CN112011848A - Preparation method of medical polylactic acid composite material fiber - Google Patents
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/06—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
- C08G63/08—Lactones or lactides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/823—Preparation processes characterised by the catalyst used for the preparation of polylactones or polylactides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/87—Non-metals or inter-compounds thereof
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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
- 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
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Abstract
The invention belongs to the technical field of polymer chemical substance synthesis, and particularly relates to a preparation method of medical polylactic acid composite material fiber, which mainly comprises the steps of prepolymerizing L-lactic acid to form an oligomer, adding a composite material into the oligomer, and carrying out polymerization reaction under the action of a catalytic composition to form a polylactic acid composite material; uniformly mixing and drying the polylactic acid composite material, transferring the polylactic acid composite material into a vacuum device, heating in vacuum, melting, and then extruding in vacuum to preliminarily form polylactic acid fibers; and (3) drafting the polylactic acid fiber and carrying out heat treatment to finally obtain a polylactic acid fiber finished product. According to the invention, the composite materials such as ethylene glycol or vinyl pyrrolidone are added into polylactic acid, so that the synthesized polylactic acid fiber has excellent hydrophilicity, and the hydrophilic groups of ethylene glycol and vinyl pyrrolidone are applied to the polylactic acid fiber, so that the hydrophilic performance of the fiber material is improved, and the fiber material is more hydrophilic and breathable when applied to medical treatment, and the comfort level is increased.
Description
Technical Field
The invention relates to the technical field of polylactic acid fibers, in particular to a preparation method of medical polylactic acid composite fibers.
Background
Polylactic acid fiber is also called corn fiber, PLA for short, and polylactide (polylactide) and belongs to the polyester family. It is made up by using corn and other cereal raw materials through the processes of fermentation, polymerization and spinning. Polylactic acid fiber is a high molecular polymer using lactic acid as a main raw material. Polylactic acid is synthesized from lactic acid, and the raw material of lactic acid is all carbohydrate-rich substances, such as food and organic wastes. The biodegradable starch can be biodegraded, is decomposed into carbon dioxide and water under the action of microorganisms, can generate the initial raw material starch through photosynthesis under the sunlight, and the starch is the raw material of lactic acid, so that the circulation realizes the sustainable utilization of closed-loop circulation of resources.
The polylactic acid fiber belongs to high-strength, medium-elongation and low-modulus fibers. The strength is high and reaches 3.0-4.5cN/dtex, which is close to polyester fiber. The fabric made by the method has soft hand feeling and good drapability, and has similar acid and alkali resistance as polyester fiber.
The moisture regain of the polylactic acid fiber with the moisture absorption, quick drying and heat retention performances is 0.4-0.6%, and is lower than most of natural fibers and synthetic fibers (except PET), the moisture absorption performance is poorer, and the water resistance performance is better. Has unique wicking action, and can make the fabric wet-conductive, quick-drying and warm-keeping. Although the flame-retardant fiber is not flame-retardant, the flame retardance of the common fiber is better. The flame performance is 1/3 for polyethylene and polypropylene fibers. The wear resistance is poor, the application in the clothing field is influenced, and the use at high temperature is limited due to low melting point. The polylactic acid fiber has excellent physical performance, good thermal stability, light weight, good dyeing property and biocompatibility, so the polylactic acid fiber has wide application. At present, the application of the fabric is mainly in the fields of medical use, clothing and the like.
In the aspect of medical treatment, the operation suture line can meet the requirement of strength and can be slowly absorbed by a human body, and the trouble and pain of disconnecting the suture line of a patient are avoided. The stretched high molecular weight polylactic acid material or polylactic acid fiber reinforced composite material can be used as a bone union part fixing material and a tissue defect part reinforcing material. It can also be used as bandage, gauze, absorbent cotton, sanitary napkin for women, and diaper for baby. However, since the hydrophilicity and other properties of the medical polylactic acid fiber are required to be enhanced, it is important to design a medical polylactic acid fiber having hydrophilicity and high stretchability.
Disclosure of Invention
The invention provides a preparation method of medical polylactic acid composite material fiber with simple method and reasonable design for solving the problems.
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material into the oligomer, and performing polymerization reaction under the action of a catalytic composition to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying the polylactic acid composite material obtained in the step S1, transferring the mixture into a vacuum device, heating in vacuum, melting, and then extruding in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (5) drafting the polylactic acid fiber extruded in the step (S2) and carrying out heat treatment to finally obtain a polylactic acid fiber finished product.
Further, the composite material in the step S1 is ethylene glycol or vinyl pyrrolidone, the addition amount of the catalytic composition is 1-5% of the mass fraction of the oligomer, and the reaction conditions are 180-200 ℃ for 6-12 h.
Further, the catalytic composition comprises 4-6 parts by weight ofSnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate.
Furthermore, the composite material in the step S2 is also mixed with polyvinyl alcohol, and the mixing mass ratio of the polyvinyl alcohol to the composite material is 1: 10-15.
Further, the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Further, the heat treatment temperature in the step S3 is 80 to 120 ℃.
The preparation method of the medical polylactic acid composite material fiber provided by the invention has the following beneficial effects:
1) according to the invention, the polylactic acid composite material fiber is prepared and used for preparing the medical fiber product, so that the performance of the polylactic acid fiber is enhanced and the polylactic acid fiber is convenient to use;
2) according to the invention, the composite materials such as ethylene glycol or vinyl pyrrolidone are added into polylactic acid, so that the synthesized polylactic acid fiber has excellent hydrophilicity, and the hydrophilic groups of ethylene glycol and vinyl pyrrolidone are applied to the polylactic acid fiber, so that the hydrophilic performance of the fiber material is improved, and the fiber material is more hydrophilic and breathable when applied to medical treatment, and the comfort level is increased;
3) according to the invention, a small amount of polyvinyl alcohol is mixed into the polylactic acid fiber, and through blending modification, the hydrophilic property of the polyvinyl alcohol is utilized in the fiber material, so that the polylactic acid fiber has the hydrophilic property of the polyvinyl alcohol;
4) according to the invention, the catalyst composition is added in the polylactic acid synthesis process to catalyze the oligomer, so that the obtained polylactic acid has high molecular weight, the performance of the obtained polylactic acid is improved, and the synthesized fiber has higher strength and better tensile property.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example 1
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding composite material ethylene glycol into the oligomer, adding a catalytic composition with the mass fraction of 1%, and carrying out polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying polyvinyl alcohol and the polylactic acid composite material obtained in the step S1 according to the mass ratio of 1:10, transferring the mixture into a vacuum device, heating the mixture in vacuum, melting the mixture, and then extruding the mixture in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (5) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 80 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Example 2
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material of vinyl pyrrolidone into the oligomer, adding a catalytic composition with the mass fraction of 3%, and carrying out polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying polyvinyl alcohol and the polylactic acid composite material obtained in the step S1 according to the mass ratio of 1:12, transferring the mixture into a vacuum device, heating the mixture in vacuum, melting the mixture, and then extruding the mixture in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (4) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 100 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Example 3
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material of vinyl pyrrolidone into the oligomer, adding a catalytic composition with the mass fraction of 5%, and carrying out polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying polyvinyl alcohol and the polylactic acid composite material obtained in the step S1 according to the mass ratio of 1:15, transferring the mixture into a vacuum device, heating the mixture in vacuum, melting the mixture, and then extruding the mixture in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (4) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 120 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Comparative example 1
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material of vinyl pyrrolidone into the oligomer, adding a catalytic composition with the mass fraction of 3%, and carrying out polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying the polylactic acid composite material obtained in the step S1, transferring the mixture into a vacuum device, heating in vacuum, melting, and then extruding in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (4) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 80-120 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Comparative example 2
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material of vinyl pyrrolidone into the oligomer, adding a catalytic composition with the mass fraction of 3%, and carrying out polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying polyvinyl alcohol and the polylactic acid composite material obtained in the step S1 according to the mass ratio of 1:12, transferring the mixture into a vacuum device, heating the mixture in vacuum, melting the mixture, and then extruding the mixture in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (4) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 100 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O and 6-8 parts of CF3SO3Me; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Comparative example 3
A preparation method of medical polylactic acid composite material fiber comprises the following steps:
step S1: preparation of polylactic acid composite material
Adding a catalytic composition with the mass fraction of 3% into an oligomer formed by pre-polymerizing L-lactic acid for polymerization reaction to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying polyvinyl alcohol and the polylactic acid composite material obtained in the step S1 according to the mass ratio of 1:12, transferring the mixture into a vacuum device, heating the mixture in vacuum, melting the mixture, and then extruding the mixture in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (4) drafting the polylactic acid fiber extruded in the step S2 and carrying out heat treatment at 100 ℃ to finally obtain a polylactic acid fiber finished product.
The catalytic composition comprises 4 to 6 parts by weight of SnCl2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate; the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
Test 1: the present invention respectively performs the molecular weight test on the medical polylactic acid composite material fibers obtained in examples 1 to 3 and comparative examples 1 to 3, and the results are shown in the following table 1:
| sample (I) | Molecular weight (. about.10)4g/mol) |
| Example 1 | 25.6 |
| Example 2 | 27.4 |
| Example 3 | 26.3 |
| Comparative example 1 | 20.9 |
| Comparative example 2 | 16.4 |
| Comparative example 3 | 21.8 |
The results in the table show that when the composite material is added in the polylactic acid synthesis process or polyvinyl alcohol is mixed in the polylactic acid composite material or the components of the catalytic composition are changed, the molecular weight of the finally formed polylactic acid composite material fiber is influenced, and the influence of the changed components of the catalytic composition on the molecular weight is the largest, so that the molecular weight of the finally obtained polylactic acid composite material fiber is increased, and the performance of the polylactic acid composite material fiber is further improved.
And (3) testing 2: the tensile properties of the polylactic acid composite material fibers obtained in examples 1 to 3 and comparative examples 1 to 3 were measured, and the results are shown in the following table 2:
| sample (I) | Monofilament Linear Density (dtex) | Breaking strength (cN/dTex) | Tensile modulus (cN/dTex) |
| Example 1 | 4.1 | 3.8 | 37.6 |
| Example 2 | 4.5 | 3.9 | 39.1 |
| Example 3 | 4.2 | 3.5 | 36.4 |
| Comparative example 1 | 1.7 | 2.4 | 19.7 |
| Comparative example 2 | 2.1 | 2.3 | 25.3 |
| Comparative example 3 | 1.5 | 2.7 | 18.6 |
The above table shows that when the composite material is added in the polylactic acid synthesis process or polyvinyl alcohol is mixed in the polylactic acid composite material or the components of the catalytic composition are changed, the tensile property of the polylactic acid composite material fiber is affected, and the tensile strength of the polylactic acid composite material fiber added with the composite material, mixed with the polyvinyl alcohol and changed in the catalytic composition is enhanced, so that the strength is better, and the polylactic acid composite material fiber has better tensile elasticity in the practical process.
And (3) testing: the hydrophilicity of the polylactic acid composite fibers obtained in examples 1 to 3 and comparative examples 1 to 3 was measured, and the results are shown in the following table 3:
the moisture regain is generally used in the textile industry to indicate the moisture absorption of the textile material, and the moisture regain refers to the moisture content in the fiber material, that is, the content of absorbed water, as shown in the results in table 3 above, when the composite material is added in the polylactic acid synthesis process or polyvinyl alcohol is mixed in the polylactic acid composite material or the catalytic composition component is changed, the moisture absorption performance of the polylactic acid composite material fiber is affected, especially when the hydrophilic material is added, the moisture absorption performance of the material is improved to a certain extent, the hydrophilicity of the polylactic acid fiber is improved, and the use is more convenient when the hydrophilic material is applied in the medical field.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of medical polylactic acid composite material fiber is characterized by comprising the following steps:
step S1: preparation of polylactic acid composite material
Pre-polymerizing L-lactic acid to form an oligomer, adding a composite material into the oligomer, and performing polymerization reaction under the action of a catalytic composition to form a polylactic acid composite material;
step S2: preparation of polylactic acid fiber
Uniformly mixing and drying the polylactic acid composite material obtained in the step S1, transferring the mixture into a vacuum device, heating in vacuum, melting, and then extruding in vacuum to preliminarily form polylactic acid fibers;
step S3: polylactic acid fiber post-treatment
And (5) drafting the polylactic acid fiber extruded in the step (S2) and carrying out heat treatment to finally obtain a polylactic acid fiber finished product.
2. The preparation method of the medical polylactic acid composite fiber according to claim 1, which is characterized in that: the composite material in the step S1 is ethylene glycol or vinyl pyrrolidone, the addition amount of the catalytic composition is 1-5% of the mass fraction of the oligomer, and the reaction condition is 180-200 ℃ for 6-12 h.
3. The preparation method of the medical polylactic acid composite fiber according to claim 2, which is characterized in that: the catalytic composition comprises 4-6 parts of SnCl by weight2·2H2O, 6-8 parts of CF3SO3Me, 3-6 parts of dialkyl zinc and 2-4 parts of stannous isozincate.
4. The preparation method of the medical polylactic acid composite fiber according to claim 1, which is characterized in that: the composite material in the step S2 is also mixed with polyvinyl alcohol, and the mixing mass ratio of the polyvinyl alcohol to the composite material is 1: 10-15.
5. The preparation method of the medical polylactic acid composite fiber according to claim 1, which is characterized in that: the drawing process of the polylactic acid fiber in the step S3 is as follows: the temperature of the hot plate is 60-100 ℃, the temperature of the hot plate is 60-120 ℃, and the drafting multiplying power is 2-8 times.
6. The preparation method of the medical polylactic acid composite fiber according to claim 1, which is characterized in that: the heat treatment temperature in the step S3 is 80-120 ℃.
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