Composition for forming fibers

 

(57) Abstract:

The inventive composition for molding fiber contains 30 - 35 wt. % mixture of cellulose triacetate with a characteristic viscosity of 6 DL/g, forming the anisotropic phase (70% ) with thermoplastic polymer forming the isotropic phase (30% ) in the total solvent. The isotropic phase is present in the form of domains with an average size of less than 300 microns. 1 C. p. F.-ly, 4 Il. , 1 table.

The invention relates to the field of technology for composite materials, in particular the production of compositions for molding fiber-composites from blends containing lyotropic polysaccharide and thermoset polymers.

Closest to the invention is a composition for forming fibers containing a derivative of cellulose, Acrylonitrile polymer and a solvent capable of dissolving the above polymer materials. This spinning composition can be used to produce a multicomponent fiber.

This composition contains about 5-50 wt. % derived cellulose and 50-95 wt. % Acrylonitrile polymer. Acrylonitrile polymer is present as a continuous phase. Fiber, izgotovlen is present in the form of the dispersion phase of the fine fibers, included in the continuous phase Acrylonitrile polymer. Due to this structure composite fiber retains the properties of the standard acrylic fibers and can be used for the manufacture of textile products.

However, the mechanical properties of such composite fibers is not high enough.

The purpose of the invention is the improvement of strength characteristics of the fiber.

The objective is ensured by the fact that the composition contains 30-35% of a mixture consisting of 70 wt. % of cellulose triacetate with a characteristic viscosity of 6 DL/g in hexafluoroisopropanol at 30aboutWith forming the anisotropic phase and 30 wt. % thermoplastic polymer, forming an isotropic phase that is present in the form of domains with an average size of less than 300 μm in the total solvent. As thermoplastic polymer composition comprises a polyacrylonitrile or a copolymer diamine, bis-p-aminocyclohexanone, ISO - and terephthalic acid in a molar ratio of 96: 4: 70: 30 respectively. The common solvent is an aqueous solution of nitric acid or a mixture triftoruksusnoi and formic acids.

In Fig. 1 shows the image obtained using transmission electronic microsc is sushestvennee; in Fig. 2 - the image obtained with a transmission electron microscope with h and depicting a longitudinal cross-section of the fiber obtained by the proposed method in its preferred implementation of Fig. 3 - the image obtained using an optical microscope while scanning the spinning solution used in example 2; Fig. 4 - the image obtained similarly snapshot in Fig. 3, but using cross-polarized light.

For the manufacture of products in accordance with the present invention, in which the first phase containing the lyotropic polysaccharide, is essentially continuous in the direction of orientation, it is necessary, as will be shown below that the size of the isotropic domains in the spinning solution was preferably less than 300 μm, and more preferably less than 100 μm. The homogeneity of the thus obtained two-phase solution visible to the naked eye. This homogeneity can be achieved by adding polymers in solution and thoroughly mixed for a long period of time, but more preferably first added to the solvent lyotropic polymer, and then to this solution add more solution is stirring the solution or molding oriented profiled products immediately after formation of the solution.

In accordance with the proposed method first form oriented anisotropic phase two-phase solution, then the solvent is removed and get oriented profiled products. For these purposes, can be used several ways, such as forming fibers by spinning, or by extrusion of the solution into the film. The orientation of the anisotropic phase can be effected by the application of shear forces or pulling of flow in a liquid solution. The method of removing the solvent must be adapted to remove solvent from solutions with high viscosity (viscosity solutions usually exceeds 100 P). This task answer the wet formation method using the air gap and method of extrusion of films, in which the solution is passed through the die plate or the cylinder of the extruder in the air gap, and then the coagulation bath, where the solution is removed from the mixture. In accordance with the invention for forming fibers are mainly used methods of spinning fibers and extrusion film used for forming lyotropic polysaccharide polymer in high-strength fibers and films. Liquid crystalline solutions can be returned in the isotropic state if naes dies, and extruded solution is passed through coagulase fluidized bed in the coagulation bath. While passing through coagulase fluidized bed extruded solution is stretched to the size, which in 1-15 times its original size (metric stretching the molded). Fluidized bed is usually air, but may be any other inert gas or even liquid, if it is coagulase for the specified solution. Coagulase fluidized bed has a thickness of, generally, from 0.1 to 10 cm

Coagulation bath may be water or even clean water and any anhydrous coagulating liquid. The bath temperature may correspond to the freezing point or even be below the specified temperature. To obtain fibers with high tensile strength it is preferable that the temperature of the coagulation bath was maintained below -10aboutC.

After passing the extruded solution through the coagulation bath solution coagulums using coagulant in the swollen fiber. This fiber must be thoroughly rinsed to remove salt and acid from the internal parts of the swollen fiber after paducha in a furnace or by rolling the wet yarn through rollers heated steam drums.

In oriented shaped article produced by the method of the invention, lyotropic polymer is a first polymer phase of a product, and thermoset polymer comprises a second polymer phase. The first polymer phase is characterized by the fact that, in General, it is continuous in the direction of orientation of the product, when treated with increasing h. For fibers with a longitudinal direction of orientation of this structure is shown in Fig. 2, which represents the image obtained using a transmission electron microscope (FACT) when h and depicting a longitudinal cross-section of the preferred fibers of the invention. On the specified drawing the first polymer phase darker more light the second polymer phase. Continuous in the direction of orientation and longitudinally continuous fiber means that the fibrils of lyotropic polysaccharide in the first polymer phase extends mainly continuously in the direction of orientation or along the length of the product, if you look at the increase h.

The high degree of orientation is preferred. For fibers of the invention, the orientation angle is preferably less than 30about.

Throughout the second product p in Fig. 2, depicting the structure of a fiber manufactured the preferred approach.

Oriented shaped articles of the invention are capable of forming in hardened parts at elevated temperature and pressure. For the formation of the hardened parts of the fibers of the invention uses a technique commonly used to obtain prepregs, for example, by placing the fibers in an appropriate mold and pressing them at a temperature (or above) the melting point, glass transition or reaction temperature thermoset polymer when forming the hardened parts. Unidirectional composites; composites containing products, woven from fibers of the invention; composites of discontinuous fibers can also be obtained using a given technology. Fibers into a pulp or fibrous product can be directly used for the manufacture of paper by the method of wet molding of laminated plastics. These paper products can be solidified at elevated temperatures and pressures in the three-dimensional composites.

In hardened parts oriented shaped articles used to obtain composites is born and becomes something of a continuous matrix of the first polymer phase. Basically, the mechanical properties of the elongated moulded products transferred composites. Mechanical properties of composites are similar to the properties of short-fiber reinforced composites, and therefore the invention allows to obtain composites with excellent properties of molded fibers and films.

Testing methods.

Transmission electron microscope.

Images using a transmission electron microscope (THEMES) for the transverse and longitudinal cross sections of the fibers were obtained as follows.

Samples received first by pouring a well-aligned beam of fibers (approximately 100 fibers) in the epoxide. The sample for cross-sectional better to fill, using ALL-capsule size 00. For making cuts through the cone-shaped tip of the capsule along the diameter and V-neck in the flat top of the capsule used the razor. Through these two neckline has introduced a bundle of fibers so that the axis of the beam coincides with the axis of the capsule. Then the capsule was filled with resin and left to cure in an oven at 70aboutWith during the night, and then filled fibrous sample was removed from the capsule. In order to get Obi beam accumulated epoxide and the sample was left overnight for curing in an oven at 70aboutC. then from the square, covered with epoxy, cut short segment and attached it with epoxy to bikinicool rack.

From flooded fibrous samples did slice thickness 2000-2500 angstroms using ultramicrotome Du pont 6000 MT and diamond cutter, working with a speed of 0.7 mm/s When receiving a cross-sectional direction of the cutting was mainly perpendicular to the longitudinal axis of the fiber, and in the case of longitudinal-section direction of the cutting was mainly parallel to the longitudinal axis of the fiber. Then the slices were transferred to the lattice electron microscope (200 mesh, diameter = 3 mm).

JEOL TEM/S equipped with the goniometer and works in the mode of accelerating voltage of 200 Kev, allowing you to explore sections of the fibers at the desired magnification (zoom lens allows you to increase the contrast), and the image to capture on film. Then the film was placed in a photographic enlarger, where the recorded image is enlarged 3 times, which was then printed onto the paper.

Mechanical tensile properties.

Properties of the yarn were measured at 21,1aboutC and 65% relative humidity , and bring to a conforming status is the weighing yarn with a known length. Strength (grams/day, g/d, elongation (%) modulus at low short-term stress (g/d), determined according to ASTM D 2101, was calculated by curve movements under load at strain rate 10% / min for samples with a length of 25.4 cm, and weight was determined the number of yarns. Before each test yarn was twisted.

Studies of the properties of individual fibers tensile strength was determined in a similar way with the gauge length of 2.54 cm for strength and elongation and 25.4 cm for the elastic modulus. The weight room one fiber was calculated by the main resonance frequency, determined by the vibration of the fiber length of 4.1 cm in tension by varying the frequency (ADTM D 1577 method).

The orientation angle of the fiber, defined rentgenograficheski.

The bundle of fibers with a diameter of about 0.5 mm was wound on the cartridge, while trying to preserve the parallelism of the fibers. Then the cartridge is filled with fiber, was subjected to x-rays using the x-ray apparatus Filipes (Model RW) mode 40 kV and 40 mA using copper long sharply focused diffraction tube (Model PW 2273/20) and Nickel metafilter.

The XRD pattern of filaments is m camera with point holes. The diameter of the collimators in the chamber was 0,64 mm Exposure lasted for approximately 15-30 minutes (the duration should be sufficient to ensure that the measured items were recorded at an optical density of 1.0).

The measured image of the diffraction pattern was recorded by a video camera. The intensity of the missing rays were calibrated using a black and white standard, the gray level was converted into optical density. The order-of-magnitude equivalent to the azimuth line, drawn through two selected Equatorial peak, was determined by interpolation on the basis of the data file of digital images; the sequence was built so that one value point corresponded to one third of a degree of arc.

The orientation angle was transferred to the arc length in degrees at the value equal to half of the maximum optical density (angle tightening points 50% maximum density) Equatorial peaks with correction for background. This was calculated from the number of reference points between the points of half the height on each side of the peak. Then measure both peak and determined the orientation angle as the average of the two measurements.

Characteristic in the tion of 0.5 g of polymer in 100 ml of the solvent of the polymer solution, and rel - relative viscosity is the ratio between the duration of the flow of polymer solution and the duration of the solvent as measured at 30aboutWith in a capillary viscometer. The values of the characteristic viscosity for a HUNDRED was determined using hexafluoroisopropanol.

The size of the domains of the spinning solutions.

Spinning solutions was investigated using an optical microscope to establish the two-phase nature of these solutions. Samples for spinning solutions of a HUNDRED, RAP and nitric acid was placed between two object glasses. Then, to obtain a thin layer of a sample of these glasses was tightly clenched hands. Edge slides were sealed with a film (Parafilm, TM) in order to avoid loss of solvent. Then the samples were left for relaxation at room temperature over night.

The samples were observed in polarized and cross polarized light using a polarizing optical microscope (Nikon) equipped with a camera. The results of observations showed that the static (relaksirano) isotropic solutions when placed transversely between polarizing elements, in the main, did not let in any light. However, anisotropic solutions of p is opnai and anisotropic, then these two phases can be distinguished by comparing their observations in polarized and cross polarized light. All samples were observed and photographed at 100x. Used film Polaroid type 57 3000 SA. Dimensions isotropic domains was determined by measuring isotropic domains on the photos.

P R I m e R 1. The cellulose triacetate (CTA) with acetyl content of 43.7 per cent and the characteristic viscosity of 6.0 DL/g in hexafluoroisopropanol at 30aboutWith and polyamide (copolymer diamine, bis - p-iminocyclohexa methane, isophthalic acid and terephthalic acid in a molar ratio of 96/4/70/30) was dried in a vacuum oven at 80aboutC. in the nitrogen atmosphere during the night. An organic solvent consisting of tractorhouse acid (TFAA) and formic acid (FA) (mass ratio of 79/21) was mixed in a glass vessel. Then 65 wt. h the mixture was dissolved TFAA/FA was added to 24.5 wt. including one HUNDRED in a two-blade stirrer with shear effort with a capacity of 500 cm3. The mixer is pre-cooled to -5aboutWith using an external cooling device to minimize the destruction of one HUNDRED and acid. Stirring was carried out for 2 h in order to reliably wetting HUNDRED. Then it could open and spatula scraped off the undissolved polymer, which stick to the walls and the blades of the mixer. The resulting spinning solution contained 35 wt. % polymer (70 wt. % HUNDRED/30 wt. % polyamide) in 65 wt. % solvent (79 wt. % TDAA/21 wt. % FA). The specified spinning solution showed the homogeneity and the light shift. In addition, the long fibers could be pulled out of the spinning solution with a spatula.

Then the spinning solution was transferred into a spinning shaft and molded at room temperature and constant throughput rate of 0.2 ml/min through a die of the extruder with 10 holes with a diameter of 0.005" (127,0 mm) and through an air gap (0.75 cm) in the coagulation bath and cooled to -10aboutWith methanol. Then the fibers were wound on a bobbin with a speed of 6.3 m/min, which gave the stretch factor equal to 4. Then the fibers were washed by impregnation bobbin water during the night to extract the remaining solvent, after which the fiber was dried by air.

Values of strength, elongation and modulus yarn of mixed fibers (having 3 steeps. /inch) were, respectively, 4.1 g/l, 5%, and 100 g/A. the orientation Angle was 18about. Study of fiber cross-section when h using a transmission electron microscope (FACT) PCNA when h using THE showed what phase of the HUNDRED and polyamide are continuous along the length of the fibers.

P R I m m e R 2. The cellulose triacetate (CTA) with acetyl content of 43.7 per cent and the characteristic viscosity of 6.0 DL/g in hexafluoroisopropanol at 30aboutWith and polyacrylonitrile (PAN) was dried in a vacuum oven at 80aboutC. in the nitrogen atmosphere during the night. Inorganic solvent consisting of nitric acid and water in a mass ratio of 87.5/12,5) was mixed in a glass vessel. Then 70 wt. including a mixture of aqueous nitric acid was added to 21 wt. including one HUNDRED and 9 wt. H. PAN in a two-blade mixer with shear effort with a capacity of 500 cm3. The mixer is pre-cooled to -5aboutWith using external of the refrigerator in order to minimize degradation HUNDRED acid. Stirring was begun in the morning and continued until the next day. Sometimes the mixer was opened and spatula scraped off the undissolved polymer that sticks to the walls and the blades of the mixer. The resulting spinning solution contained 30 wt. % polymer (70 wt. % HUNDRED/30 wt. % polyacrylonitrile) 70 wt. % solvent (to 87.5 wt. % nitric acid/12.5 wt. % water). The specified spinning solution showed the homogeneity and the light shift. Fig. 3 and 4, representing fotografia vzaimorezerviruemym. The size of the domains in the isotropic phase was about 100-300 μm. In addition, the long fibers could be pulled out of the spinning solution with a spatula.

Then the spinning solution was transferred into a spinning shaft and molded at room temperature and constant throughput rate of 0.4 ml/min through a die of the extruder with 10 holes with a diameter of 0.005" (27.0 mm) and through an air gap (1 cm) in the coagulation bath with a mixture of ethanol and water (volume ratio of 75/25), cooled to 0aboutC. Then, the fiber was wound on a bobbin with a speed of 12.8 m/min, resulting received the stretch factor equal to 4. Then the fibers were washed by impregnation bobbin water during the night to extract the remaining solvent, after which the fiber was dried by air.

Values of strength, elongation and modulus of the fibers obtained from the mixed spun fibers, were respectively of 6.1 g/d, 6% and 129 g/L. the orientation Angle was 27about. Study of fiber cross-section when h using a transmission electron microscope (FACT) (see Fig. 2) revealed a single HUNDRED domains. The study is a longitudinal cross-section of the fiber obtained by using the FACT showed that the phase of the HUNDRED and polyacrylonitrile are the two shall elocon prototype shown in the table.

1. COMPOSITION FOR FORMING FIBERS, containing 30 - 35 wt. % mixture of a derivative of cellulose, forming the anisotropic phase, with a thermoplastic polymer, forming an isotropic phase in a common solvent, characterized in that, to improve strength characteristics of the fiber, as derived cellulose composition contains a cellulose triacetate with a characteristic viscosity of 6 DL/g in hexafluoroisopropanol at 30oWith the isotropic phase is present in the form of domains with an average size of less than 300 microns, with the following content of components of a mixture, by weight. % ,

The cellulose triacetate with a characteristic viscosity of 6 DL/

g hexafluoroisopropanol at 30o70

Thermoplastic polymer 30

2. The composition according to p. 1, characterized in that thermoplastic polymer it contains polyacrylonitrile or a copolymer diamine, bis-p-aminocyclohexanone, ISO - and terephthalic acid, taken in a molar ratio of 96 : 4 : 70 : 30, respectively, and as a General solvent - aqueous solution of nitric acid or a mixture triftoruksusnoi and formic acids.

 

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