Thread of aromatic polyamide and method of its manufacturing. RU patent 2505628.

IPC classes for russian patent Thread of aromatic polyamide and method of its manufacturing. RU patent 2505628. (RU 2505628):

D01F6/60 - from polyamides (from polyamino acids or polypeptides D01F0006680000)

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Film is featured with para-orentation of at least 95% polymer bonds. The method for film making includes polymerisation of para-oriented aromatic diamine and para-oriented aromatic dicarbon acid haloid in the mixture of solvents consisting of N-methylpyrrolidone or dimethylacetamyde and calcium chloride or lithium with obtaining of aramide polymer containing only para-oriented bounds. Then the spinning solution is obtained by solution of the polymer in solvent mixture up to concentration 2 - 6 wt %. The spinning solution is transformed to para-aramide fibrid film with usual known methods used for meta-aramide fibrids production.

FIELD: textiles, paper.

SUBSTANCE: thread consists entirely of aromatic polyamide. The thread has a high crystallinity (C), large apparent crystal size (ACS) and a reduced amount of defects of the crystal itself.

EFFECT: creation of a thread of aromatic polyamide which has improved physical properties such as strength and modulus.

7 cl, 1 tbl, 2 dwg, 2 ex

AREA OF TECHNICAL USE

The present invention relates to a thread that is composed entirely of aromatic polyamide, and to a method of manufacturing of such threads, and more particularly to a method of making a new thread, completely composed of aromatic polyamide, has physical properties, including high strength and high value of the module.

ANALOGUES AND PROTOTYPE

As disclosed in the known documents, for example, in patents of USA № 3869429 and № 3869430, yarn, consisting entirely of aromatic polyamide, and were using a number of processes including: process preparation of the polymer consists entirely of aromatic polyamide, by the polymerization of aromatic diamine and aromatic chloride in solvent containing N-methyl-2-pyrrolidone; the cooking process of the spinning solution by dissolving prepared polyamide in the solvent of concentrated sulfuric acid; the process of forming elementary threads by extruding the spinning solution through a die and pass spinning material through a layer of a liquid medium, does not cause coagulation, in a tub of coagulant; and the process of cleaning received result of the threads through the execution of washing, drying and heat treatment.

In Fig. 1 schematically depicts a typical way of manufacturing of threads, completely composed of aromatic polyamide, through the use of generally known «dry-wet moulding.

In the normal process is illustrated in figure 1, due to the fact that the spinning material serves the coagulation bath 50, passing through a layer of a fluid medium, does not cause coagulation, and produce coagulation in the tub, superficial part of the spinning material coagulates faster and to a greater extent than its internal part, thus creating the problem consists in the fact that the physical properties of the surface and the inner part of the spinning material are irregular and differ from each other. In accordance with this, in the case of high speed spinning and winding usually happens many breakages of filaments and/or the emergence of , which means you won't increase the speed of the spinning and winding above 600 m/min

Such limitation of speed of the spinning and winding has a detrimental effect on the properties of the finished product, that is, the thread that is composed entirely of aromatic polyamide, so that she may not have the strength and module, which would be above desired levels, and this creates a problem that prevents the performance of its manufacture.

Meanwhile, the Korean laid patent application № 1995-934 offered method of manufacture of fibre, is composed entirely of aromatic polyamide, which are used two spray nozzles in the tub 50 with coagulant; where through one of the nozzles mounted at the top of the bath, spray water or aqueous solution of sulfuric acid on the spinning material, while through another nozzle at the bottom of the bath, sprayed water on the spinning material.

However, in the above-described method does not use the recirculation system for recovery and re-use of coagulant, which leads to increased costs of production and to serious pollution of the environment.

In addition, since this method does not employ the mechanism for controlling the speed of spraying depending on the level of dilution of a sulfuric acid in , the method has a disadvantage, namely that it is impossible to provide a uniform coagulation of surface and internal parts of the spinning material.

In the result of intensive research performed by the author of the invention for the solution of the above-mentioned problems faced during the implementation of the customary method, created the present invention, in which it was proposed to manufacture a new thread that is composed entirely of aromatic polyamide, has the increased durability and higher value of the modulus at low cost and without pollution.

DETAILED DESCRIPTION OF THE INVENTION

TECHNICAL TASK

Thus, the objective of this invention is to increase strength and modulus, the thread that is composed entirely of aromatic polyamide, as the finished product, by ensuring uniform coagulation of surface and internal parts of the spinning material to ensure the possibility of spinning with high speed and without breakages threads.

Another aim of the present invention is the repeated use of coagulant or water that has already been used and restored in the process so as to reduce the cost of manufacturing and reduce environmental pollution.

Another objective of the present invention is to create a thread that is composed entirely of aromatic polyamide, with a significantly improved values of the module and strength, which can withstand the external load due to the structural changes introduced high (designated as «K»), a large visible crystal size (marked as «VRK») and reduced parameter (marked as «g II »), which determine the defects of the crystal, due to uniform coagulation of surface and internal parts of the spinning material.

TECHNICAL MEANS FOR THE SOLUTION OF THE TASK

For solving common problems and achieve the above goals the present invention created a method of manufacturing of threads, completely composed of aromatic polyamide, including: the dissolution of the polymer consists entirely of aromatic polyamide, solvent - concentrated sulfuric acid for the preparation of the spinning solution; skip the spinning solution through a Spinneret with the receipt of the spinning material; and submission of the spinning material through a layer of a fluid medium, does not cause coagulation, reservoir for spraying coagulant, containing coagulant, characterized in that it includes the multi-spray coagulant with consistently concentration of sulphuric acid from stage to stage the spinning material is fed into the tank for spraying.

Additionally thread, fully consisting of aromatic polyamide, according to the present invention differs in that crystallinity () To the heat treatment is in the range from 70% to 79%and the apparent size of the crystal (WRC) (calculated on 200 faces) to heat treatment is within 42Å to 50Å.

The present invention is described in more detail below, with links to enclosed drawings.

According to the present invention, at first prepare a polymer that consists entirely of aromatic polyamide, by the polymerization of aromatic diamine and aromatic chloride in solvent containing N-methyl-2-.

Aromatic diamine preferably contains n-phenylenediamine and aromatic chloride preferably contains .

Besides solvent preferably contains N-methyl-2-pyrrolidone containing dissolved chloride calcium.

Polymer, fully consisting of aromatic polyamide, has the characteristic viscosity constituting not less than 5.0, preferred to increase the strength and modulus threads.

Conditions of polymerization of the above polymer are essentially the same as those previously known, for example, described in U.S. patent № 3869429 or similar document.

In a preferred embodiment, the method of receiving the polymer receive polymer in the form of ultra-fine powder by a solution, which can be obtained by dissolving 1 mole of n-phenylenediamine N-methyl-2- containing about 1 mole of calcium chloride, and 1 mol in the reactor for polymerization of the mixing process in the reactor with the receipt of the polymer in the form of a gel; and stages of crushing, washing and drying of the polymer in the form of a gel, obtaining thus the polymer in the form of ultra-fine powder. can be injected into the reactor half doses in two stages.

Then polymer, fully consisting of aromatic polyamide, prepared as described above, is dissolved in a solvent - concentrated sulfuric acid with the formation of the spinning solution.

Concentrated sulphuric acid, used in the preparation of the spinning solution, preferably has a concentration ranging from 97% to 100% and can be replaced acid or acid.

If the concentration of the sulfuric acid less than 97%, the solubility of polymer decreases, and the solution cannot be easy to form a liquid-crystal structure. Thus, it is difficult to get the spinning solution constant viscosity and, in turn, manage the process of spinning, thus causing the deterioration of mechanical properties of finished textile product.

On the other hand, if the concentration of the sulfuric acid exceeds 100%, the content of the SO 3 becomes excessive in any steaming sulfuric acid containing overly group 3 SO ; therefore, it is undesirable to process and use sulfuric acid as an additive in the spinning solution, as it causes partial decomposition of the polymer. In addition, even if the fiber can be obtained by use of the spinning solution, it has a loose internal structure, essentially matte color, if to speak about appearance, and this decreases the speed of diffusion of a sulfuric acid in solution of coagulant, so that it can lead to the problem, consisting in the reduction of mechanical properties of fibers.

In the alternative case, the concentration of polymer in spinning solution is preferably within 10 wt.% up to 25 wt.%.

However, the concentration of sulfuric acid, and the concentration of polymer in spinning solution is not particularly limited.

At the next stage, as shown in Fig. 2, produce spraying coagulant , where the concentration of the sulfuric acid is consecutively from stage to stage, preferably, two to five stages, the spinning material, received in the result of crossing spinning solution through the die 40. Coagulant is preferably any of the selected solutions from water solutions of sulfuric acid and water. According to a preferred embodiment of the present invention is made a thread by passing spinning material, as shown in figure 2, through the first tank 10 spray coagulant, the second tank 20 for spraying coagulant and third tank 30 spray coagulant to spray coagulants the spinning material through a layer of a fluid medium, does not cause coagulation.

A layer of fluid does not cause coagulation, may be, in General, air layer or a layer of inert gas.

Figure 2 shows a schematic view of illustrating the process of manufacturing of threads, completely composed of aromatic polyamide, when implementing «dry-wet» method of molding according to the present invention.

Depth of the layer of a fluid medium, does not cause coagulation, i.e. the distance from the bottom dies 40 to the surface of the coagulant in the tub 50 with coagulant preferably in the range from 0.1 cm to 15 cm, to improve spinning ability, or to enhance the physical properties of the thread.

From the first to the third reservoirs 10, 20 and 30 for spraying fitted spray nozzles 11, 21 and 31, respectively, for spraying coagulant on the spinning material for moulding.

Each tank 10, 20 and 30 for spraying coagulant preferably contains bottom, inclined enough to be easy to collect and return for reuse sprayed coagulant on the previous stage, and also a perforated bottom for education openings through which pass the spinning material.

Coagulant, sprayed in the tanks of 10, 20 and 30 for spraying coagulant, partially collects in the bottom of the relevant storage tank, and its re-use the preceding steps, while the rest of the coagulant, as well as spinning material flows down, and is preserved in the tub 51 to collect coagulant.

In the first tank 10 spray coagulant sprayed water solution of sulfuric acid with concentration of sulphuric acid from 10% to 20%, the solvent, and with the speed of spraying from 1 m/s to 10 m/sec, through a spray nozzle 11 of the spinning material. After spraying water solution of sulfuric acid is taken from the first tank 10 spray coagulant.

Used the aqueous solution of sulfuric acid is coagulant, which is used in the second tank 20 for spraying coagulant and that of the second tank 20 for spraying coagulant serves the spray nozzle 11 pipeline L1 for the transportation of coagulant.

In the second tank 20 for spraying coagulant sprayed as a coagulant water solution of sulfuric acid with concentration of sulphuric acid, a component from 3% to 10%, and with the speed of spraying from 13 m/s to 20 m/s through a spray nozzle 21 of the spinning material.

After spraying water solution of sulfuric acid contained in the second tank 20 for spraying coagulant, passed in the first tank 10 spray coagulant, equipped with spray nozzle

11, pipeline L1 for the transportation of coagulant and re-use, as described above.

Aqueous solution of sulfuric acid with a concentration of sulphuric acid from 3% to 10%), used in the second tank 20 for spraying coagulant, has a concentration of sulfuric acid, high up 10-20% after spraying, and thus, it can be used as a coagulant in the first tank 10 spray coagulant.

In addition, the water solution of sulfuric acid, sprayed from the second tank 20 for spraying coagulant, is a coagulant used in the third tank 30 spray coagulant passed from the third tank 30 spray coagulant to the spray nozzle 21 pipeline L2 for the transportation of coagulant.

Similarly, in the third tank 30 spray coagulant sprayed as a coagulant water, especially clean water, with the speed of 20 m/s up to 25 m/s through a spray nozzle 31 of the spinning material.

After spraying a coagulant contained in the third tank 30 spray coagulant, pass the second tank 20 for spraying coagulant, equipped with spray nozzle 21 pipeline L2 for the transportation of coagulant, and re-use, as described above.

Water used in the third tank 30 spray coagulant, after spraying has a concentration of sulphuric acid increased up to 3-10%, and thus it can be used as a coagulant in the second tank 20 for spraying coagulant.

Water, especially clean water, sprayed in the third tank 30 spray coagulant, serves the spray nozzle 31 pipeline 32 for water supply.

As a result of the surface and the inner parts of the spinning material is uniform coagulation, and thus provide advantages lies in the fact that according to the present invention, not losing the thread, even in high-speed spinning and yarn to have significantly higher values of the module and strength, and the thread can withstand external load due to structural changes, submitted by the high (To), a large visible crystal size (WRC) and reduced the g option II , which determine defects of the crystal.

After the formation of the thread is subjected to washing, drying and heat treatment with obtaining threads, completely composed of aromatic polyamide.

The speed of the spinning and winding is in the range of 700 m/min up to 1500 m/min

The resulting fully aromatic polyamide, according to the present invention has uniformly surface and internal parts of the spinning material and has a high (To), a large visible crystal size (WRC) and reduced the g option II , which determine defects of the crystal, and thus he has a very high strength before and after heat treatment, amounting to at least 26 g/denier, and a very high value of the module to the heat treatment, constituting not less than 750 g/denier, and after thermal processing, constituting not less than 950 g/denier.

More specifically, thread, fully consisting of aromatic polyamide, according to the present invention has (To) in the range of 70% to 95%; preferably from 76% to 79%; and visible crystal size (WRC) (calculated on 200 faces) to heat processing components within 42Å to 50Å, and more preferably, 47Å to 50Å.

In addition, thread, fully consisting of aromatic polyamide, according to the present invention has the g option II ranging from 1.7% to 1.9% to heat treatment and from 1.3% to 1.6% after heat treatment at 300 C under tension 2% within 2 C.

Besides crystallinity (K) is in the range from 76% to 83%and the apparent size of the crystal (WRC) (calculated on 200 faces) is within 46Å to 55Å, respectively, after heat treatment at 300 C under tension 2% within 2 C.

When and crystallinity (K), and the apparent size of the crystal (WRC) exceed the limits above, strength decreases, while the value of the modulus increases. And, Vice versa, in the case when the crystallinity (K) and The apparent size of the crystal (WRC) is less than the above limits, then slightly increased the value of the module.

Besides, if parameter g II exceeds the limits above, the value of the module is reduced. If this parameter is less than the above limits, while the value of the modulus increases, it is within a region that is difficult is achievable by the present invention.

In accordance with this, in comparison with common thread that is composed entirely of aromatic polyamide thread, fully consisting of aromatic polyamide, according to the present invention, contains surface and inner parts evenly and, thus, reported higher (To), higher value (WRC) and a lower value parameter g II before and after heat treatment, so that it has a high degree of crystallization. As a result of polymer, fully consisting of aromatic polyamide, has a very high strength and significantly improved the value of the modulus.

ADVANTAGES

As described above, this use of the present invention allows uniform coagulation of surface and internal parts of the spinning material, thus providing the opportunity to increase the speed of the spinning and winding without thread breakages.

In accordance with this thread, fully consisting of aromatic polyamide, manufactured according to the present invention, contains surface and inner parts evenly , thus, it has high (To), higher value (WRC) and a lower value parameter g II and less defects crystallization, so that demonstrates the very high strength and significantly improved value of the module.

BRIEF DESCRIPTION OF DRAWINGS

The above purpose, features and advantages of the present invention will become more obvious to a person skilled in the art when reading the following variants of carrying out the invention in conjunction with the accompanying drawings.

Figure 1 schematically illustrates the method of manufacturing of threads, completely composed of aromatic polyamide, by using the famous «dry-wet» method of molding.

Figure 2 schematically illustrates the method of manufacturing of threads, completely composed of aromatic polyamide, by using the «dry-wet» method of molding according to the present invention.

Transcript of rooms positions of the main parts shown on the drawings:

10 - the first tank for spraying of coagulant;

20 - second tank for spraying of coagulant;

80 - a device for thermal processing;

90 - device.

THE BEST WAY OF CARRYING OUT THE INVENTION

Distinctive features of the present invention described above, other benefits you can more fully understand when reading the following, not limiting the scope of the invention, examples and comparative examples. However, it is clear for specialists in this area, that the present invention is not limited to specific content of the examples below.

EXAMPLE 1

1000 kg N-methyl-2- kept at a temperature of 80 C and connected with 80 kg of calcium chloride and 48,67 kg n-phenylenediamine, which then dissolved for preparation of a solution of aromatic diamine.

After the introduction of the solution of aromatic diamine in reactor 20 and molten in a molar dimension equal to the quantity of n-phenylenediamine, simultaneously in the reactor 20, both mixed and compound received poly-n- with the characteristic viscosity of 6.8.

The polymer continuously dissolved in concentrated sulfuric acid (99%) for the formation of an anisotropic optical spinning solution for spinning with the content of polymer 18%.

The resulting spinning solution is passed through the die of 40, as shown in figure 2. After crossing spinning material through the air layer thickness of 7 mm, it was served on the first tank 10 to spray water solution of sulfuric acid with concentration of sulphuric acid 13% and with a speed of 3 m/s at the spinning material. Then the spinning material treated by first spraying was passed through the second tank 20 for spraying coagulant and subjected to a dissipation of other aqueous solution of sulfuric acid with concentration of sulphuric acid, 5% with the speed of spraying 15 m/S. finally, spinning material processed by the second spraying, served in the third tank 30 spray coagulant and subjected spraying of water, especially clean water, with a speed of 23 m/S. as A result of spinning material became the desired thread.

The coagulant used in the third tank 30 spray coagulant, re-used as a coagulant in the second tank 20 for spraying coagulant. Similarly, coagulant, which was used in the second tank 20 for spraying coagulant, re-used as a coagulant in the first tank 10 spray coagulant.

Next, the resulting thread inflicted water sprayed at a temperature of 25 C for washing thread, and then missed a thread through two-stage swivel drying unit with temperature of a surface of rollers 150 C, was reeled dried thread and received as a result of a string of poly-n- to heat processing.

Then the resulting thread subjected to thermal treatment at the temperature of 300 C under tension 2% year 2 with the finished product, i.e. a thread of poly-n- after heat treatment.

Determined the various physical properties of the produced yarn of poly-n- before and after heat treatment, the results are presented in Table 1.

EXAMPLE 2

1000 kg N-methyl-2- kept at a temperature of 80 C and connected with 80 kg of calcium chloride and 48,67 kg n-phenylenediamine, which then dissolved for preparation of a solution of aromatic diamine.

After the introduction of the solution of aromatic diamine in reactor 20 and molten in the molar quantity equal to the number of n-phenylenediamine, simultaneously in the reactor 20, both mixed and compound received poly-n- with the characteristic viscosity of 6.8.

The polymer continuously dissolved in concentrated sulfuric acid (99%) for the formation of an anisotropic optical spinning solution for spinning with the content of polymer 18%.

The resulting spinning solution is passed through the die 40 (as shown in figure 2). After crossing spinning material through the air layer thickness of 7 mm, it was served on the first tank 10 to spray water solution of sulfuric acid with concentration of sulphuric acid 18% and speed of 5 m/s at the spinning material. Then the spinning material treated by first spraying was passed through the second tank 20 for spraying coagulant and subjected to a dissipation of other water solution of sulfuric acid with concentration of sulphuric acid 8% with the speed of spraying 13 m/S. And, finally, spinning material processed by the second spraying, served in the third tank 30 spray coagulant and subjected spraying of water, especially clean water, with a speed of 20 m/S. as A result of spinning material became the desired thread.

Then the resulting thread subjected to thermal treatment at the temperature of 300 C under tension 2% year 2 with the finished product, i.e. a thread of poly-n- after heat treatment.

Determined the various physical properties of the produced yarn of poly-n- before and after heat treatment, the results are presented in Table 1.

A COMPARATIVE EXAMPLE 1

Manufacturing of yarns of poly-n- before and after heat treatment was carried out, using the same procedure and maintaining the same conditions as in Example 1, except that the spinning material passed through tub 50 with coagulant, as shown in figure 1.

Determined the various physical properties of the produced yarn of poly-n- before and after heat treatment, the results are presented in Table 1.

TABLE 1

Evaluation of physical properties of threads

Parameter

Example 1

Example 2

A comparative example 1

Crystallinity (To)

Before thermal processing

77% 78% 74%