CN114045562B - High-stability bio-based polyamide 56 fiber and preparation process thereof - Google Patents
High-stability bio-based polyamide 56 fiber and preparation process thereof Download PDFInfo
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- CN114045562B CN114045562B CN202111351452.0A CN202111351452A CN114045562B CN 114045562 B CN114045562 B CN 114045562B CN 202111351452 A CN202111351452 A CN 202111351452A CN 114045562 B CN114045562 B CN 114045562B
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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
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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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
- D01D1/00—Treatment of filament-forming or like material
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/04—Melting filament-forming substances
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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
- D01D5/098—Melt spinning methods with simultaneous stretching
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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
- D01F1/04—Pigments
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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
- D01F1/06—Dyes
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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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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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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- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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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
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
- D02G1/0206—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
- D02G1/0213—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting after drawing the yarn on the same machine
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/224—Selection or control of the temperature during stretching
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/228—Stretching in two or more steps, with or without intermediate steps
Abstract
The invention belongs to the technical field of textile materials, and discloses a high-stability bio-based polyamide 56 fiber, which comprises a high-stability bio-based polyamide 56 as a raw material, wherein the relative viscosity of the high-stability bio-based polyamide 56 is 2.2 to 3.6, the content of amino end groups is 30 to 65meq/kg, tiO is 2 The content is 0% -2% of the weight of the fiber. And a method for preparing the fiber is also disclosed. The invention adopts the high-stability nylon polymer raw material to prepare the high-stability bio-based polyamide fiber, and has good spinnability; the prepared fiber still has good aging resistance under the long-term use state.
Description
Technical Field
The invention belongs to the technical field of textile materials, and particularly relates to a high-stability bio-based polyamide 56 fiber and a preparation process thereof.
Background
The polyamide 56 is used as a bio-based polyamide material, and the main raw materials of the polyamide are pentanediamine and adipic acid, wherein the pentanediamine is prepared by biological fermentation, and the source of the pentanediamine is plant raw materials such as corn starch. Like other polyamide fibers, polyamide 56 fibers are susceptible to degradation under light, heat, oxygen and impurities, resulting in aging and yellowing. At present, the spinnability and the dyeing property of the polyamide 56 fiber and the long-term stability of the fabric are still puzzled problems after the development of the polyamide 56 filament fiber is started, so that the market popularization is limited, and particularly in the aspect of brand clothing application. The high-stability nylon 56 polymer raw material is a very key quality guarantee for developing downstream applications of nylon 56 such as textile fibers or engineering plastics.
The patent "nylon fiber and its preparation method (201710193878.8)" discloses a preparation method of nylon fiber, which comprises the steps of directly spinning after carrying out polymerization reaction on raw materials containing 1, 5-pentanediamine and adipic acid. The patent "a nylon fiber (201310060413.4)" discloses a nylon fiber, the raw material of which comprises nylon resin prepared by taking pentanediamine and aliphatic dibasic acid as raw materials, wherein at least one of the pentanediamine and the aliphatic dibasic acid is prepared by a biological method, and the nylon fiber also comprises polyamide 56 fiber. However, polyamide 56 is easily degraded under high temperature conditions, and similar to polyamide 66, it is easily gelled under high temperature conditions, which has a great influence on the stability of industrial production for a long time and the quality of the product. According to the literature data available at present, the melting point of polyamide 56 is generally between 250 and 255 ℃, and the spinning temperature is generally between 280 and 290 ℃ in order to maintain the stability of spinning (physical properties and spinnability of nylon 56 [ J ], polyester industry [ 2014, 27 (1): 38-39 ], preparation and characterization of novel nylon 56 fibers [ D ], donghua university, 2014 ]. However, when the temperature reaches 275 ℃, the polyamide 56 starts to degrade and gel, and the processing temperature is not suitable to exceed 275 ℃ for a long time in order to ensure the production stability and the product quality, but the good fluidity of the melt of the polyamide 56 cannot be ensured because the melting point of the polyamide 56 is 250-255 ℃ and the processing temperature is below 275 ℃.
The patent 'polyamide resin' (application number 200780017406.9) provides polyamide resin with excellent retention thermal stability and higher biomass ratio, nylon 56 salt generated by the reaction of pentanediamine and adipic acid is polymerized with caprolactam with the addition ratio of 3% -25%, and phosphite is used as a heat stabilizer. The patent 'a heat-resistant modified chinlon 56 polymer and a preparation method thereof' (application number 201610428381.2) adopts modified montmorillonite such as alkylamine salt or alkyl ammonium phosphate salt and the like as a heat-resistant agent to improve the heat resistance of chinlon 56, but no subsequent industrialization work exists. The patent "a yellowing-resistant polyamide resin and a preparation method thereof" (application No. 201811473696.4) relates to a polyamide resin with good yellowing resistance and a preparation method thereof. According to the method, the anti-yellowing agent and the antioxidant are added, and the oxygen removal operation treatment is used, so that the generation of impurities in the pentamethylene diamine-adipic acid nylon salt is effectively inhibited, and the yellowing resistance of the polyamide resin under high-temperature and illumination conditions can be improved. The invention discloses a one-step continuous forming and flexible deformation preparation process and equipment for a polyamide 56 filament (application number 202011403474.2), and discloses the one-step continuous forming and flexible deformation preparation process and equipment for the polyamide 56 filament. The one-step continuous forming and flexible deformation preparation process of the polyamide 56 filament mainly comprises three parts: the invention relates to a polyamide salt solution polymerization process, a spinning forming process and a flexible post-processing process, and the method can be used for continuously preparing Fully Drawn Yarns (FDY), draw Textured Yarns (DTY), air Textured Yarns (ATY) and the like in one step. The patent does not solve the light and heat stability problems of nylon 56 fiber, and the produced fiber is easy to have dyeing problem.
These methods can significantly improve the thermal stability of bio-based nylon, but have two problems: 1) The heat-resistant agent of the bio-based nylon has the problem of saturated use and failure in a long-term use state; 2) The anti-yellowing agent or antioxidant employed may react with titanium dioxide, a delustering agent for textile fibers, to cause coagulation of titanium dioxide, thereby affecting the spinnability of the bio-based nylon resin.
Disclosure of Invention
In response to the above-mentioned deficiencies of the prior art, one aspect of the present invention is directed to a high stability bio-based polyamide 56 fiber.
The high-stability bio-based polyamide 56 fiber comprises a raw material of high-stability bio-based polyamide 56, wherein the relative viscosity of the high-stability bio-based polyamide 56 is 2.2 to 3.6, the content of amino end groups is 30 to 65meq/kg, and TiO 2 The content of the (titanium dioxide) is 0-2.0% of the weight of the fiber.
Preferably, the high-stability bio-based polyamide 56 has a relative viscosity of 2.4 to 2.8.
Preferably, the content of the amino end groups is 35 to 65 meq/kg.
Preferably, the high-stability organismWhen the polyamide 56 fiber is bright, tiO 2 The content is 0 percent of the weight of the fiber; the high-stability bio-based polyamide 56 fiber is semi-extinction TiO 2 The content is 0.3 percent of the weight of the fiber; the high-stability bio-based polyamide 56 fiber is TiO when being fully extinguished 2 The content of the fiber is 1.0-2% of the weight of the fiber.
Another aspect of the invention relates to a process for preparing the high-stability bio-based polyamide 56 fiber.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
i) drying the high-stability bio-based polyamide 56 slices;
II) spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box body, a metering pump, a spinning pack and a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments.
Further, in the step 2), before winding, the fiber is drafted to obtain fully drawn yarn FDY; if no drafting is carried out and the winding speed is 4000-5000 m/min, the pre-oriented yarn can be obtained.
Further, the step 1) may adopt batch vacuum drum drying or continuous nitrogen drying, and preferably adopts continuous nitrogen drying.
Further, in the step 1), when continuous nitrogen is adopted for drying, the dew point of the nitrogen is controlled to be minus 10 ℃ to minus 70 ℃; the temperature of nitrogen is 50-100 ℃; the oxygen content in nitrogen is 0-10ppm; drying for 10-30 hours; the water content of the dried slices is 200ppm to 1500ppm.
Preferably, the dew point of nitrogen is controlled to be minus 30 ℃ to minus 60 ℃; the temperature of nitrogen is 60-85 ℃; the oxygen content in nitrogen is 0 to 5ppm; drying for 15-24 hours; the water content of the dried slices ranges from 500ppm to 1200ppm.
Further, the step 2) is that the temperature of the screw for extruding and melting the polyamide 56 chip is set as follows: first zone temperature: 250-300 ℃; temperature in the second zone: 250 to 300 ℃; third zone temperature: 250-300 ℃; temperature in the fourth zone: 250-300 ℃; temperature in the fifth zone: 250-300 ℃; temperature in the sixth zone: 250-300 ℃.
Further, the temperature of the screw for extruding and melting the polyamide 56 chips was set as follows: first zone temperature: 260-290 ℃; temperature in the second zone: 270-290 ℃; temperature of the third zone: 270-290 ℃; temperature in the fourth zone: 270-290 ℃; temperature in the fifth zone: 270-290 ℃; temperature in the sixth zone: 270 ℃ to 290 ℃.
Further, in the step 2), the rotating speed of the screw is 50-100 r/min; preferably 55 to 95r/min;
further, the temperature of the spinning manifold is 260-300 ℃, preferably 270-290 ℃;
further, the cooling air blower is cooled by adopting a side air blowing mode, the air speed is 0.20-0.90 m/min, and preferably 0.3-0.6 m/min; the wind temperature is 15-25 ℃, preferably 18-24 ℃; the wind pressure is 300-500 Pa, preferably 350-480Pa;
further, the POY spinning speed is 4000 to 5500m/min, preferably 4200 to 5000m/min.
Further, the FDY drawing multiple is 1.1 to 2.0, preferably 1.2 to 1.6; the speed of the first roller (GR 1) is 3000 to 5000m/min, preferably 3500 to 4500m/min; the speed of the second roller (GR 2) is 4000 to 5500m/min, preferably 3500 to 5000m/min; the temperature of the first roller (GR 1) is 20 to 50 ℃, preferably 30 to 45 ℃; the temperature of the second roller (GR 2) is 120 to 200 ℃, preferably 130 to 160 ℃.
The winding speed of FDY is 4000-5500 m/min, preferably 4200-5000 m/min.
Further, POY is subjected to stretching false twisting deformation to obtain stretching deformation yarn DTY, and the POY is sequentially subjected to post-processing processes of hot stretching, twisting, networking, heat setting, oiling and winding: the hot drawing process can be primary drawing, secondary drawing or multistage drawing, the temperature is 100-220 ℃, and the temperature is preferably 160-200 ℃; the draft multiple is 1.01-2.00, preferably 1.1-1.9; the speed of the drawing roller is 300-1000 m/min; preferably 400 to 900m/min; the twisting is divided into S twisting or Z twisting, the twisting tension is 20-60 cN, preferably 25-55cN; untwisting tension of 25-65 cN, preferably 25-60cN; the ratio D/Y of the surface speed of the friction disc to the speed of the yarn leaving the false twister is 1.2 to 2.5, preferably 1.5 to 2.0; the network wind pressure is 0.5-3.0 bar, preferably 1.0-2.0 bar; the diameter of the nozzle is 1.0 to 3.0mm, preferably 1.2 to 1.8mm; the heat setting temperature is 180-220 ℃, preferably 190-215 ℃; the winding speed is 400-1200 m/min, preferably 500-800m/min.
Further, FDY or a mixed yarn of FDY and POY is subjected to post-processing processes of hot drawing, thermal spraying deformation, cooling stabilization and winding in sequence to obtain the polyamide 56 Air Textured Yarn (ATY).
If the air textured yarn adopts FDY as a raw material, drafting is not needed; if the raw material contains POY, the hot drawing process can be primary drawing, the temperature is 100-190 ℃, the drawing multiple is 1.01-2.00, and preferably 1.1-1.9; the speed of the drawing roller is 1500-2500 m/min, preferably 1600-240m/min; the temperature of hot spraying deformation air is 190-230 ℃, preferably 195-225 ℃; the air injection pressure is 195-550 kPa, preferably 200-500kPa; the overfeed rate is 15-30%, preferably 18-28%; the temperature of the cooling air is 15-30 ℃, preferably 18-28 ℃; the winding speed is 1500-2800 m/min; preferably 1600 to 2750m/min.
The preparation of the high-stability bio-based polyamide 56 comprises the following steps:
1) Under the protection of nitrogen, pentanediamine and dibasic acid in stoichiometric ratio react in water at room temperature to prepare a nylon 56 salt solution; or directly and uniformly mixing nylon 56 salt and water to prepare a nylon 56 salt solution, wherein the mass concentration of the nylon 56 salt solution is 40-70%, and the pH value is 6.0-10.0;
2) Adding 0.1 to 5 parts of hindered phenol antioxidant and 0.1 to 5 parts of hindered amine light stabilizer into 90 to 100 parts of nylon 56 salt solution according to a ratio, and uniformly stirring; heating the nylon 56 salt solution to a boiling point for concentration, wherein the concentration of the concentrated polyamide 56 salt solution is 65-95%;
3) Feeding the concentrated polyamide 56 salt solution obtained in the step 2) into a continuous polymerization pre-polymerizer, and controlling the reaction temperature to be 200-270 ℃, the pressure to be 1.0-3.0 MPa and the reaction time to be 1-4 hours;
4) Flashing, reducing the pressure of a reaction system to 0.0Pa, and keeping the flashing temperature at 260-300 ℃;
5) Feeding the melt obtained after flash evaporation into an after-polymerizer, controlling the temperature to be 260-300 ℃, the pressure to be 0.0 pa-0.1 Mpa, and the after-polymerization retention time to be 20-60 minutes to obtain a nylon 56 polymer final-polymerized melt;
if the flatting agent is added, the prepared TiO2 and water suspension can be added in any step of the steps 1) to 5);
6) And (3) carrying out strand cutting on the melt obtained in the step 5) to obtain polyamide 56 chips.
Preferably, in the step 1), the molar ratio of the pentanediamine to the dibasic acid is 1-1.05, the concentration of the nylon 56 salt solution is 50% -65%, and the pH value is 7.0-9.0; in the step 2), the concentration of the concentrated polyamide 56 salt solution is 75-90%; in the step 3), controlling the reaction temperature to be 220 to 250 ℃, the pressure to be 1.5 to 2.5MPa, and the reaction time to be 2 to 3 hours; in the step 4), the flash evaporation temperature is 275-285 ℃; in the step 5), the temperature is controlled to be 270 to 290 ℃, and the polymerization residence time is 30 to 40 minutes.
Preferably, the mass percentage of the hindered phenol antioxidant to the hindered amine light stabilizer is 0.3 to 2 parts.
Preferably, the hindered phenol antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; the hindered amine light stabilizer is 4-amino-2, 6-tetramethylpiperidine and/or bis (2, 6-tetramethyl-3-piperidinylamino) -isophthalamide; particularly preferably, the hindered amine light stabilizer is 4-amino-2, 6-tetramethylpiperidine.
Preferably, the high stability bio-based polyamide 56 chip may further include any auxiliary agent that does not impair the effects of the present invention. Such adjuvants include, but are not limited to: plasticizers, antistatic agents, flame retardants, catalysts, molecular weight regulators, hydrolysis resistance agents, fluorescent agents, dyes, inorganic powders such as inorganic pigments, delustering agents, nucleating agents, and anti-ultraviolet agents, and the like, any of which may be added alone or in any combination.
Compared with the prior art, the high-stability bio-based polyamide fiber prepared by the high-stability nylon polymer has good spinnability; the prepared fiber still has good aging resistance in a long-term use state.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
The following examples, a sample of polyamide 56 filaments, was tested for properties according to the following method:
breaking strength, elongation at break: GB/T143442008 chemical fiber filament tensile property test method;
moisture regain: GB/T65032017 chemical fiber moisture regain test method;
limiting oxygen index: GB/T54541997 textile flammability test oxygen index method;
melting point: the test was carried out using a differential scanning calorimeter model Q2000 from TA, USA, with a temperature rise from room temperature to 300 ℃ at a rate of 10 ℃/min under nitrogen.
Example 1
The high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity of 2.45, the content of terminal amino groups of 35 meq/kg and bright TiO 2 The content is 0%; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 600ppm water;
the continuous nitrogen drying equipment comprises a feeding bin, two intermediate bins (used for storing intermediate materials and replacing air in the materials with nitrogen), a drying tower and a nitrogen circulating system for drying (comprising a molecular sieve or a cold dryer for reducing the dew point of nitrogen, a heat exchanger for heating and raising the temperature of nitrogen, a fan, a cyclone separator, a hydrogen adding system, a palladium catalyst reactor and the like). The continuous nitrogen drying equipment is commercially available.
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning assembly and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps: the rotating speed of the screw is 70r/min; the screw is generally provided with 6 zones, the first three: particularly, the heating power of the second area and the third area is larger, the slicing is changed into a melt state from a solid state, and the rapid temperature rise is mainly completed in the front three areas, and the temperature of each area of the screw is as follows in sequence: 250 ℃ in the first region, 288 ℃ in the second region, 285 ℃ in the third region, 283 ℃ in the fourth region, 283 ℃ in the fifth region and 283 ℃ in the sixth region; the temperature of a spinning box body is 283 ℃; cooling and solidifying the melt thin flow into fibers by side air blowing, wherein the cooling air speed is 0.6m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil feeding amount is controlled by the oil feeding amount of an oil pump, and the oil feeding amount of the POY is 0.3 percent; POY spinning speed is 4350m/min; the POY specification is 33dtex/24f, the breaking strength is 3.0cn/dtex, and the elongation at break is 75 percent.
The polyamide 56POY is subjected to stretching false-twist texturing to obtain DTY, and the DTY process of the false-twist textured yarn comprises the following steps: the drafting temperature is 200 ℃; the drawing multiple is 1.2; the speed of the drawing roller is 550m/min; the twisting is divided into S twisting or Z twisting, and the twisting tension is 30cN; untwisting tension 30cN; the ratio D/Y of the surface speed of the friction disc to the speed of the filament leaving the false twister is 1.5; the network wind pressure is 1.0bar; the diameter of the nozzle is 1.0mm; the heat setting temperature is 200 ℃; the winding speed was 500m/min.
The DTY specification is 27.5dtex/24f, the breaking strength is 3.8cn/dtex, the elongation at break is 28 percent, and the moisture regain is 5.5 percent. The DTY fiber is placed in an oven at 180 ℃ for 30min, the fiber does not yellow, the breaking strength is detected to be 3.7cn/dtex, and the elongation at break is 26%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the breaking elongation of the fiber are detected to be 3.8cn/dtex and 27 percent.
Example 2
A high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity is 2.55, the content of terminal amino groups is 45 meq/kg, and the content of semi-dull TiO2 is 0.3%; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 600ppm water;
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning pack and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps:
the rotating speed of the screw is 70r/min, and the temperatures of all zones of the screw are as follows in sequence: 250 ℃ in the first region, 288 ℃ in the second region, 285 ℃ in the third region, 283 ℃ in the fourth region, 283 ℃ in the fifth region and 283 ℃ in the sixth region; the temperature of a spinning box body is 283 ℃; cooling and solidifying the melt thin flow into fibers by side air blowing, wherein the cooling air speed is 0.6m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil loading of the POY is 0.4 percent; POY spinning speed is 4350m/min; POY specification 55dtex/24f, breaking strength 3.0cn/dtex, and elongation at break 75%.
The polyamide 56POY is subjected to stretching false-twist texturing to obtain DTY, and the DTY process of the false-twist textured yarn comprises the following steps: the drafting temperature is 200 ℃; the drawing multiple is 1.2; the speed of the drawing roller is 650m/min; the twisting is divided into S twisting or Z twisting, and the twisting tension is 30cN; untwisting tension of 30cN; the ratio D/Y of the surface speed of the friction disc to the speed of the yarn leaving the false twister is 1.5; the network wind pressure is 1.0bar; the diameter of the nozzle is 1.0mm; the heat setting temperature is 200 ℃; the winding speed was 600m/min.
The DTY specification is 44dtex/24f, the breaking strength is 3.7cn/dtex, the elongation at break is 28 percent, and the moisture regain is 5.5 percent. The DTY fiber is placed in an oven at 180 ℃ for 30min, the fiber does not yellow, the breaking strength is detected to be 3.6 cn/dtex, and the elongation at break is 26%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the breaking elongation of the fiber are detected to be 3.7cn/dtex and 27 percent.
Example 3
A high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity is 2.65, the content of terminal amino groups is 55 meq/kg, and the content of full-dull TiO2 is 1.6%; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 1000ppm water;
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning assembly and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps:
the rotating speed of the screw is 60r/min, and the temperatures of all zones of the screw are as follows in sequence: 250 ℃ in the first region, 285 ℃ in the second region, 285 ℃ in the third region, 283 ℃ in the fourth region, 283 ℃ in the fifth region and 283 ℃ in the sixth region; the temperature of a spinning box body is 283 ℃; the melt thin flow is cooled and solidified into fiber by side air blowing, and the cooling air speed is 0.4m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil amount on the POY is 1.0 percent;
the FDY drafting multiple is 1.2, and the speed of a first roller (GR 1) is 4000m/min; the speed of the second roll (GR 2) is 4880m/min; the temperature of the first roller (GR 1) is 30 ℃; the temperature of the second roller (GR 2) is 150 DEG C
Winding speed: 4880m/min;
FDY specification 22dtex/24f, breaking strength 4.0cn/dtex, elongation at break 43%, moisture regain 5.5%. Placing the FDY fiber in an oven at 180 ℃ for 30min, wherein the fiber is not yellowed, and detecting that the breaking strength of the FDY fiber is 4.1 cn/dtex and the elongation at break is 44%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the elongation at break of the fiber are detected to be 3.9cn/dtex and 42 percent.
Example 4
A high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity is 2.75, the content of terminal amino groups is 60 meq/kg, and the content of semi-dull TiO2 is 0.3%; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 600ppm water;
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning pack and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps:
the rotating speed of the screw is 70r/min, and the temperatures of all zones of the screw are as follows in sequence: 250 ℃ in a first area, 285 ℃ in a second area, 285 ℃ in a third area, 283 ℃ in a fourth area, 280 ℃ in a fifth area and 280 ℃ in a sixth area; the temperature of a spinning box body is 280 ℃; the melt thin flow is cooled and solidified into fiber by side air blowing, and the cooling air speed is 0.4m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil amount on the POY is 1.0 percent;
the FDY drafting multiple is 1.2, and the speed of a first roller (GR 1) is 4000m/min; the second roll (GR 2) speed was 4880m/min; the temperature of the first roller (GR 1) is 30 ℃; the temperature of the second roller (GR 2) is 150 DEG C
Winding speed: 4880m/min;
FDY specification 44dtex/34f, breaking strength 4.5cn/dtex, elongation at break 45 percent and moisture regain 5.5 percent; the oxygen index was 27. Placing the FDY fiber in an oven at 180 ℃ for 30min, wherein the fiber does not yellow, and detecting that the breaking strength of the FDY fiber is 4.4cn/dtex and the elongation at break is 44%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the elongation at break of the fiber are detected to be 4.4cn/dtex and 45 percent respectively.
Example 5
A high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity is 3.0, the content of terminal amino groups is 40 meq/kg, and the fiber is bright; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 600ppm water;
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning pack and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps:
the rotating speed of the screw is 70r/min, and the temperatures of all zones of the screw are as follows in sequence: the temperature of the first zone is 255 ℃, the temperature of the second zone is 285 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 285 ℃, the temperature of the fifth zone is 283 ℃, and the temperature of the sixth zone is 283 ℃; the temperature of a spinning box body is 283 ℃; cooling and solidifying the melt thin flow into fibers by side air blowing, wherein the cooling air speed is 0.6m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil amount on the POY is 1.0 percent;
the FDY drafting multiple is 1.4, and the speed of a first roller (GR 1) is 3500m/min; the second roll (GR 2) speed was 4900m/min; the temperature of the first roller (GR 1) is 30 ℃; the temperature of the second roller (GR 2) is 150 DEG C
Winding speed: 4850m/min;
FDY specification 111dtex/34f, breaking strength 6.0cn/dtex, elongation at break 35%, moisture regain 5.5%; the oxygen index was 27. Placing the FDY fiber in an oven at 180 ℃ for 30min, wherein the fiber is not yellowed, and detecting that the breaking strength of the FDY fiber is 5.8cn/dtex and the elongation at break is 33%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the breaking elongation of the fiber are detected to be 5.9cn/dtex and 34 percent.
Example 6
A high-stability bio-based polyamide 56 fiber comprises the raw materials of high-stability bio-based polyamide 56, the relative viscosity is 3.4, the content of terminal amino groups is 40 meq/kg, and the fiber is bright; melting point 252 ℃.
The preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
1) Drying the high-stability bio-based polyamide 56 slices; and (3) a drying process: the dew point of nitrogen is-40 ℃; the oxygen content in the nitrogen is less than 3ppm; the drying temperature is 72 ℃; drying time is 18 hours; the dry slices contained 400ppm water;
2) Spinning the chips obtained after drying in the step 1), extruding and melting the polyamide 56 chips by a screw, spraying the molten polyamide 56 chips through a spinning pipeline, a spinning box, a metering pump and a spinning assembly and finally a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain the polyamide 56 filaments. The spinning process comprises the following steps:
the rotating speed of the screw is 70r/min, and the temperatures of all zones of the screw are as follows in sequence: 255 ℃ in the first zone, 290 ℃ in the second zone, 290 ℃ in the third zone, 285 ℃ in the fourth zone, 285 ℃ in the fifth zone and 285 ℃ in the sixth zone; the temperature of a spinning manifold is 285 ℃; the melt thin flow is cooled and solidified into fiber by side air blowing, and the cooling air speed is 0.6m/min; the wind temperature is 21 ℃, and the wind pressure is 400Pa; the oil amount on the POY is 1.0 percent;
the FDY drafting multiple is 1.6, and the speed of a first roller (GR 1) is 3000m/min; the speed of the second roller (GR 2) is 4800m/min; the temperature of the first roller (GR 1) is 30 ℃; the temperature of the second roller (GR 2) is 150 DEG C
Winding speed: 4750m/min;
FDY specification 111dtex/34f, breaking strength 7.5cn/dtex, elongation at break 25%, moisture regain 5.5%; the oxygen index was 27. Placing the FDY fiber in an oven at 180 ℃ for 30min, wherein the fiber does not yellow, and detecting that the breaking strength of the FDY fiber is 7.3cn/dtex and the elongation at break is 23%; the fiber is not yellowed after being irradiated by an ultraviolet lamp for 120 hours, and the breaking strength and the breaking elongation of the fiber are detected to be 7.4cn/dtex and 24 percent.
Example 7
Raw materials: high-stability polyamide 56FDY44dtex/34f, semi-dull, 4.5cn/dtex breaking strength and 45% elongation at break;
ATY process: no drafting is required; the temperature of hot-spraying deformation air is 220 ℃; air injection pressure 500kPa; the overfeed rate is 20 percent; the temperature of the cooling air is 25 ℃; the winding speed was 2750m/min.
ATY specification: 99dtex/68f, breaking strength of 3.8cn/dtex, elongation at break of 45 percent and moisture regain of 5.5 percent.
Example 8
The preparation method of the high-stability bio-based polyamide 56 comprises the following steps:
1) Under the protection of nitrogen with the purity of more than 99%, the molar ratio of the pentanediamine to the adipic acid is 1.03:1 neutralizing in desalted water to obtain nylon 56 salt with the pH value of 7.5;
2) 0.5 part of tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid]Pentaerythritol ester, 0.5 part of 4-amino-2, 6-tetramethylpiperidine and 1.6 parts of TiO 2 Adding 99 parts of nylon 56 salt solution, and uniformly stirring; concentrating the nylon 56 salt solution under the conditions of 0.15MPa of pressure and 150 ℃ to reach the polymer concentration of 85 percent;
3) Feeding 85% nylon 56 salt solution into a pre-polymerizer, wherein the pressure is 1.7MPa, the pre-polymerization time is 3 hours in total at three temperatures of 220 ℃, 235 ℃ and 250 ℃, and the reaction time is about 1 hour at each temperature;
4) Flashing the polymer, reducing the pressure to 0.0Pa, and enabling the temperature of the polymer system to reach 275 ℃;
5) The melt enters a post-polymerizer, the temperature is maintained at 280 ℃, the pressure is normal, and the reaction time is 20 minutes, so that a final polymer is obtained;
6) And cooling the melt in circulating water at 2 ℃, and granulating and forming.
The resulting nylon 56 was determined to have a relative viscosity of 2.75 and a melting point of 252 ℃.
The foregoing description has described specific embodiments of the present invention. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (7)
1. The high-stability bio-based polyamide 56 fiber is characterized in that raw materials comprise the high-stability bio-based polyamide 56, the relative viscosity of the high-stability bio-based polyamide 56 is 2.2 to 3.6, the content of amino end groups is 30 to 65meq/kg, tiO is 2 The content is 0% -2.0% of the weight of the fiber;
the preparation process of the high-stability bio-based polyamide 56 fiber comprises the following steps:
i) drying the high-stability bio-based polyamide 56 slices;
II) spinning the slices obtained after drying in the step I), extruding and melting the high-stability bio-based polyamide 56 slices by a screw, and then spraying the slices through a spinning pipeline, a spinning box body, a metering pump, a spinning assembly and a spinneret plate to obtain melt trickle, cooling and blowing the melt trickle to solidify the melt trickle into fibers, and oiling and winding the fibers to obtain high-stability bio-based polyamide 56 filaments;
the step I) adopts continuous nitrogen for drying, and when the continuous nitrogen is adopted for drying, the dew point of the nitrogen is controlled to be minus 10 ℃ to minus 70 ℃; the temperature of nitrogen is 50-100 ℃; the oxygen content in nitrogen is 0-10ppm; drying for 10-30 hours; the water content of the dried slices is 200ppm to 1500ppm;
the preparation process of the high-stability bio-based polyamide 56 slice comprises the following steps:
1) Under the protection of nitrogen, pentanediamine and dibasic acid in stoichiometric ratio react in water at room temperature to prepare a nylon 56 salt solution; or directly and uniformly mixing nylon 56 salt and water to prepare a nylon 56 salt solution, wherein the mass concentration of the nylon 56 salt solution is 40-70%, and the pH value is 6.0-10.0;
2) Adding 0.1 to 5 parts of hindered phenol antioxidant and 0.1 to 5 parts of hindered amine light stabilizer into 90 to 100 parts of nylon 56 salt solution according to a ratio, and uniformly stirring; heating the nylon 56 salt solution to a boiling point for concentration, wherein the concentration of the concentrated nylon 56 salt solution is 65-95%;
3) Feeding the concentrated nylon 56 salt solution obtained in the step 2) into a continuous polymerization pre-polymerizer, and controlling the reaction temperature to be 200-270 ℃, the pressure to be 1.0-3.0 MPa and the reaction time to be 1-4 hours;
4) Flashing, reducing the pressure of a reaction system to 0.0Pa, and keeping the flashing temperature at 260-300 ℃;
5) Feeding the melt obtained after flash evaporation into a post-polymerizer, controlling the temperature to be 260-300 ℃, the pressure to be 0.0 pa-0.1 Mpa, and the post-polymerization residence time to be 20-60 minutes to obtain a nylon 56 polymer final polymerization melt;
adding TiO in any step of the steps 1) to 5) 2 ；
6) And 5) bracing and dicing the melt obtained in the step 5) to obtain high-stability bio-based polyamide 56 slices.
2. The high-stability bio-based polyamide 56 fiber as claimed in claim 1, wherein the high-stability bio-based polyamide 56 has a relative viscosity of 2.4 to 2.8; the content of the terminal amino groups is 35 to 65 meq/kg.
3. The high-stability bio-based polyamide 56 fiber as claimed in claim 1, wherein the step ii) is to draft the fiber before winding to obtain fully drawn yarn FDY; if no drafting is carried out, and the winding speed is 4000 m/min-5000 m/min, the pre-oriented yarn POY is obtained.
4. The high stability bio-based polyamide 56 fiber as claimed in claim 1, wherein said step ii), the temperature setting of the screw for extruding and melting the high stability bio-based polyamide 56 slice: the temperature of the first zone to the temperature of the sixth zone are 250-300 ℃, and the rotating speed of the screw is 50-100 r/min; the temperature of the spinning manifold is 260-300 ℃; the cooling air is cooled by adopting a side blowing mode, the air speed is 0.20-0.90 m/min, the air temperature is 15-25 ℃, and the air pressure is 300-500 Pa.
5. The high-stability bio-based polyamide 56 fiber as claimed in claim 3, wherein the POY spinning speed is 4000-5500 m/min; the FDY drafting multiple is 1.1 to 2.0, the first roll speed is 3000 to 5000m/min, the second roll speed is 4000 to 5500m/min, the first roll temperature is 20 to 50 ℃, and the second roll temperature is 120 to 200 ℃; the winding speed of FDY is 4000-5500 m/min.
6. The high-stability bio-based polyamide 56 fiber as claimed in claim 3, wherein the POY is subjected to draw false twist texturing to obtain draw textured yarn DTY, and the POY is subjected to post-processing procedures of hot drawing, twisting, network, heat setting, oiling and winding in sequence: the hot drawing process is primary drawing, secondary drawing or multistage drawing, the temperature is 100-220 ℃, the drawing multiple is 1.01-2.00, the speed of a drawing roller is 300-1000 m/min, the twisting is divided into S twisting or Z twisting, the twisting tension is 20-60 cN, the untwisting tension is 25-65 cN, the ratio of the surface speed of a friction disc to the speed of a strand thread leaving a false twister is 1.2-2.5, the network wind pressure is 0.5-3.0 bar, the diameter of a nozzle is 1.0-3.0 mm, the heat setting temperature is 180-220 ℃, and the winding speed is 400-1200 m/min;
the air textured yarn ATY is obtained by carrying out post-processing processes of hot drawing, thermal jet texturing, cooling stabilization and winding on FDY or mixed yarn of FDY and POY in sequence; if the air textured yarn adopts FDY as a raw material, drawing is not needed; if the raw material contains POY, the hot drawing process is primary drawing, the temperature is 100-190 ℃, the drawing multiple is 1.01-2.00, the speed of a drawing roller is 1500-2500 m/min, the temperature of hot jet deformation air is 190-230 ℃, the air jet pressure is 195-550 kPa, the overfeed rate is 15-30%, the temperature of cooling stable air is 15-30 ℃, and the winding speed is 1500-2800 m/min.
7. The high stability bio-based polyamide 56 fiber as claimed in claim 1, wherein the hindered phenolic antioxidant is pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; the hindered amine light stabilizer is 4-amino-2, 6-tetramethylpiperidine and/or bis (2, 6-tetramethyl-3-piperidinylamino) -isophthalamide.
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