CN108950716B - Polyamide 56 mowing filament and preparation method thereof - Google Patents
Polyamide 56 mowing filament and preparation method thereof Download PDFInfo
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- CN108950716B CN108950716B CN201710376174.1A CN201710376174A CN108950716B CN 108950716 B CN108950716 B CN 108950716B CN 201710376174 A CN201710376174 A CN 201710376174A CN 108950716 B CN108950716 B CN 108950716B
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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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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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
- D01D5/08—Melt spinning methods
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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
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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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
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; 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
- D01D7/00—Collecting the newly-spun products
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a polyamide 56 lawn mower, which is prepared from 1, 5-pentanediamine and hexanedioic acid; or polyamide 56 obtained by polymerizing 1, 5-pentanediamine and adipic acid as monomers. The invention also relates to a preparation method of the polyamide 56 grass cutting silk, which comprises the following steps: (1) polymerizing 1, 5-pentanediamine and adipic acid to form a polyamide 56 melt; alternatively, the polyamide 56 resin is heated to a molten state to form a melt of polyamide 56; (2) spinning the polyamide 56 melt to form primary yarn; (3) and treating the primary yarn to obtain the polyamide 56 mowing yarn. The lawn mower produced by the invention has the characteristics of environmental protection, softness, high elasticity, good wear resistance and the like.
Description
Technical Field
The invention belongs to the technical field of polyamide materials, and particularly relates to a polyamide 56 mowing filament and a preparation method thereof.
Background
The grass cutting filament is one kind of monofilament, and is produced through slicing spinning, and has filament thickness of 1-5mm, and subsequent forming process different from that of common fiber, including hot water drawing process with liquid cooling.
The grass cutting filaments are generally made of polyamide, copolyamide, polypropylene and the like. At present, along with the improvement of living standard, the demand of people on greening area is further improved, and the requirements on the wear resistance, the flexibility and the elasticity of the mowing filament are higher and higher. The polyamide material has better wear resistance, flexibility and elasticity than polypropylene, and the common grass cutting filament material is polyamide 6, polyamide 66 and 6/66 copolyamide.
Disclosure of Invention
Compared with polyamide 6, polyamide 66 and 6/66 copolyamide, the polyamide 56 has better wear resistance and elasticity, the initial modulus is relatively small, the prepared grass cutting filament is softer and can meet the requirements of a high-speed mower, the polyamide 56 belongs to a biological base material, the polymerized monomer of the polyamide 56 is prepared by a biological fermentation method, the environment is protected, and the application of the polyamide 56 in the preparation of the grass cutting filament is the initiative of the invention.
The first purpose of the invention is to provide polyamide 56 grass cutting filaments with soft and high elasticity and good wear resistance.
The second purpose of the invention is to provide a preparation method of the polyamide 56 grass cutting filament, wherein the production raw material of the method adopts non-petroleum-based (bio-based) materials, so that the method does not generate large pollution and is beneficial to environmental protection.
In order to achieve the above purpose, the solution of the invention is as follows:
[ Polyamide 56 grass cutting string ]
A polyamide 56 grass cutting filament comprises the following raw materials: 1, 5-pentanediamine and adipic acid; or polyamide 56 obtained by polymerizing 1, 5-pentanediamine and adipic acid as monomers.
Wherein, the 1, 5-pentanediamine can be prepared from bio-based raw materials by a fermentation method or an enzyme conversion method.
The structural formula of polyamide 56 is as follows:
wherein m is 5 and n is 6.
The circumscribed circle diameter of the polyamide 56 grass cutting filament is 0.5-8mm, preferably 0.7-7mm, more preferably 0.8-6mm, still more preferably 0.9-5mm, and still more preferably 1-4 mm;
the breaking strength of the polyamide 56 grass-cutting filaments is 2.0-7.0cN/dtex, preferably 2.5-6.5cN/dtex, more preferably 3.0-6.0cN/dtex, and even more preferably 4.0-5.5 cN/dtex;
the elongation at break of the polyamide 56 grass cutting filaments is 20-50%, preferably 23-48%, more preferably 26-46%, and still more preferably 28-44%;
the initial modulus of the polyamide 56 grass cutting filaments is 30-50cN/dtex, preferably 32-48cN/dtex, more preferably 35-45cN/dtex, and still more preferably 38-43 cN/dtex;
the elastic recovery rate of the polyamide 56 grass cutting filaments is 95-100% when the elongation rate is 10%;
the elastic recovery rate of the polyamide 56 grass cutting filaments is 90-100%, preferably 93-98% when the elongation rate is 15%; the elastic recovery rate of the polyamide 56 grass-cutting filament is more than 85% when the elongation rate is 20%, preferably 88-96%, and more preferably 90-94%.
[ preparation method of Polyamide 56 grass cutting yarn ]
The preparation method of the polyamide 56 grass cutting silk comprises the following steps:
1) polymerizing 1, 5-pentanediamine and adipic acid to form a polyamide 56 melt; alternatively, the polyamide 56 resin is heated to a molten state to form a melt of polyamide 56;
2) spinning the polyamide 56 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 56 mowing yarn.
Wherein, in step 1), the polymerization process comprises the following steps:
1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; the molar ratio of the 1, 5-pentanediamine to the adipic acid is (1-1.2): 1;
1-2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.2-2.6Mpa, exhausting, maintaining the pressure, then reducing the pressure to reduce the pressure in the reaction system to gauge pressure of 0-0.5Mpa, vacuumizing to-0.085-0.1 Mpa of vacuum degree, and obtaining a polyamide melt;
in the step 1-2), the temperature of the reaction system is 225-275 ℃ when the pressure maintaining is finished;
in the step 1-2), the temperature of the reaction system after the pressure reduction is finished is 255-270 ℃;
in the step 1-2), the temperature after the vacuum pumping is 250-270 ℃.
In the step 1), the polyamide 56 resin is polyamide 56 chips;
the relative viscosity of the polyamide 56 resin is 2.3 to 4.0, preferably 2.5 to 4.3, more preferably 3.0 to 4.0, and still more preferably 3.2 to 3.5;
the water content of the polyamide 56 resin is 30-1000ppm, preferably 100-800ppm, more preferably 200-600ppm, and still more preferably 300-500 ppm;
in the step 1), the heating is carried out in a screw extruder, the screw extruder is divided into five zones for heating, the temperature of the first zone is 100-;
preferably, the temperature of the first zone is 130-.
The spinning process in the step 2) comprises the following steps:
feeding the polyamide 56 melt into a spinning manifold, and spraying out the melt through a spinneret plate to form the primary yarn;
the temperature of the spinning manifold is 250-330 ℃, preferably 260-320 ℃, more preferably 280-310 ℃, and even more preferably 290-300 ℃;
the internal pressure of the spinning manifold is 7-25MPa, preferably 8-23MPa, and more preferably 10-18 MPa;
the radius of the spinneret plate is 30-200mm, preferably 40-180mm, more preferably 50-160mm, and still more preferably 60-150 mm;
the aperture of the spinneret orifice of the spinneret plate is 1-5mm, preferably 1.2-4.8mm, more preferably 1.5-4.0mm, and even more preferably 2.0-3.5 mm;
the spinneret orifice section of the spinneret plate is one of a triangle, a diamond, a cross, a flat, a square, a pentagon and a hexagon.
The treatment process in the step 3) comprises the following steps:
firstly, carrying out liquid cooling forming on the primary yarn, then feeding the primary yarn into a first group of godet rollers and a second group of godet rollers, carrying out hot water drawing between the first group of godet rollers and the second group of godet rollers, then carrying out heat setting in a continuous secondary oven, and finally winding to obtain polyamide 56 grass cutting yarn;
the hot water stretching temperature is 70-130 ℃, preferably 90-120 ℃,
the stretching ratio in hot water stretching is 2.0-5.0, preferably 2.2-4.8, more preferably 2.5-4.5;
the temperature of the first-stage drying oven is 150-250 ℃, preferably 160-240 ℃ and more preferably 180-230 ℃ during the shaping;
the temperature for the second-stage drying oven is 120-230 ℃, preferably 130-220 ℃, and more preferably 150-200 ℃;
the winding speed during the winding forming is 50-500m/min, preferably 60-450m/min, more preferably 80-400m/min, and still more preferably 100-300 m/min.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the production raw material of the polyamide 56 grass cutting silk is prepared from the pentamethylene diamine by a biological method, is a green material, does not depend on petroleum resources to cause serious pollution to the environment, and can reduce the emission of carbon dioxide and reduce the generation of greenhouse effect.
Secondly, the polyamide 56 lawn mower of the invention is soft, wear-resistant and has better elasticity.
Detailed Description
The invention relates to a polyamide 56 mowing filament and a preparation method thereof.
< Polyamide 56 cut grass filaments >
The raw materials for producing the polyamide 56 grass cutting filament contain 1, 5-pentanediamine and adipic acid; or polyamide 56 obtained by polymerizing 1, 5-pentanediamine and adipic acid as monomers.
[1, 5-Pentanediamine ]
The 1, 5-pentanediamine can be prepared from bio-based raw materials through a biological method.
The biological method comprises producing 1, 5-pentanediamine by biological conversion method (such as fermentation method and enzyme conversion method) with bio-based raw material; or 1, 5-pentanediamine is produced by adopting petroleum-based raw materials through a biotransformation method; or biological raw materials are adopted to produce the 1, 5-pentanediamine by a chemical method. Thus, pentanediamine contains a renewable source of organic carbon that meets the ASTM D6866 standard.
Specifically, lysine or lysine salt can be subjected to decarboxylation at two ends under the action of lysine decarboxylase (such as EC 4.1.1.18) to generate 1, 5-pentanediamine, such as a method for preparing pentanediamine by a specific biological method disclosed in L-lysine decarboxylase property and application research (Jiangli, Nanjing university, 2007); for example, the research on the transformation of L-lysine into cadaverine by microorganisms (ZhuJing, Tianjin science and technology university, 2009.3) also discloses a specific biological method for preparing pentanediamine.
The properties of the polyamide 56 grass-cutting filaments described above are as follows:
the diameter of the circumscribed circle of the polyamide 56 grass cutting filament is 0.5-8mm, preferably 0.7-7mm, more preferably 0.8-6mm, further preferably 0.9-5mm, and further preferably 1-4 mm;
the breaking strength of the polyamide 56 grass-cutting filaments is 2.0-7.0cN/dtex, preferably 2.5-6.5cN/dtex, more preferably 3.0-6.0cN/dtex, and further preferably 4.0-5.5 cN/dtex;
the elongation at break of the polyamide 56 grass cutting filaments is 20-50%, preferably 23-48%, more preferably 26-46%, and further preferably 28-44%;
the initial modulus of the polyamide 56 grass cutting filaments is 30-50cN/dtex, preferably 32-48cN/dtex, more preferably 35-45cN/dtex, and further preferably 38-43 cN/dtex;
the elastic recovery rate of the polyamide 56 grass cutting filaments is 95-100% when the elongation rate is 10%;
the elastic recovery rate of the polyamide 56 grass cutting filaments is 90-100%, preferably 93-98% when the elongation rate is 15%; the elastic recovery rate of the polyamide 56 grass cutting filament is more than 85% when the elongation rate is 20%, preferably 88-96%, and more preferably 90-94%.
The method for evaluating each performance index of the embodiment of the invention comprises the following steps:
(1) nominal diameter
The cross section of the mowing filament is measured at 10 different positions by a handheld thickness gauge, and then an average value is obtained.
(2) Linear density of
The mowing filament is thicker, a certain length of mowing filament is taken by a ruler, the length is more than 3m, the mowing filament is weighed and then converted into 10000 meters of weight in dtex.
(3) Breaking Strength, elongation at Break, initial modulus
The universal strength tester, measured according to the method of GB/T21032-2007, had a breaking strength (breaking strength/linear density) × 100%, and an initial modulus (breaking strength/linear density for 1% elongation at break) × 100%.
(4) Wear resistance
Reciprocating type abrasion tester
The strength retention rate (breaking strength after abrasion for a certain period of time/breaking strength before abrasion) × 100%; the number of unit linear density wear-out times is (total number of times at wear-out/linear density) × 100%; mass loss of the cut grass filament is (mass before abrasion-mass after abrasion for a certain time)/mass before abrasion) x 100%; the sand mass loss is ((mass before abrasion-mass after abrasion for a certain time)/mass before abrasion) × 100%.
(5) Elastic recovery rate
And (3) setting test parameters according to a GB/T14344-2008 test method by adopting a YG061 type yarn strength and elongation instrument. The stretching gauge is 500mm, the pre-tension is 0.1cN/dtex, and the stretching speed is 500 mm/min. Stretching to a set elongation (E10, 20, 30%).
Elastic recovery (%) - (% L-L1/(L-L0) × 100%;
in the formula: l0 is the original length of the sample, L is the length of the sample after stretching to a fixed extension, and L1 is the length of the sample after resetting.
< preparation of Polyamide 56 cut grass filaments >
The preparation method of the polyamide 56 grass cutting silk comprises the following steps:
1) polymerizing 1, 5-pentanediamine and adipic acid to form a polyamide 56 melt; alternatively, the polyamide 56 resin is heated to a molten state to form a melt of polyamide 56;
2) spinning the polyamide 56 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 56 mowing yarn.
Wherein, in step 1), the polymerization process comprises the following steps:
1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; the molar ratio of the 1, 5-pentanediamine to the adipic acid is (1-1.2): 1;
1-2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.2-2.6Mpa, exhausting, maintaining the pressure, then reducing the pressure to reduce the pressure in the reaction system to gauge pressure of 0-0.5Mpa, vacuumizing to-0.085-0.1 Mpa of vacuum degree, and obtaining a polyamide melt;
in the step 1-2), the temperature of the reaction system is 225-275 ℃ when the pressure maintaining is finished;
in the step 1-2), the temperature of the reaction system after the pressure reduction is finished is 255-270 ℃;
in the step 1-2), the temperature after the vacuum pumping is 250-270 ℃.
In the step 1), the polyamide 56 resin is polyamide 56 chips;
the relative viscosity of the polyamide 56 resin is 2.3 to 4.0, preferably 2.5 to 4.3, more preferably 3.0 to 4.0, and further preferably 3.2 to 3.5;
the relative viscosity was determined as follows:
the relative viscosity of the polyamide 56 resin was measured by the concentrated sulfuric acid method with an Ubbelohde viscometer, which comprises the following steps: the dried polyamide 56 cut tobacco sample was weighed accurately at 0.25. + -. 0.0002g, dissolved by adding 50mL of concentrated sulfuric acid (96 wt%), and the flow time t0 of the concentrated sulfuric acid and the flow time t of the polyamide 56 cut tobacco sample solution were measured and recorded in a thermostatic water bath at 25 ℃.
The relative viscosity is calculated by the formula: the relative viscosity VN is t/t 0;
t-solution flow time;
t 0-time of solvent flow.
The water content of the polyamide 56 resin is 30-1000ppm, preferably 100-800ppm, more preferably 200-600ppm, and still more preferably 300-500 ppm;
the heating is carried out in a screw extruder which is divided into five zones for heating, wherein the temperature of the first zone is 100-;
preferably, the temperature of the first zone is 130-.
The spinning process in the step 2) comprises the following steps:
feeding the polyamide 56 melt into a spinning manifold, and spraying out the melt through a spinneret plate to form the primary yarn;
the temperature of the spinning manifold is 250-330 ℃, preferably 260-320 ℃, more preferably 280-310 ℃, and even more preferably 290-300 ℃;
the internal pressure of the spinning manifold is 7-25MPa, preferably 8-23MPa, and more preferably 10-18 MPa;
the radius of the spinneret plate is 30-200mm, preferably 40-180mm, more preferably 50-160mm, and still more preferably 60-150 mm;
the diameter of the orifice of the spinneret is 1 to 5mm, preferably 1.2 to 4.8mm, more preferably 1.5 to 4.0mm, and still more preferably 2.0 to 3.5 mm.
The spinneret orifice section of the spinneret plate is one of a triangle, a diamond, a cross, a flat, a square, a pentagon and a hexagon.
The treatment process in the step 3) comprises the following steps:
firstly, carrying out liquid cooling forming on the primary yarn, then feeding the primary yarn into a first group of godet rollers and a second group of godet rollers, carrying out hot water drawing between the first group of godet rollers and the second group of godet rollers, then carrying out heat setting in a continuous secondary oven, and finally winding to obtain polyamide 56 grass cutting yarn;
the hot water stretching temperature is 70-130 ℃, preferably 90-120 ℃,
the stretching ratio in hot water stretching is 2.0-5.0, preferably 2.2-4.8, more preferably 2.5-4.5;
the temperature of the first-stage drying oven is 150-250 ℃, preferably 160-240 ℃ and more preferably 180-230 ℃ during the shaping;
the temperature for the second-stage drying oven is 120-230 ℃, preferably 130-220 ℃, and more preferably 150-200 ℃;
the winding speed during the winding forming is 50-500m/min, preferably 60-450m/min, more preferably 80-400m/min, and still more preferably 100-300 m/min.
The present invention will be further described with reference to the following examples.
Example 1: polyamide 56 lawn mower
The embodiment provides a preparation method of polyamide 56 grass cutting filaments, which comprises the following steps:
1) heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
2) spinning the polyamide 56 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 56 mowing yarn.
In step 1), the polyamide 56 resin (in the form of chips) had a relative viscosity of 3.0 and was prepared by a biological fermentation method, and the water content of the chips was 500 ppm.
The heating in step 1) is carried out in a single screw extruder, which is divided into five zones of heating, wherein the temperature of the first zone is 130 ℃, the temperature of the second zone is 220 ℃, the temperature of the third zone is 260 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 310 ℃.
The spinning in the step 2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 300 ℃, and the pressure of the spinning assembly of the spinning beam is 16.0 MPa.
The processing in step 3) comprises the following steps:
the raw silk is firstly subjected to liquid cooling forming, then fed into a first group of godet rollers and a second group of godet rollers, hot water drawing is carried out between the first group of godet rollers and the second group of godet rollers, then heat setting is carried out in a continuous secondary oven, and finally winding is carried out to obtain the polyamide 56 grass cutting silk, wherein the temperature during hot water drawing is 100 ℃, the drawing multiple during hot water drawing is 3.5, the temperature during first-stage oven setting is 240 ℃, the temperature during second-stage oven setting is 200 ℃, and the winding speed during winding forming is 200 m/min.
Example 2: polyamide 56 lawn mower
The embodiment provides a preparation method of polyamide 56 grass cutting filaments, which comprises the following steps:
1) heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
2) spinning the polyamide 56 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 56 mowing yarn.
In step 1), the polyamide 56 resin (in the form of chips) had a relative viscosity of 2.9 and was prepared by a biological fermentation method, and the water content of the chips was 700 ppm.
The heating in step 1) is carried out in a single screw extruder, which is divided into five zones for heating, wherein the temperature of the first zone is 120 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 320 ℃, and the temperature of the fifth zone is 290 ℃.
The spinning in the step 2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 295 ℃, and the pressure of the spinning assembly of the spinning beam is 18.0 MPa.
The processing in step 3) comprises the following steps:
the raw silk is firstly subjected to liquid cooling forming, then fed into a first group of godet rollers and a second group of godet rollers, hot water drawing is carried out between the first group of godet rollers and the second group of godet rollers, then heat setting is carried out in a continuous secondary oven, and finally winding is carried out to obtain the polyamide 56 cut grass silk, wherein the temperature during hot water drawing is 85 ℃, the drawing multiple during hot water drawing is 3.0, the temperature during first-stage oven setting is 220 ℃, the temperature during second-stage oven setting is 190 ℃, and the winding speed during winding forming is 180 m/min.
Example 3: polyamide 56 lawn mower
The embodiment provides a preparation method of polyamide 56 grass cutting filaments, which comprises the following steps:
1) heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
2) spinning the polyamide 56 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 56 mowing yarn.
In step 1), the polyamide 56 resin (in the form of chips) had a relative viscosity of 3.4 and was prepared by a biological fermentation method, and the water content of the chips was 400 ppm.
The heating in step 1) is carried out in a single screw extruder, which is divided into five zones for heating, wherein the temperature of the first zone is 160 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 300 ℃, and the temperature of the fifth zone is 300 ℃.
The spinning in the step 2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 300 ℃, and the pressure of the spinning assembly of the spinning beam is 15.0 MPa.
The processing in step 3) comprises the following steps:
the raw silk is firstly subjected to liquid cooling forming, then fed into a first group of godet rollers and a second group of godet rollers, hot water drawing is carried out between the first group of godet rollers and the second group of godet rollers, then heat setting is carried out in a continuous secondary oven, and finally winding is carried out to obtain the polyamide 56 cut grass silk, wherein the temperature during hot water drawing is 105 ℃, the drawing multiple during hot water drawing is 2.8, the temperature during first-stage oven setting is 225 ℃, the temperature during second-stage oven setting is 205 ℃, and the winding speed during winding forming is 260 m/min.
Comparative example 1: polyamide 6 lawn mower
The embodiment provides a preparation method of polyamide 6 grass cutting filaments, which comprises the following steps:
1) heating polyamide 6 resin to a molten state to form a polyester melt;
2) spinning the polyamide 6 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 6 grass cutting yarn.
In step 1), the relative viscosity of the polyamide 6 resin (in the form of chips) was 3.0, and the water content of the chips was 550 ppm.
The heating in step 1) is carried out in a single screw extruder, which is divided into five zones with a first zone temperature of 165 ℃, a second zone temperature of 210 ℃, a third zone temperature of 260 ℃, a fourth zone temperature of 290 ℃ and a fifth zone temperature of 280 ℃.
The spinning in the step 2) comprises the following steps: and (3) feeding the polyamide 6 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 280 ℃, and the pressure of the spinning assembly of the spinning beam is 14.0 MPa.
The processing in step 3) comprises the following steps:
the raw silk is firstly subjected to liquid cooling forming, then fed into a first group of godet rollers and a second group of godet rollers, hot water drawing is carried out between the first group of godet rollers and the second group of godet rollers, then heat setting is carried out in a continuous secondary oven, finally, the polyamide 6 grass cutting silk is obtained by winding, the temperature during hot water drawing is 75 ℃, the drawing multiple during hot water drawing is 2.9, the temperature during first-stage oven setting is 220 ℃, the temperature during second-stage oven setting is 200 ℃, and the winding speed during winding forming is 250 m/min.
Comparative example 2: polyamide 66 lawn mower
The embodiment provides a preparation method of polyamide 66 grass cutting filaments, which comprises the following steps:
1) heating the polyamide 66 resin to a molten state to form a polyester melt;
2) spinning the polyamide 66 melt to form primary yarn;
3) and treating the primary yarn to obtain the polyamide 66 lawn mower yarn.
In step 1), the relative viscosity of the polyamide 6 resin (in the form of chips) was 2.8, and the water content of the chips was 450 ppm.
The heating in step 1) is carried out in a single screw extruder, which is divided into five zones with a first zone temperature of 175 ℃, a second zone temperature of 220 ℃, a third zone temperature of 280 ℃, a fourth zone temperature of 290 ℃ and a fifth zone temperature of 285 ℃.
The spinning in the step 2) comprises the following steps: and (3) feeding the polyamide 66 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 290 ℃, and the pressure of the spinning assembly of the spinning beam is 13.0 MPa.
The processing in step 3) comprises the following steps:
the raw silk is firstly subjected to liquid cooling forming, then fed into a first group of godet rollers and a second group of godet rollers, hot water drawing is carried out between the first group of godet rollers and the second group of godet rollers, then heat setting is carried out in a continuous secondary oven, finally, the polyamide 66 mowing silk is obtained by winding, the temperature during hot water drawing is 95 ℃, the drawing multiple during hot water drawing is 3.0, the temperature during first-stage oven setting is 240 ℃, the temperature during second-stage oven setting is 220 ℃, and the winding speed during winding forming is 270 m/min.
TABLE 1 comparison of the properties of the products of the inventive and comparative examples
Claims (22)
1. A polyamide 56 grass cutting filament comprises the following raw materials: 1, 5-pentanediamine and adipic acid; or polyamide 56 obtained by polymerizing 1, 5-pentanediamine and adipic acid as monomers;
the 1, 5-pentanediamine is prepared from bio-based raw materials by a fermentation method or an enzyme conversion method; the initial modulus of the polyamide 56 grass cutting filament is 30-41.2cN/dtex, and the elastic recovery rate of the polyamide 56 grass cutting filament is 95-100% when the elongation rate is 10%;
the polyamide 56 grass cutting filaments are obtained by spinning a polyamide 56 melt to form primary filaments and processing the primary filaments; the processing process comprises the following steps:
firstly, carrying out liquid cooling forming on the raw silk, then feeding the raw silk into a first group of godet rollers and a second group of godet rollers, carrying out hot water drawing between the first group of godet rollers and the second group of godet rollers, then carrying out heat setting in a continuous secondary oven, and finally winding to obtain the polyamide 56 grass cutting silk;
the winding speed during winding forming is 100-260 m/min.
2. Polyamide 56 grass-cutting string according to claim 1, characterized in that:
the diameter of the circumscribed circle of the polyamide 56 grass cutting wire is 0.5-8 mm; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 56 grass cutting filaments is 2.0-7.0 cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide 56 grass cutting filaments is 20-50%; and/or the presence of a gas in the gas,
the initial modulus of the polyamide 56 grass cutting filaments is 32-41.2 cN/dtex.
3. Polyamide 56 grass-cutting string according to claim 2, characterized in that:
the diameter of the circumscribed circle of the polyamide 56 grass cutting wire is 0.7-7 mm; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 56 grass cutting filaments is 2.5-6.5 cN/dtex; and/or the presence of a gas in the gas,
the initial modulus of the polyamide 56 grass cutting filaments is 35-41.2 cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide 56 grass cutting filaments is 23-48%.
4. Polyamide 56 grass-cutting string according to claim 2, characterized in that:
the diameter of the circumscribed circle of the polyamide 56 grass cutting wire is 0.8-6 mm; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 56 grass cutting filaments is 3.0-6.0 cN/dtex; and/or the presence of a gas in the gas,
the initial modulus of the polyamide 56 grass cutting filaments is 38-41.2 cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide 56 grass cutting filaments is 26-46%.
5. Polyamide 56 grass-cutting string according to claim 2, characterized in that:
the diameter of the circumscribed circle of the polyamide 56 grass cutting wire is 0.9-5 mm; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 56 grass cutting filaments is 4.0-5.5 cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide 56 grass cutting filaments is 28-44%.
6. Polyamide 56 grass-cutting string according to claim 2, characterized in that:
the diameter of the circumscribed circle of the polyamide 56 grass cutting wire is 1-4 mm.
7. Polyamide 56 grass-cutting string according to any one of claims 1 to 6, characterized in that:
the elastic recovery rate of the polyamide 56 grass cutting filaments is 90-100% when the elongation rate is 15%; and/or the presence of a gas in the gas,
the elastic recovery rate of the polyamide 56 grass cutting filament is more than 85% when the elongation rate is 20%.
8. Polyamide 56 grass-cutting string according to claim 7, characterized in that:
the elastic recovery rate of the polyamide 56 grass cutting filaments is 93-98% when the elongation rate is 15%; and/or the presence of a gas in the gas,
the elastic recovery rate of the polyamide 56 grass cutting filaments is 88-96% when the elongation rate is 20%.
9. Polyamide 56 grass-cutting string according to claim 7, characterized in that: the elastic recovery rate of the polyamide 56 grass cutting filaments is 90-94% when the elongation rate is 20%.
10. A process for the preparation of polyamide 56 grass-cutting filaments as claimed in any one of claims 1 to 9, characterized in that: the preparation method comprises the following steps:
1) polymerizing 1, 5-pentanediamine and adipic acid to form a polyamide 56 melt; alternatively, the polyamide 56 resin is heated to a molten state to form a melt of polyamide 56;
2) spinning the polyamide 56 melt to form primary yarn;
3) treating the primary cut tobacco to obtain polyamide 56 cut tobacco; the processing process comprises the following steps:
firstly, carrying out liquid cooling forming on the raw silk, then feeding the raw silk into a first group of godet rollers and a second group of godet rollers, carrying out hot water drawing between the first group of godet rollers and the second group of godet rollers, then carrying out heat setting in a continuous secondary oven, and finally winding to obtain the polyamide 56 grass cutting silk; the winding speed during winding forming is 100-260 m/min.
11. The method of manufacturing according to claim 10, wherein:
in step 1), the polymerization process comprises the following steps:
1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; the molar ratio of the 1, 5-pentanediamine to the adipic acid is (1-1.2): 1;
1-2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.2-2.6MPa, exhausting, maintaining the pressure, reducing the pressure to reduce the pressure in the reaction system to gauge pressure of 0-0.5MPa, and vacuumizing to the vacuum degree of-0.085-0.1 MPa to obtain a polyamide melt; alternatively, the first and second electrodes may be,
in step 1), the polyamide 56 resin is polyamide 56 chips;
the relative viscosity of the polyamide 56 resin is 2.3-4.0;
the water content of the polyamide 56 resin is 30-1000 ppm;
in the step 1), the heating is performed in a screw extruder, the screw extruder is divided into five zones for heating, the temperature of the first zone is 100-.
12. The method of claim 11, wherein:
the relative viscosity of the polyamide 56 resin is 2.5-4.3;
the water content of the polyamide 56 resin is 100-800 ppm;
the temperature of the first zone is 130-150 ℃, the temperature of the second zone is 160-250 ℃, the temperature of the third zone is 210-270 ℃, the temperature of the fourth zone is 250-300 ℃ and the temperature of the fifth zone is 280-300 ℃.
13. The method of claim 11, wherein:
the relative viscosity of the polyamide 56 resin is 3.0-4.0;
the water content of the polyamide 56 resin is 200-600 ppm.
14. The method of claim 11, wherein:
the relative viscosity of the polyamide 56 resin is 3.2-3.5;
the water content of the polyamide 56 resin is 300-500 ppm.
15. The method of claim 11, wherein:
in the step 1-2), the temperature of the reaction system is 225-275 ℃ when the pressure maintaining is finished; and/or the presence of a gas in the gas,
in the step 1-2), the temperature of the reaction system after the pressure reduction is finished is 255-270 ℃; and/or the presence of a gas in the gas,
in the step 1-2), the temperature after the vacuum pumping is 250-270 ℃.
16. The production method according to any one of claims 10 to 15, characterized in that:
the spinning process in the step 2) comprises the following steps:
feeding the polyamide 56 melt into a spinning manifold, and spraying out the melt through a spinneret plate to form the primary yarn;
the temperature of the spinning box body is 250-330 ℃; and/or the presence of a gas in the gas,
the internal pressure of the spinning manifold is 7-25 MPa; and/or the presence of a gas in the gas,
the radius of the spinneret plate is 30-200 mm; and/or the presence of a gas in the gas,
the aperture of a spinneret orifice of the spinneret plate is 1-5 mm; and/or the presence of a gas in the gas,
the spinneret orifice section of the spinneret plate is one of a triangle, a diamond, a cross, a flat, a square, a pentagon and a hexagon.
17. The method of manufacturing according to claim 16, wherein:
the temperature of the spinning manifold is 260-320 ℃; and/or the presence of a gas in the gas,
the internal pressure of the spinning manifold is 8-23 MPa; and/or the presence of a gas in the gas,
the radius of the spinneret plate is 40-180 mm; and/or the presence of a gas in the gas,
the aperture of the spinneret orifice of the spinneret plate is 1.2-4.8 mm.
18. The method of manufacturing according to claim 16, wherein:
the temperature of the spinning manifold is 280-310 ℃; and/or the presence of a gas in the gas,
the internal pressure of the spinning manifold is 10-18 MPa; and/or the presence of a gas in the gas,
the radius of the spinneret plate is 50-160 mm; and/or the presence of a gas in the gas,
the aperture of the spinneret orifice of the spinneret plate is 1.5-4.0 mm.
19. The method of manufacturing according to claim 16, wherein:
the temperature of the spinning box body is 290-300 ℃; and/or the presence of a gas in the gas,
the radius of the spinneret plate is 60-150 mm; and/or the presence of a gas in the gas,
the aperture of the spinneret orifice of the spinneret plate is 2.0-3.5 mm.
20. The method of manufacturing according to claim 10, wherein:
the hot water stretching temperature is 70-130 ℃, and/or,
the stretching ratio of the hot water stretching is 2.0-5.0; and/or the presence of a gas in the gas,
the temperature of the first-stage drying oven during shaping is 150-250 ℃; and/or the presence of a gas in the gas,
the temperature of the second-stage oven is 120-230 ℃.
21. The method of claim 20, wherein:
the hot water stretching temperature is 90-120 deg.C, and/or,
the stretching ratio of the hot water stretching is 2.2-4.8; and/or the presence of a gas in the gas,
the temperature of the first-stage drying oven during shaping is 160-240 ℃; and/or the presence of a gas in the gas,
the temperature of the second-stage oven is 130-220 ℃.
22. The method of claim 20, wherein:
the stretching ratio of the hot water stretching is 2.5-4.5; and/or the presence of a gas in the gas,
the temperature of the first-stage drying oven during shaping is 180-230 ℃; and/or the presence of a gas in the gas,
the temperature of the second-stage drying oven during shaping is 150-200 ℃.
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| CN111378121B (en) * | 2020-03-31 | 2023-03-10 | 上海凯赛生物技术股份有限公司 | High-viscosity polyamide 56 resin, high-strength polyamide 56 industrial yarn and preparation method and application thereof |
| CN115262049A (en) * | 2021-04-30 | 2022-11-01 | 上海凯赛生物技术股份有限公司 | Polyamide 56 textured yarn and preparation method thereof |
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| CN102046859A (en) * | 2008-03-26 | 2011-05-04 | 东丽株式会社 | Polyamide 56 filament, and fiber structure and air-bag base cloth each comprising the same |
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| CN102046859A (en) * | 2008-03-26 | 2011-05-04 | 东丽株式会社 | Polyamide 56 filament, and fiber structure and air-bag base cloth each comprising the same |
| JP2009240239A (en) * | 2008-03-31 | 2009-10-22 | Toray Monofilament Co Ltd | Bush cutting cord and production method thereof |
| CN103980486A (en) * | 2013-02-07 | 2014-08-13 | 上海凯赛生物技术研发中心有限公司 | Preparation method of nylon |
| CN105256395A (en) * | 2015-11-24 | 2016-01-20 | 马海燕 | Nano-modified large-diameter copolymerized polyamide monofilament and production method thereof |
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