Method of producing fibres, threads, films from heterocyclic aromatic polyamidoimides, containing benzimidazole fragments, and fabric based on said threads

FIELD: chemistry.

SUBSTANCE: method involves preparation of two solutions of a mixture of 5(6)-amino-2(para-aminophenyl)benzimidazole with 5(6)-amino-2(para-iminoquinone)benziimide in dimethylacetamide which contains lithium chloride, and then addition of paraphenylenediamine and an equimolar amount of terephthaloyl chloride to the first solution, and to the second solution - an equimolar amount of a dianhydride of pyromellitic acid. Said solutions are mixed at room temperature until formation of a spinning solution with dynamic viscosity of 300-600 P and concentratio of 3.5-4.0 wt %. The solution is filtered, vacuum treated and formed in a water-salt or water-alcohol settling bath, dried and thermally treated in free state. Industrial fireproof ballistic fabric is then produced from the obtained fibres. Threads obtained according to the invention have elementary fibre diametre higher than 10 mcm, rupture resistance not lower than 280 cN/tex and relative elongation of 3.8-4.5%.

EFFECT: invention enables to obtain fibres, threads, films with high elasticity while retaining good strength properties.

2 cl, 3 tbl, 4 ex

 

The invention relates to a technology for obtaining molded products in the form of fibres, filaments or films made of synthetic polymers, in particular of heterocyclic aromatic polyamidoimides containing benzimidazole fragments, and can be used for the production of fabrics for special purposes or composite materials.

1. A method of obtaining the threads of heterocyclic aromatic polyamide, comprising the synthesis of aromatic depolimerizatia based on 5(6)-amino-2-para-aminobenzimidazole, para-phenylenediamine, terephthaloylchloride with the prior dissolution of the diamines, cooling solution to 15-20°C, the addition of first 80-92% of the equimolar ratio terephthaloylchloride, and then after stirring for 30 minutes the introduction of gradually cooling the remaining quantity terephthaloylchloride. The obtained 3,5-5,0%solution after filtration and deaeration is formed in a precipitation of water-dimethylacetamide bath with negative spunbond hood, subjected to orientation stretching, drying and heat treatment under vacuum at 340-360°C (EN 2277139 C1, published. 27.05.2006).

The resulting yarn has a tensile strength of up to 270 g/Tex, ultimate tensile stress in the micro-plastic up to 600 kgf/mm2.

However, in the above analogy, the filament has a tensile strength of not more than 27 g/Tex and elongation in the range of 2.5-3.0%.

2. A method of obtaining heat-resistant polyimide film of polyamidoamine salts based on various dianhydrides aromatic tetracosanoic acids, including pyromellitates of dianhydride, irrigation solution on a substrate immersed in a precipitation bath, drying, and heat treatment (U.S. patent 6716270, published. 06.04.2004).

The polymer from which the film according to the specified method, only contains polyimide group, film intended for the manufacture of the separation membranes.

3. From the patent of the Russian Federation 2352595, publ. 20.04.2009, a method of obtaining a polyimide fibers of the polycondensation solution Polynicotinate. For polycondensation in the environment amide solvent, a mixture of diamines 4,41-diaminodiphenylamine and 5(6)-amino-2-para-aminobenzimidazole and a mixture of dianhydride 3,314,41-benzophenonetetracarboxylic acid dianhydride pyromellitic acid.

At the specified method at the stage of polycondensation of a mixture of 5(6)-amino-2-para-aminobenzimidazole and pyromellitates the dianhydride is injected to prevent studnyvrtane and stabilization technology.

4. Known fabric for the manufacture of ballisticheskih resistant articles made from filaments formed from a spinning solution of aromatic copolymer of a dibasic acid chloride of terephthalic what Islami and diamines benzimidazole and p-phenylenediamine (patent 2337304, published. 27.10.2008).

According to this patent the polymer, from which are made the thread contains only polyamideimide groups, and the filament has a filament diameter of not more than 10 μm.

5. A method of obtaining heat-resistant fibers or films of polyamidimide received high-temperature polycondensation with use of aromatic dicarboxylic acids or mixtures thereof and mixtures of dianhydrides trimellitates and pyromellitates acid (SU 359836 And published. 16.01.1973). These fibers have a strength 45-62 g/Tex and elongation of 5.5 and 11.8%.

According to the mentioned method of obtaining heat-resistant fibers pyromellitic dianhydride injected into the mixture of diisocyanates to increase the solubility of the spinning solution, the filaments have a low strength level 45-62 HS/Tex.

Technical problem on which this invention is directed, is to obtain fibers, filaments or films having high elasticity while maintaining the high strength characteristics, technically safe way.

The goal of the project is achieved by carrying out copolycondensation in amido-salt system on the basis of dimethylacetamide bifunctional reactive compounds a mixture of aromatic diamines and dianhydrides aromatic acids.

As aromatica is such diamines used a mixture of 5(6)-amino-2(para-AMINOPHENYL)benzimidazole (DFBI) 5(6)-amino-2(pair-imengine) bezdikian (AFDI) and p-phenylenediamine (PPD).

As dianhydrides aromatic acids using dichlorohydrin terephthalic acid (DHA) and pyromellitic diandre (KDP).

The polycondensation is carried out in the system cooled to 10°C dimethylacetamide containing lithium chloride to 4 wt.%. The polycondensation process consists of the stages of obtaining the solution of polyamides and solution polyamidation, their mixing.

Obtaining a solution of the polyamide includes sequential dissolution of the mixture of DAHBI and IFDI in the crystalline state in a mass ratio of 55:45-10:90 and after complete dissolution of the mixture adding PPD in the number of 0-0,3 molar fractions relative to the mixture of DFBI+IFDI and adding equimolar amount of DHA relative to the mixture of diamines.

Obtaining solution polyamidation includes sequential dissolution of the mixture of DAHBI and IFDI in the crystalline state in a mass ratio of(55:45)-(10:90) and after complete dissolution of the mixture adding equimolar amount duodenum relative to the mixture of diamines.

Getting the spinning solution spend 5-10 volume fraction of solution Polynicotinate in 90-95 volume fraction of solution of the polyamide at room temperature.

The spinning solution has a concentration of the polymer is 3.5-4.0 wt.% and a viscosity of at least 300 P.

The obtained spinning solution is filtered, obezvozhivani e.g. the keys on spinning in salt-water or water-alcohol bath. The obtained fibers, filaments and films are subjected plastification the hood no more than 20%, washed, dried at a temperature not higher than 120°C and thermoablative in the free state at a temperature not higher than 350°C., the polymer is characterized by the presence of polyamide, polemically, polyimide groups on the basis of benzimidazole.

Obtained according to the invention, the product contains these fragments, identified by the method of infrared polarization spectroscopy on the fluctuations of the characteristic absorption bands (table 1).

No.View radicalConnection typePolarizationFrequency, cm-1
1σ1651
π1600
2π S1773
σaS1723
π1600
3σ3300-3360
Arπ1600
4σ3300-3350
π3200-330
5Arπ1600
6σ Of 3,200-3,300
7π1630
Arπ1600
8π1630
Ar
9π1630
π3600
Arπ1600

Obtained according to the invention the filaments have a filament diameter of over 10 μm, a tensile strength not lower than 280 CN/Tex and elongation in the range of 3.8 to 4.5%.

From the obtained filaments or yarn on the basis of the declared product is made of fabric, high strength, heat resistant and ballistic properties. The invention is illustrated in the examples.

Example 1. 95 g of lithium chloride are dissolved 2.85 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 55:45 in number, 36,18 After complete dissolution the solution add 32,62 g DHA.

To prepare a second solution of 5 g of lithium chloride are dissolved in 0.15 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 55:45 in number 1,90 after complete dissolution the solution add 1,95 g duodenum. The solutions are mixed at room temperature and get spinning solution with a concentration of polymer of 3.85 wt.% and a viscosity of 450 P. After filtration and degassing spend formation through the die plate 200 by a wet method. The obtained filament is pulled to draw the hood -20%, dried at a temperature of 120°C and thermoablative at a temperature of 350°C. Data on the properties of the finished yarn are shown in table 2.

Example 2. 95 g of lithium chloride are dissolved 2.85 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 15:85 in number 26,88, After full is rastvoreniya in solution add PPD in the amount of 10.4 g, then enter 34,34 g DHA. To prepare a second solution of 5 g of lithium chloride are dissolved in 0.15 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 11:89 number of 1.41, After complete dissolution the solution add PPD in the amount of 0.55 g, then give 1.91 g of the duodenum.

The solutions are mixed at room temperature and get spinning solution with a concentration of the polymer 4.0 wt.% and a viscosity of 600 P. After filtration and degassing spend formation through the die plate 200 by a wet method. The obtained filament is pulled to draw the hood - 20%, dried at a temperature of 120°C and thermoablative at a temperature of 350°C. Data on the properties of the finished yarn are shown in table 2.

Example 3. 90 g of lithium chloride are dissolved in 2.7 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 20:80 in number 30,72, After complete dissolution the solution add PPD in the number 6,93 g, then enter 30,91 g DHA. To prepare a second solution of 10 g of lithium chloride are dissolved in 0.3 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 20:80 in number 3,41 after full Rast is orenia in solution add PPD in the amount of 0.37 g, then add 1,93 g WPC.

The solutions are mixed at room temperature and get spinning solution with a concentration of polymer of 3.7 wt.% and viscosity 404 P. After filtration and degassing spend formation through the die plate 200 by a wet method. The obtained filament is pulled to draw the hood -20%, dried at a temperature of 120°C and thermoablative at a temperature of 350°C. Data on the properties of the finished yarn are shown in table 2.

Example 4. 85 g of lithium chloride are dissolved in 2.55 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 25:75 in number 32,30, After complete dissolution the solution add 29,21 g DHA.

To prepare a second solution of 15 g of lithium chloride are dissolved in 0.45 l of dimethylacetamide (DMAA). Received amido-salt solvent is cooled to T=10°C and add the mixture of DAHBI and AFDI at a ratio of 25:75 in the amount of 5.7 after complete dissolution the solution was added 6.0 g of the KDP. The solutions are mixed at room temperature and get solution with the concentration of the polymer in 3.5 wt.% and a viscosity of 300 P. After filtration of conduct forming the film by the dry-wet method. The obtained film stretch hood -30%, dried at a temperature of 120°C and thermoablative at a temperature of 350°C. Data properties the am films are shown in table 2.

Table 2
The ratio of monomer components for polycondensation and properties of the obtained filaments and films
# exampleThe composition of the mixtureElongation at break, %Specific strength thread, CN/Tex
the diaminesdianhydride acids
PPD, mol. shareDAHBI, wt.%AFDI, wt.%DOSA, mol. shareKDP, mol. share
1055450,940,063,95295
20,315850,950,054,1305
30.220800,90,14.5281
4 (film)025750,80,2the 3.8150 mV/mm2

Example 5.From the obtained multifilament yarn with a linear density of 29 Teks with elementary fiber diameter of 14.3 μm on the weaving looms STB-180 produce fabric weave twill 2/2 with density in the warp and weft threads 212 10 cm and weighing 198 g/m2.

Performance fabrics are presented in table 3, indicate that the fabric has high strength, ballistic, fire-retardant properties.

Table 3
Performance fabrics
No.IndexValue
1The breaking load of the fabric strips 50×200 mm, H
on the basis of
- at the ku
5826
6166
2Elongation at break, %
on the basis of
- duck
6,0
4,54
3Tearing load strips of cloth size h mm, N
on the basis of>100
- duck85,3
4Abrasion resistance, cycles
- on cloth>30000
- abrasive1300
5Ballistic resistance of the package V50m/s
-18 layers of fabric537
- 30 layers of fabric606
6Fire is th (the dwell time in the flame 30) No burns, no glow after removal of the flame

1. A method of obtaining a molded product in the form of fibers, filaments, films of heterocyclic aromatic polyamidoimides containing benzimidazole fragments comprising preparing a first solution by dissolving a mixture of 5(6)-amino-2(para-AMINOPHENYL) benzimidazole, 5(6)-amino-2(pair-imengine) bezdikian mass ratio(55:45)-(10:90) cooled to 10°C dimethylacetamide, containing up to 4 wt.% lithium chloride, the addition first, 0-0,3 mol. share paraphenylenediamine in relation to the above-mentioned mixture, and then equimolar amount of dichlorohydrin terephthalic acid, preparing a second solution by dissolving a mixture of 5(6)-amino-2(para-AMINOPHENYL) benzimidazole, 5(6)-amino-2(pair-imengine) bezdikian mass ratio(55:45)-(10:90) cooled to 10°C dimethylacetamide, containing up to 4 wt.% lithium chloride, the addition of equimolar amount of dianhydride pyromellitic acid, a mixture of 90 to 95 volume fraction of the first solution with 5-10 volume fractions of the second solution at room temperature before the formation of the spinning solution with a dynamic viscosity of 300-600 CPS and a concentration of 3.5 to 4.0 wt.%, filtering the obtained spinning solution, degassing, molding in salt-water or water-alcohol Sagitullin the th tub, drying at a temperature not higher than 120°C. and the heat treatment in the free state at a temperature not higher than 350°C.

2. Technical fire resistant ballistic fabric made of filaments and/or yarns of heterocyclic aromatic polyamidoimides containing benzimidazole fragments obtained by the method according to claim 1.



 

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