has high yield and is suitable for industrial production.
(5) The sheath material PLA of the sheath-core PLA/PHBV composite fiber is PLA with the content of a structural unit of dextrolactic acid being 10-50 mol%, the crystallinity is extremely low, the PLA is almost amorphous polymer, the stretching temperature is higher than the glass transition temperature of the sheath, the viscosity of the core layer is gradually increased along with the crystallization of the core layer PHBV, and the sheath layer is always in a high-elastic state in the stretching process, so that the stretching stress mainly acts in the core layer PHBV to be beneficial to the formation of beta type crystals, the fiber fully plays the role of the core layer PHBV, and the sheath-core PLA/PHBV composite fiber is prepared.
(6)CO2The laser irradiation heating drawing technology is an effective means for preparing high-strength fiber, and CO2CO in laser radiation heating technology2The laser energy is high, the fiber can be heated quickly and uniformly, and in addition, the energy of the laser is concentrated, so that the heating is reducedIn the hot zone, the deformation (thin neck) area is reduced, so that the deformation rate is obviously improved, the ordered structure of the fiber is improved, and the mechanical property of the fiber is improved.
(7) The invention is based on the content of D-lactic acid structure and CO2The effects of high strength, industrialization and full play of the PHBV function can be realized only by mutually matching the laser irradiation heating stretching temperature and the distance between the heating point and the output side guide wire roller.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
Measurement methods of breaking strength and breaking elongation: the test is carried out according to the national standard GB/T14344-.
Example 1
(1) PLA with the D-LA content of 10% (the viscosity average molecular weight is 2.0 multiplied by 10)5) Drying at 60 deg.C for 36h in vacuum oven, adding PHBV (viscosity average molecular weight of 3.9 × 10) with HV content of 2.5 mol%5) Drying in a vacuum oven at 80 deg.C for 24h, with water content of PLA and PHBV of 200 ppm.
(2) According to the following steps: 85 (mass ratio), adding the PLA and PHBV raw materials obtained in the step (1) into a hopper corresponding to a composite spinning machine, and performing melt spinning, side-blown cooling, oiling, winding, on-line stretching and heat setting to obtain the PLA/PHBV composite fiber with the sheath-core structure, wherein the melt extrusion temperature of the sheath layer in the melt spinning process is 160 ℃, the melt extrusion temperature of the core layer is 170 ℃, and the number of holes of a spinneret plate is 144; the temperature of the cross air blow is 30 ℃, the relative humidity of the cooling air is 65%, and the speed of the cross air blow is 1 m/s; the spinning speed is 5000 m/min; the primary filament winding speed in the winding process is 50m/min, and CO in the on-line stretching process2The temperature of laser irradiation heating online stretching is 80 ℃, the distance between the laser irradiation heating online stretching and the output side guide wire roller is 40cm, the stretching multiple is 15 times, and the heat setting temperature is 95 ℃.
The performance test of the prepared composite fiber shows that the breaking strength of the composite fiber is 6.9cN/dtex, and the elongation at break is 25%.
Example 2
(1) PLA with a D-LA content of 50% (viscosity average molecular weight of 1.5X 10)5) Drying at 55 deg.C for 48h in vacuum oven, adding PHBV (viscosity average molecular weight of 5.0 × 10) with HV content of 8.0 mol%5) Drying in a vacuum oven at 80 deg.C for 24 h; the water content of PLA and PHBV is 150 ppm;
(2) according to the following steps of 10: 90 (mass ratio) of the PLA and the PHBV raw materials obtained in the step (1) are weighed and added into a hopper corresponding to a composite spinning machine, and the PLA/PHBV composite fiber with the sheath-core structure is prepared by melt spinning, side-blown cooling, oiling, winding, on-line stretching and heat setting, wherein the melt extrusion temperature of the sheath layer in the melt spinning process is 160 ℃, the melt extrusion temperature of the core layer is 175 ℃, and the number of holes of a spinneret plate is 70; the temperature of the cross air blow is 20 ℃, the relative humidity of the cooling air is 80 percent, and the speed of the cross air blow is 0.5 m/s; the spinning speed is 4500 m/min; the winding speed of the primary filament in the winding process is 20m/min, and CO in the on-line stretching process2The temperature of laser irradiation heating online stretching is 65 ℃, the distance between the laser irradiation heating online stretching and the guide roll at the output side is 30cm, the stretching multiple is 20 times, and the heat setting temperature is 100 ℃.
The performance test of the prepared composite fiber shows that the breaking strength of the composite fiber is 7.8cN/dtex, and the elongation at break is 10%.
Example 3
(1) PLA (viscosity average molecular weight of 2.0 multiplied by 10) with the D-LA content of 12 percent5) Drying at 60 deg.C for 36h in vacuum oven, adding PHBV (viscosity average molecular weight of 3.9 × 10) with HV content of 2.5 mol%5) Drying at 80 deg.C for 24 hr in vacuum oven, with water content of PLA and PHBV of 100 ppm;
(2) according to the following steps of 20: 80 (mass ratio) of the PLA and the PHBV raw materials obtained in the step (1) are weighed and added into a hopper corresponding to a composite spinning machine, and the PLA/PHBV composite fiber with the sheath-core structure is prepared by melt spinning, side-blown cooling, oiling, winding, on-line stretching and heat setting, wherein the melt extrusion temperature of the sheath layer is 170 ℃, the melt extrusion temperature of the core layer is 170 ℃ in the melt spinning process, and the core layer is sprayedThe number of the holes of the silk plate is 24; the temperature of the cross air blow is 35 ℃, the relative humidity of the cooling air is 50 percent, and the speed of the cross air blow is 1.5 m/s; the spinning speed is 6000 m/min; the winding speed of the primary filament in the winding process is 30m/min, and CO in the on-line stretching process2The temperature of laser irradiation heating on-line stretching is 75 ℃, the distance between the laser irradiation heating on-line stretching and the output side guide wire rollers is 50cm, the stretching multiple is 20 times, and the heat setting temperature is 95 ℃.
The performance test of the prepared composite fiber shows that the breaking strength of the composite fiber is 8.8cN/dtex, and the elongation at break is 9.8%.
Example 4
(1) PLA with the D-LA content of 10% (viscosity average molecular weight is 1.8 multiplied by 10)5) Drying at 60 deg.C for 36h in vacuum oven, adding PHBV (viscosity average molecular weight of 3.0 × 10) with HV content of 2.5 mol%5) Drying at 80 deg.C for 24h in a vacuum oven for use, with water content of PLA and PHBV of 150 ppm;
(2) according to the following steps of 20: 80 (mass ratio) of the PLA and the PHBV raw materials obtained in the step (1) are weighed and added into a hopper corresponding to a composite spinning machine, and the PLA/PHBV composite fiber with the sheath-core structure is prepared by melt spinning, side-blown cooling, oiling, winding, on-line stretching and heat setting, wherein the melt extrusion temperature of the sheath layer in the melt spinning process is 165 ℃, the melt extrusion temperature of the core layer is 170 ℃, and the number of holes of a spinneret plate is 40; the temperature of the cross air blow is 25 ℃, the relative humidity of the cooling air is 60 percent, and the speed of the cross air blow is 1 m/s; the spinning speed is 4500 m/min; the winding speed of the primary filament in the winding process is 30m/min, and CO in the on-line stretching process2The temperature of laser irradiation heating online stretching is 80 ℃, the distance between the laser irradiation heating online stretching and the output side guide wire roller is 45cm, the stretching multiple is 15 times, and the heat setting temperature is 90 ℃.
The performance test of the prepared composite fiber shows that the breaking strength of the composite fiber is 7.1cN/dtex, and the elongation at break is 36%.
Comparative example 1
PHBV in example 3 is omitted and other conditions or parameters are the same as those in example 3.
With PLA alone, the breaking strength was only 2.8cN/dtex and the elongation at break was 18.3%.
Comparative example 2
The D-LA content (%), the temperature (. degree. C.) for in-line stretching and the distance (cm) from the guide rolls on the output side were set as shown in Table 1 below, and the other conditions or parameters were the same as those in example 3. The specific test results are shown in table 1 below:
TABLE 1
As can be seen from table 1 above: the contents of D-LA are adjusted by serial numbers 1 and 2, the online stretching temperature is adjusted by serial numbers 3 and 4, the distance between the guide rollers on the output side is adjusted by serial numbers 5 and 6, and two parameters are adjusted by serial numbers 7 and 8 at the same time, so that the final test result shows that: the effect of sequence numbers 1 to 8 is far from the effect of the present application. Therefore, the effects of PHBV can be exhibited only when the D-LA content (%), the temperature of in-line stretching (. degree. C.), and the distance (cm) from the output-side guide roll are within the ranges of the present invention.
Comparative example 3
The D-LA contents were adjusted to 5%, 10%, 15%, 60%, and the other data were consistent with example 3, and the test results are shown in Table 2 below:
TABLE 2
| Serial number | D-LA content (%) | Breaking strength (cN/dtex) | Elongation at Break (%) |
| 1 | 5 | 5.2 | 8.6 |
| 2 | 10 | 8.5 | 9.4 |
| 3 | 15 | 8.7 | 10.7 |
| 4 | 60 | 4.9 | 9.3 |
As can be seen from table 2: number 1 belongs to less than the scope of the present application and number 4 belongs to more than the scope of the present application, as can be seen from the test results: too much or too little content of D-LA affects the strength of the final fiber.
Comparative example 4
The in-line stretching temperature in example 3 was adjusted to 45 ℃, 65 ℃, 100 ℃, and other parameters were consistent with those in example 3, and the specific test results are shown in table 3 below:
TABLE 3
As can be seen from table 3: when the drawing temperature is 45 ℃, drawing may be difficult due to less than Tg of PLA. When the drawing temperature is 100 ℃, the drawing ratio of 20 cannot be reached at all. Therefore, the technical effects of the present invention can be achieved only if the draft temperature is within the range of the present application.
Comparative example 5
The distances between the guide rolls on the output side in example 3 were adjusted to 5cm, 8cm and 12cm, and other parameters were kept in agreement with those in example 3, and the specific test results are shown in table 4 below:
TABLE 4
As can be seen from table 4: when the distance between the guide rollers at the output side is less than 10cm, the fiber is bonded with the guide rollers, and normal spinning cannot be performed. Therefore, it is important that the distance between the guide rolls on the output side is not less than 10 cm.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. A preparation method of sheath-core PLA/PHBV composite fiber is characterized by comprising the following steps:
(1) respectively drying a skin layer raw material polylactic acid (PLA) and a core layer raw material poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV); the water content of PLA and PHBV is not higher than 200 ppm;
(2) weighing the PLA and PHBV raw materials obtained in the step (1) according to the compounding ratio, and carrying out composite spinning, specifically, preparing the PLA/PHBV composite fiber with the skin-core structure through melt spinning, side-blown air cooling, oiling, winding, on-line stretching and heat setting; wherein the number of holes of the spinneret plate adopted in the spinning process is 24-144 holes;
the skin layer raw material is PLA with a D-LA (D-LA) structural unit content of 10-15 mol%;
the heating mode in the on-line stretching process is CO2Heating by laser irradiation; the specific parameters are as follows: the temperature of the on-line stretching is 60-80 ℃, and the stretching multiple is 8-20 times;
the CO is2The distance between the heating point of laser irradiation and the output side guide roll of the equipment used for composite spinning is not less than 50 cm;
the mass ratio of the skin layer to the core layer is 20: 80.
2. the preparation method of the sheath-core PLA/PHBV composite fiber according to claim 1, wherein the melt extrusion temperature of the sheath layer is 130-200 ℃ in the melt spinning process; the melt extrusion temperature of the core layer is 150-200 ℃.
3. The sheath-core PLA/PHBV composite fiber prepared by the method for preparing the sheath-core PLA/PHBV composite fiber according to claim 1 or 2.
4. Yarn, fabric, film, packaging material comprising the sheath-core PLA/PHBV composite fiber of claim 3.
5. The use of the sheath-core PLA/PHBV composite fiber according to claim 3 in the fields of medical materials, agricultural textiles, disposables or packaging materials.
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| CN113122957A (en) * | 2021-03-15 | 2021-07-16 | 南京千兆亿贸易合伙企业(有限合伙) | Preparation method of antibacterial and antiviral polyester filament containing PHBV material |
| CN114250528B (en) * | 2021-12-23 | 2023-08-04 | 台州益普高分子材料有限公司 | Environment-friendly coated yarn based on biological material and preparation method thereof |
| CN114540983A (en) * | 2022-03-22 | 2022-05-27 | 中国纺织科学研究院有限公司 | Low-cost biodegradable composite fiber and preparation method and application thereof |
| CN118029010A (en) * | 2024-01-31 | 2024-05-14 | 广州市双雄化纤有限公司 | Chemical fiber composite fiber and processing method thereof |
| CN118029011A (en) * | 2024-02-27 | 2024-05-14 | 苏州大学 | A PLA-PHA parallel composite elastic fiber and preparation method thereof |
| CN117802595B (en) * | 2024-02-29 | 2024-05-28 | 北京蓝晶微生物科技有限公司 | Polyhydroxyalkanoate monofilament and continuous preparation method thereof |
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| US5698322A (en) * | 1996-12-02 | 1997-12-16 | Kimberly-Clark Worldwide, Inc. | Multicomponent fiber |
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