CN114411280B - Preparation method of nylon 56 short fiber with low shrinkage - Google Patents
Preparation method of nylon 56 short fiber with low shrinkage Download PDFInfo
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- CN114411280B CN114411280B CN202210111597.1A CN202210111597A CN114411280B CN 114411280 B CN114411280 B CN 114411280B CN 202210111597 A CN202210111597 A CN 202210111597A CN 114411280 B CN114411280 B CN 114411280B
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- 229920006118 nylon 56 Polymers 0.000 title claims abstract description 76
- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000009987 spinning Methods 0.000 claims abstract description 38
- 238000009998 heat setting Methods 0.000 claims abstract description 24
- 238000004804 winding Methods 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 229920006052 Chinlon® Polymers 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 9
- 238000009736 wetting Methods 0.000 claims abstract description 7
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 16
- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001361 adipic acid Substances 0.000 claims description 14
- 235000011037 adipic acid Nutrition 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- 239000004472 Lysine Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000002074 melt spinning Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 3
- 108010048581 Lysine decarboxylase Proteins 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 2
- 238000006114 decarboxylation reaction Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 abstract description 4
- 238000002788 crimping Methods 0.000 abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 1
- 239000000155 melt Substances 0.000 description 13
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 7
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- OKMZYAZKTBCUNV-UHFFFAOYSA-N C(C)(=O)O.C(CCCC)(N)N Chemical compound C(C)(=O)O.C(CCCC)(N)N OKMZYAZKTBCUNV-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 235000018977 lysine Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 108090000489 Carboxy-Lyases Proteins 0.000 description 1
- 235000019766 L-Lysine Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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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
- D01F6/90—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 polyamides
-
- 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
-
- 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
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
-
- 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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of a nylon 56 short fiber with low shrinkage rate, and particularly relates to the field of fiber preparation. The method comprises the steps of preparing chinlon 56 saline solution; preparing chinlon 56 slices; preparing nylon 56 polymer melt trickle; spinning the nylon 56 polymer melt trickle through a spinneret plate, cooling, guiding to a winding machine for oiling and wetting, and sequentially carrying out drafting, tension heat setting, crimping, oiling, relaxation heat setting and cutting to obtain the nylon 56 short fiber. The nylon 56 short fiber with high strength and low shrinkage rate prepared by the invention has excellent product performance, meets the industrial requirements, and can be used for various clothes such as army and army clothing, combat uniform, bags, shoes and boots, tents, sleeping bags, raincoats, protective clothing for severe weather, parachutes, socks, underwear and the like, home furnishings and knitted clothing.
Description
Technical Field
The invention relates to the field of fiber preparation, in particular to a preparation method of nylon 56 short fibers with low shrinkage.
Background
The bio-based nylon 56 fiber is a novel bio-based fiber product, has the excellent characteristics of low density, good moisture absorption and quick drying performance, high strength, good wear resistance, softness, elasticity, easiness in dyeing, low flame retardant cost, environmental protection, sustainability and the like, is derived from biological raw materials, has competitive price, has multiple functions and wide application, ensures that the raw materials of textile clothing in China are free from the constraint of petroleum raw materials, and is beneficial to the long-term development of China, particularly the army.
The bio-based nylon 56 is applied to the textile industry because it has superior strength and abrasion resistance, hygroscopicity, elasticity, intimacy to human skin, and aesthetic properties. The application of the nylon short fiber in industrial cloth has considerable prospect. The yarn for chinlon industry in China is mainly used for producing chinlon cord fabrics, conveyor belts, safety rope nets, sports materials, aquaculture materials and the like. Along with the rapid and great improvement of the domestic automobile yield, the application of automobile textiles can be greatly increased, nylon occupies a certain proportion in middle-high-grade automobile textiles, and along with the increasing requirements of people on the automobile interior trim grade, the application amount of nylon fibers in the aspect of automobile textiles in the future can be obviously increased. The performance of nylon 56 fiber such as wear resistance and flame retardance can meet the changing requirements of troops, and can be used for developing wear resistance and flame retardance protective clothing, bags, shoes, tents, sleeping bags, raincoats, protective clothing for severe weather, parachutes and the like.
The bio-based nylon 56 fiber has soft hand feeling, high melting point, good strength and wide application range, and the fiber is required to have low thermal shrinkage rate on the basis of keeping high strength in application, so that the product has good dimensional stability, for example, the dry thermal shrinkage rate is less than 4%. At present, the dry heat shrinkage rate of the common nylon 56 fiber is about 5-7%, and the application range of the fiber is limited. In order to obtain the nylon 56 fiber with high strength and low shrinkage, the nylon 56 fiber is generally produced by a two-step method, namely, firstly spinning undrawn yarn or low-oriented yarn, and then stretching and heat setting the yarn to obtain a stable fiber product.
Disclosure of Invention
Therefore, the invention provides a preparation method of nylon 56 short fiber with low shrinkage rate, which aims to solve the problem of higher heat shrinkage rate in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation method of the nylon 56 short fiber with low shrinkage rate provided by the invention comprises the following steps:
under the protection of nitrogen, bio-based pentanediamine and adipic acid react in water to obtain a nylon 56 salt water solution;
step two, adding a chinlon 56 salt aqueous solution and a molecular weight regulator into a reactor, and maintaining the pressure under the conditions that the temperature is 210-250 ℃ and the pressure is 1.7-1.85 MPa; releasing the pressure in the reactor and raising the temperature to 275-290 ℃; vacuumizing and stirring to obtain a nylon 56 polymer melt, cooling and cutting to obtain slices, and obtaining nylon 56 slices;
step three, nylon 56 slices enter a pre-spinning bin after vacuum drying, are fully stirred and mixed with quantitative nano ZnO whisker powder in the pre-spinning bin to form coated slices, and enter a spinning screw for melt spinning to obtain nylon 56 polymer melt trickle; spinning the nylon 56 polymer melt trickle through a spinneret plate, cooling, guiding to a winding machine for oiling and wetting, and sequentially carrying out drafting, tension heat setting, crimping, oiling, relaxation heat setting and cutting to obtain the nylon 56 short fiber.
In the first step, the bio-pentylene diamine is obtained by decarboxylation of lysine or lysine salt under the action of lysine decarboxylase; the molar ratio of adipic acid to bio-based pentanediamine is 1:1 to 1.15; the specific method can be 1:1.05 to 1.15, 1:1.05, 1:1.15.
further, the mass percentage of the chinlon 56 salt aqueous solution can be 30% -70%, and can be 40% -60%, 40%, 50%, 60% or 70%.
Further, in the second step, the molecular weight regulator is an acetic acid solution of bio-based pentanediamine; the addition amount of the molecular weight regulator is 0.2% -2% of the sum of the mass of the bio-based pentanediamine and the mass of the adipic acid in the first step.
Further, in the second step, the pressure maintaining time is 1-3 hours;
further, the pressure in the reactor was released and the temperature was raised to 275-290 ℃.
Further, the time of vacuum pumping and stirring can be 2 to 3.5 hours.
Further, in the third step, the step of vacuum drying is as follows: firstly, drying for 3.5-4.5 h at 90-95 ℃, then heating to 95-120 ℃ and drying for 2.5-3.5 h, and further preserving heat for 3-6 h at 120 ℃.
Further, the nano ZnO whisker is quantitatively input into a pre-spinning bin through a screw pump and mixed with the nylon 56 dry slice to form a coated slice, and the addition amount can be 0.1-0.3% of the mass of the bio-based nylon 56 slice.
Further, the melt index of the bio-based nylon 56 slice is 23-26 g/10min, and can be specifically 24.5g/10min.
Further, in the third step, the temperature conditions of the melt spinning are as follows: the temperature of the first region can be 240-250 ℃, the temperature of the second region can be 255-265 ℃, the temperature of the third region can be 270-280 ℃, the temperature of the fourth region can be 275-280 ℃, the temperature of the fifth region can be 275-285 ℃, the temperature of the sixth region can be 270-285 ℃, and the temperature of a spinning box body used can be 270-280 ℃.
In the third step, the cooling is performed by a side air blowing device, the cooling air speed is 0.5-1.3 m/min, and the air temperature is 17-26 ℃.
In the third step, the winding speed of the winding machine is 600-1200 m/min.
In the third step, the drafting is performed by a drafting roller, and the temperature of the drafting roller is 140-200 ℃; the drafting is two-stage drafting, the primary drafting multiplying power is 2.0-4.0, and the secondary drafting multiplying power is 1.0-2.0; the temperature range of tension heat setting is 160-220 ℃; the relaxation heat setting is carried out at the temperature of 90-120 ℃.
Further, the temperature of the three pairs of drafting rollers for realizing drafting is controlled as follows: the temperature of the first roller is higher than the glass transition temperature of the nylon 56 fiber, the second roller and the third roller are mainly subjected to high-power stretching, the temperature control is required to meet the stretching multiple requirement, the temperature distribution is required to be gradually increased according to the sequence of the second stretching roller and the third stretching roller so as to meet the requirement that the fiber can be gradually stretched, and the temperature range of the stretching rollers is 140-200 ℃; the drafting is secondary drafting, the primary drafting multiplying power is 2.0-4.0, and the secondary drafting multiplying power is 1.0-2.0; the tension heat setting adopts hot plate contact type heating heat setting, and the heat setting temperature range is 160-220 ℃.
Further, the number of curls of the curls may be 10 to 30.
Further, the relaxation heat setting can be carried out at the temperature of 90-120 DEG C
The invention has the following advantages:
the bio-based nylon 56 fiber prepared by the method has soft hand feeling, high melting point, good strength and wide application range, and has low thermal shrinkage rate on the basis of keeping high strength in application, so that the product has good dimensional stability, for example, the dry thermal shrinkage rate is less than 4%.
The study of the heat setting process not only can improve the dimensional stability of the fiber, but also can further improve the physical and mechanical properties of the fiber, such as wear resistance and crimping degree, and improve the dyeing property of the fiber, and the nylon 56 fiber prepared by the invention has uniform coloring, full color and good color fastness.
The nylon 56 short fiber with high strength and low shrinkage rate prepared by the invention has excellent product performance, meets the industrial requirements, and can be used for various clothes such as army and army clothing, combat uniform, bags, shoes and boots, tents, sleeping bags, raincoats, protective clothing for severe weather, parachutes, socks, underwear and the like, home furnishings and knitted clothing.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Nano ZnO whisker powder purchased from Ejia new material science and technology Co., ltd
The bio-pentylene diamine is prepared by removing carboxyl groups at two ends of lysine (salt) under the action of lysine decarboxylase (EC4.1.1.18), and specifically according to the method disclosed in literature L-lysine decarboxylase property and application research (Jiang Lili, nanjing university, shus, 2007).
The measuring method of each index in the embodiment of the invention comprises the following steps:
melting point: measured by a micro-melting point meter.
Fineness: the measurement was carried out by using a fiber fineness measuring instrument.
Density: the density gradient method is adopted to measure, two liquids with different densities and mutual miscibility are mixed in a certain proportion and a certain method, the density of the mixed liquid is gradually increased from top to bottom and has linearity by utilizing the molecular diffusion effect, and then the fiber is put into a density gradient tube according to the suspension principle, and the density of the liquid at the balance position is the density of the fiber after the fiber is balanced.
Breaking strength: taking a 10cm sample, wherein the uniform descending speed is 10mm/min, and the load during fracture is the fracture strength and the unit is the unit of force.
Elongation at break: the ratio (%) of the length extended until the fiber breaks to the length of the sample itself.
The standard moisture regain in the following examples refers to the moisture regain of the fibers in the standard state, moisture regain= (wet weight of fibers-dry weight of fibers)/dry weight of fibers.
Dry heat shrinkage: the measurement is carried out by adopting a full-automatic single fiber thermal shrinkage tester, and the detection process of the full-automatic single fiber thermal shrinkage tester implements FZ/T50004-1991 standard.
Example 1 preparation method of Low shrinkage Chinlon 56 short fiber
(1) Under the protection of nitrogen, dissolving bio-based pentanediamine in deionized water, gradually adding adipic acid, and controlling the molar ratio of the adipic acid to the bio-based pentanediamine to be 1:1.1, preparing nylon 56 salt water solution with the mass concentration of 50 percent.
(2) Adding the prepared nylon 56 salt water solution and 1% bio-based pentanediamine acetic acid solution into a reactor, and maintaining the pressure for 2 hours under the conditions of 240 ℃ and 1.8 MPa; then releasing the pressure in the reactor, vacuumizing when the temperature is raised to 285 ℃, reducing the pressure of the system to-0.06 MPa, continuously stirring for 2 hours in a vacuum state, and cooling the obtained nylon 56 polymer melt to prepare slices.
(3) The bio-based nylon 56 slice is dried in a vacuum environment, and the specific conditions are as follows: firstly, drying for 4 hours at 95 ℃, then drying for 2.5 hours at the temperature of 110 ℃, and further preserving heat for 3 hours at the temperature of 120 ℃. Then the mixture is added into a pre-spinning bin at the speed of 26 kg/hour, and a screw pump quantitatively inputs 0.3 percent of nano ZnO whisker and nylon 56 dry slices and mixes to form coated slices. The slices are melted by a screw and then enter a spinning box. The temperature of the spinning screw is: the first zone temperature is 245 ℃, the second zone temperature is 265 ℃, the third zone temperature is 275 ℃, the fourth zone temperature is 280 ℃, the fifth zone temperature is 285 ℃, the sixth zone temperature is 280 ℃, and the temperature of the spinning manifold is 280 ℃. In the spinning box, the diameter of the spinneret plate is 300mm, the number of holes is 3500 holes, the length-diameter ratio of the spinneret holes is 1.5, the assembly pressure is 10MPa, and the melt temperature is 280 ℃.
(4) The nylon 56 polymer melt is sprayed out of a spinneret plate to obtain melt trickle, and is cooled by a side air blowing device, wherein the cooling air speed is 0.6m/min, and the air temperature is 25 ℃. Cooling and solidifying the melt trickle, and then feeding the melt trickle into a winding machine, wherein the winding speed is 1100m/min. The cooled and solidified fiber tows are led to a winding panel through a jacket type spinning channel (with an exhaust valve). And (3) carrying out double-sided oil tanker oiling on the cooled and solidified yarn on a winding frame, and carrying out oiling and wetting on the yarn bundles. Drawing the oiled biobased nylon 56 primary fiber at 160 ℃ to obtain a first drawing multiple of 3.0 times and a second drawing multiple of 1.0 times, carrying out heat setting at 190 ℃, curling after drawing, carrying out curling number of 28, oiling, carrying out relaxation heat setting at 90 ℃, cutting and packaging to obtain the biobased nylon 56 short fiber with the length of 38mm.
The physical and chemical parameters of the bio-based nylon 56 short fiber prepared in the embodiment are as follows:
the melting point is 254 ℃, the standard moisture regain is 5.6%, the fineness is 1.3dtex, the density is 1.14g/cm < 3 >, the breaking strength is 6.0CN/dtex, the elongation at break is 35%, and the dry heat shrinkage is 3.0%.
Example 2 preparation method of Low-shrinkage Chinlon 56 short fiber
(1) Under the protection of nitrogen, dissolving bio-based pentanediamine in deionized water, gradually adding adipic acid, and controlling the molar ratio of the adipic acid to the bio-based pentanediamine to be 1:1.05, preparing nylon 56 salt water solution with the mass concentration of 50 percent.
(2) The prepared nylon 56 salt water solution and 1.5% bio-based pentanediamine acetic acid solution are added into a reactor together, and the pressure is maintained for 2.5 hours under the conditions of 245 ℃ and 1.85 MPa. Then releasing the pressure in the reactor, vacuumizing when the temperature is raised to 285 ℃, reducing the pressure of the system to-0.06 MPa, continuously stirring for 2.5 hours in a vacuum state, and cooling the obtained nylon 56 polymer melt to prepare slices.
(3) The bio-based nylon 56 slice is dried in a vacuum environment, and the specific conditions are as follows: firstly, drying for 4.5 hours at 90 ℃, then drying for 3.5 hours at the temperature of 95 ℃, and further preserving heat for 3 hours at 120 ℃. Then adding the mixture into a pre-spinning bin at the speed of 35.4 KG/hour, quantitatively inputting 0.1% of nano ZnO whisker and nylon 56 dry slices by a screw pump, and mixing to form coated slices. The slices are melted by a screw and then enter a spinning box. The temperature of the spinning screw is: the first zone temperature was 250 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 280 ℃, the fifth zone temperature was 285 ℃, the sixth zone temperature was 285 ℃, and the spinning manifold temperature was 280 ℃. In the spinning box, the diameter of the spinneret plate is 300mm, the number of holes is 3500 holes, the length-diameter ratio of the spinneret holes is 1.5, the assembly pressure is 10MPa, and the melt temperature is 282 ℃.
(4) The nylon 56 polymer melt is sprayed out of a spinneret plate to obtain melt trickle, and is cooled by a side air blowing device, wherein the cooling air speed is 0.8m/min, and the air temperature is 17 ℃. Cooling and solidifying the melt trickle, and then feeding the melt trickle into a winding machine, wherein the winding speed is 600m/min. The cooled and solidified fiber tows are led to a winding panel through a jacket type spinning channel (with an exhaust valve). And (3) carrying out double-sided oil tanker oiling on the cooled and solidified yarn on a winding frame, and carrying out oiling and wetting on the yarn bundles. Drafting the oiled bio-based nylon 56 primary fiber at 140 ℃, wherein the first traction multiple is 2.4 times, the second traction multiple is 1.03 times, the tension heat setting temperature is 180 ℃, curling is carried out after stretching, the number of curls is 24, oiling, loosening heat setting at 120 ℃, cutting and packaging to obtain the bio-based nylon 56 short fiber with the length of 65mm.
The physical and chemical parameters of the bio-based nylon 56 short fiber prepared in the embodiment are as follows:
the melting point is 254 ℃, the standard moisture regain is 5.0%, the fineness is 3.2dtex, the density is 1.14g/cm < 3 >, the breaking strength is 5.6CN/dtex, the elongation at break is 46%, and the dry heat shrinkage is 3.6%.
Example 3 preparation method of Low shrinkage Chinlon 56 short fiber
(1) Under the protection of nitrogen, dissolving bio-based pentanediamine in deionized water, gradually adding adipic acid, and controlling the molar ratio of the adipic acid to the bio-based pentanediamine to be 1:1.15, preparing nylon 56 salt water solution with the mass concentration of 30 percent.
(2) The prepared nylon 56 salt water solution and 0.2% bio-based pentanediamine acetic acid solution are added into a reactor together, and the pressure is maintained for 3 hours under the conditions of 210 ℃ and 1.85 MPa. Then releasing the pressure in the reactor, vacuumizing when the temperature is raised to 290 ℃, reducing the pressure of the system to minus 0.06MPa, continuously stirring for 2.5 hours in a vacuum state, and cooling the obtained nylon 56 polymer melt to prepare slices.
(3) The bio-based nylon 56 slice is dried in a vacuum environment, and the specific conditions are as follows: firstly, drying for 3.5h at 95 ℃, then drying for 3h at 110 ℃, and further preserving heat for 5h at 120 ℃. Then the mixture is added into a pre-spinning bin at the speed of 30 kg/hour, and a screw pump quantitatively inputs 0.2 percent of nano ZnO whisker and nylon 56 dry slices and mixes to form coated slices. The slices are melted by a screw and then enter a spinning box. The temperature of the spinning screw is: the first zone temperature is 245 ℃, the second zone temperature is 255 ℃, the third zone temperature is 270 ℃, the fourth zone temperature is 275 ℃, the fifth zone temperature is 280 ℃, the sixth zone temperature is 275 ℃, and the spinning manifold temperature is 280 ℃. In the spinning box, the diameter of the spinneret plate is 300mm, the number of holes is 3500 holes, the length-diameter ratio of the spinneret holes is 1.5, the assembly pressure is 10MPa, and the melt temperature is 280 ℃.
(4) The nylon 56 polymer melt is sprayed out of a spinneret plate to obtain melt trickle, and is cooled by a side air blowing device, wherein the cooling air speed is 0.5m/min, and the air temperature is 21 ℃. Cooling and solidifying the melt trickle, and then feeding the melt trickle into a winding machine, wherein the winding speed is 1000m/min. The cooled and solidified fiber tows are led to a winding panel through a jacket type spinning channel (with an exhaust valve). And (3) carrying out double-sided oil tanker oiling on the cooled and solidified yarn on a winding frame, and carrying out oiling and wetting on the yarn bundles. Drafting the oiled bio-based nylon 56 primary fiber at 180 ℃, wherein the first traction multiple is 3.8 times, the second traction multiple is 1.5 times, the tension heat setting temperature is 200 ℃, curling is carried out after stretching, the number of curls is 29, oiling, loosening heat setting at 95 ℃, cutting and packaging to obtain the bio-based nylon 56 short fiber with the length of 38mm.
The physical and chemical parameters of the bio-based nylon 56 short fiber prepared in the embodiment are as follows:
the melting point is 254 ℃, the standard moisture regain is 5.5%, the fineness is 1.7dtex, the density is 1.14g/cm < 3 >, the breaking strength is 5.9CN/dtex, the elongation at break is 38%, and the dry heat shrinkage is 3.2%.
Example 4 preparation method of Low-shrinkage Chinlon 56 short fiber
(1) Under the protection of nitrogen, dissolving bio-based pentanediamine in deionized water, gradually adding adipic acid, and controlling the molar ratio of the adipic acid to the bio-based pentanediamine to be 1:1.05, preparing chinlon 56 salt aqueous solution with the mass concentration of 60 percent.
(2) The prepared nylon 56 salt water solution and 2% bio-based pentanediamine acetic acid solution are added into a reactor together, and the pressure is maintained for 1.5 hours under the conditions of 230 ℃ and 1.75 MPa. Then releasing the pressure in the reactor, vacuumizing when the temperature is raised to 275 ℃, reducing the pressure of the system to-0.06 MPa, continuously stirring for 3.5 hours in a vacuum state, and cooling the obtained nylon 56 polymer melt to prepare slices.
(3) The bio-based nylon 56 slice is dried in a vacuum environment, and the specific conditions are as follows: firstly, drying for 3.5 hours at 93 ℃, then drying for 3.5 hours at 115 ℃ and further preserving heat for 5 hours at 120 ℃. Then adding the mixture into a pre-spinning bin at the speed of 32 kg/hour, quantitatively inputting 0.15% of nano ZnO whisker and chinlon 56 dry slices by a screw pump, and mixing to form coated slices. The slices are melted by a screw and then enter a spinning box. The temperature of the spinning screw is: the temperature of the first zone is 240 ℃, the temperature of the second zone is 260 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 275 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 275 ℃, and the temperature of the spinning manifold is 270 ℃. In the spinning box, the diameter of the spinneret plate is 300mm, the number of holes is 3500 holes, the length-diameter ratio of the spinneret holes is 1.5, the assembly pressure is 10MPa, and the melt temperature is 273 ℃.
(4) The nylon 56 polymer melt is sprayed out of a spinneret plate to obtain melt trickle, and is cooled by a side air blowing device, wherein the cooling air speed is 1.2m/min, and the air temperature is 19 ℃. Cooling and solidifying the melt trickle, and then feeding the melt trickle into a winding machine, wherein the winding speed is 800m/min. The cooled and solidified fiber tows are led to a winding panel through a jacket type spinning channel (with an exhaust valve). And (3) carrying out double-sided oil tanker oiling on the cooled and solidified yarn on a winding frame, and carrying out oiling and wetting on the yarn bundles. Drafting the oiled bio-based nylon 56 primary fiber at 200 ℃, wherein the first traction multiple is 2.7 times, the second traction multiple is 1.03 times, the tension heat setting temperature is 220 ℃, curling is carried out after stretching, the number of curls is 26, oiling, loosening heat setting at 110 ℃, cutting and packaging to obtain the bio-based nylon 56 short fiber with the length of 65mm.
The physical and chemical parameters of the bio-based nylon 56 short fiber prepared in the embodiment are as follows:
the melting point is 254 ℃, the standard moisture regain is 5.3%, the fineness is 2.2dtex, the density is 1.14g/cm < 3 >, the breaking strength is 5.8CN/dtex, the elongation at break is 43%, and the dry heat shrinkage is 3.4%.
Comparative example
The properties of the fibers having the same fineness as the conventional fiber in the examples of the present invention in terms of breaking strength, elongation at break and dry heat shrinkage are shown in Table 1.
Table 1 comparison table of performance indexes of conventional chinlon 56 staple fibers and embodiments of the present invention
As can be seen from the table, compared with the existing fiber with the same fineness in the embodiment of the invention, the fiber has higher breaking strength and lower elongation at break; lower dry heat shrinkage.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (2)
1. The preparation method of the nylon 56 short fiber with low shrinkage rate is characterized by comprising the following steps:
under the protection of nitrogen, bio-based pentanediamine and adipic acid react in water to obtain a nylon 56 salt water solution;
step two, adding a chinlon 56 salt aqueous solution and a molecular weight regulator into a reactor, and maintaining the pressure under the conditions that the temperature is 210-250 ℃ and the pressure is 1.7-1.85 MPa; releasing the pressure in the reactor and raising the temperature to 275-290 ℃; vacuumizing and stirring to obtain a nylon 56 polymer melt, cooling and cutting to obtain slices, and obtaining nylon 56 slices;
step three, nylon 56 slices enter a pre-spinning bin after vacuum drying, are fully stirred and mixed with quantitative nano ZnO whisker powder in the pre-spinning bin to form coated slices, and enter a spinning screw for melt spinning to obtain nylon 56 polymer melt trickle; spinning nylon 56 polymer melt trickles through a spinneret plate, cooling, guiding to a winding machine for oiling and wetting, and sequentially carrying out drafting, tension heat setting, curling, oiling, relaxation heat setting and cutting to obtain nylon 56 short fibers;
in the first step, bio-pentylene diamine is obtained by decarboxylation of lysine or lysine salt under the action of lysine decarboxylase; the molar ratio of adipic acid to bio-based pentanediamine is 1:1 to 1.15;
in the second step, the molecular weight regulator is an acetic acid solution of bio-pentylene diamine; the addition amount of the molecular weight regulator is 0.2% -2% of the sum of the mass of the bio-based pentanediamine and the mass of the adipic acid in the first step;
in the second step, the pressure maintaining time is 1-3 hours; stirring for 2-3.5 hours under vacuum condition;
in the third step, the vacuum drying step is as follows: firstly, drying for 3.5-4.5 hours at the temperature of 90-95 ℃, then heating to the temperature of 95-120 ℃ and drying for 2.5-3.5 hours, and continuously preserving heat for 3-6 hours at the temperature of 120 ℃;
in the third step, the nano ZnO whisker is quantitatively input into a pre-spinning bin through a screw pump and is mixed with the nylon 56 dry slice to form a coated slice, wherein the addition amount of the nano ZnO whisker is 0.1-0.3% of the mass of the bio-based nylon 56 slice;
in the third step, the temperature conditions of the melt spinning are as follows: the temperature of the first region is 240-250 ℃, the temperature of the second region is 255-265 ℃, the temperature of the third region is 270-280 ℃, the temperature of the fourth region is 275-280 ℃, the temperature of the fifth region is 275-285 ℃, the temperature of the sixth region is 270-285 ℃, and the temperature of a spinning box body used is 270-280 ℃;
in the third step, cooling is carried out by adopting a side air blowing device, the cooling air speed is 0.5-1.3 m/min, and the air temperature is 17-26 ℃;
in the third step, the drafting is performed by a drafting roller, and the temperature range of the drafting roller is 140-200 ℃; the drafting is two-stage drafting, the primary drafting multiplying power is 2.0-4.0, and the secondary drafting multiplying power is 1.0-2.0; the temperature range of tension heat setting is 160-220 ℃; the relaxation heat setting is carried out at the temperature of 90-120 ℃.
2. The method for preparing nylon 56 staple fiber with low shrinkage according to claim 1, wherein in the third step, the winding speed of the winding machine is 600-1200 m/min.
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