Method for preparing polyvinylidenefluoride thread with carbine cover

FIELD: polymers.

SUBSTANCE: invention relates to technology for preparing and modification of chemical fibers and threads, in particular, to polyvinylidene fluoride (PVDF) fibers and threads. Method for preparing thread with carbine cover involves preliminary impregnation of PVDF thread of diameter 0.07-0.90 mm with dimethylformamide or dimethylsulfoxide for 1-4 h and the following treatment with 15-17% potassium hydroxide solution in n-butanol or n-propanol medium at temperature 60-80°C. Optimal treatment time is 0.5-4 h. Invention provides simplifying technology in preparing PVDF thread with carbine cover of different diameter and possessing higher physical-mechanical indices, among them, unit strength based on simultaneous elimination of highly toxic and highly inflammable substances, using a single-component highly boiling solvent, decreasing the potassium hydroxide concentration and elimination the ultrasonic field using. Invention can be used chemical industry, in particular, in manufacturing filtering and fettling materials and in medicine as suture biocompatible surgery threads showing the enhanced resistance to thrombosis.

EFFECT: improved preparing method, enhanced and valuable properties of cover.

2 cl, 1 tbl, 41 ex

 

The invention relates to the technology for production and modification of chemical fibers and filaments, in particular PVDF, and can be used in the chemical industry: in the manufacture of filtration and lining materials in medicine: as a biocompatible suture sutures with high thromboresistance.

A method of obtaining thromboresistance suture material (journal proceedings of the Academy of Sciences, series of chemical, 1993, No. 3, S. 452), which lies in the fact that the poly (vinylidene fluoride) with the aim of obtaining kurbinovo coverage is affected by a mixture of saturated solution of potassium hydroxide in ethanol with acetone in the ratio 10:90. The main disadvantage of this method is that the suture material received by him, has insufficient thromboresistance and biocompatible properties due to the presence on the surface of 7% fluorine. In addition, regeneration of the solvent is difficult because of bicomponent composition, as well as both components are flammable substances (flammable liquids), which increases the Flammability of the production.

The closest technical solution is the method of obtaining karunadasa PVDF (PVDF) thread (patent RF №02115438 published 20.07.1998 year). The invention relates to a method of obtaining material, the possession is the future thromboresistance and biocompatible properties, which can be used in General and vascular surgery, such as suture material or implant. How is that polyvinylidenechloride fiber is treated with a saturated solution of potassium hydroxide in a mixture of methyl alcohol and acetone in their mass ratio 10:90 at a temperature of 18-20°for 20-50 min with simultaneous influence of ultrasonic field. The main disadvantage of this method is that the resulting fiber from carbin has a bursting strength of 35 g/Tex (0,343 N/Tex or 603 MPa) when the thread diameter of 0.05 mm and, respectively, lower strength in the node (Ekonomski, Gverment "Chemical fibres ed. "Light industry". M., 1966, s), insufficient for use threads in industrial goods and surgical suture material (requirements of the European Pharmacopoeia (EP)). The disadvantage of this method is the need of the use of methyl alcohol, referred to particularly dangerous toxic substances, and acetone, both components are flammable substances (flammable liquids), at the same time, the use of bicomponent solvent makes its regeneration. In addition, the method requires additional equipment - ultrasonic generator, which makes the production even more harmful because of mostasteless as the staff, and on the strength characteristics of the fibers in the direction of their deterioration.

The technical problem to be solved by the present invention is directed, is to simplify the technology for PVDF thread with karbinovym coating of different diameters, with a higher physical and mechanical properties, including strength in the node, due to the simultaneous exclusion of highly toxic and flammable substances, the use of one high-boiling solvent, reduce the concentration of potassium hydroxide and exclude the application of ultrasonic fields.

The technical problem is solved due to the fact that the inventive method of obtaining thread with karbinovym coating includes a preliminary impregnation PVDF threads with a diameter of 0.07-0.90mm dimethylformamide (DMF) or dimethylsulfoxide (DMSO) for 1-4 h and subsequent processing 15-17% solution of potassium hydroxide in n-butanol or n-propanol at 60-80°C with the formation of the surface of the carbin. The optimal processing time is 0.5-4 hours

According to the claimed technical solution is the use of pre-swelling fibers (DMF) or (DMSO) and subsequent treatment with a solution of potassium hydroxide in n-butanol or n-propanol eliminates toxic substances from the production, to exclude ultrasound, reduce the shape of the concentration of potassium hydroxide and to use one-component solvent, that allows you to save thromboresistance and biocompatible properties with increase in strength in the node, to facilitate regeneration of the solvent, which will lead to lower material costs and reduced environmental burden on the environment.

The invention is implemented as follows.

Examples. PVDF monofilament bursting strength 630-649 MPa and strength in the node 603-647 MPa 0.07 to about 0.90 mm and a length of 20 meters placed in 30 ml of DMF or DMSO and incubated for 1-4 h, then the thread is immersed in 15-17% solution of potassium hydroxide in n-butanol or n-propanol at a temperature of 60-80°s With a duration of 0.5 to 4 hours After this monofilament washed from potassium hydroxide to a pH of 7.3. The properties of the yarn depending on the parameters of the method are presented in the table.

The advantage of the present invention in comparison with the prototype is that getting carbin is carried out in a single solvent is n-butanol or n-propanol, which facilitates the regeneration of the solvent, thereby reducing the cost of products. In addition, the concentration of potassium hydroxide (15-17%) lower than in the prototype, this leads to reduced demands on the corrosion resistance of the equipment. Also the decrease in the concentration of potassium hydroxide can get, for example, surgical products with higher performance is prochnosti, namely 630-649 MPa against 603 MPa (in the prototype, the strength 35 g/Tex, which corresponds to the above) prototype indicators adhesion of platelets is significantly lower, i.e. the material has a high thromboresistance. The higher strength allows the use of surgical suture thread of smaller diameter, which reduces the body's reaction to a foreign body and, consequently, the risk of negative consequences of surgical intervention. High strength properties of filaments of poly (vinylidene fluoride) by the present method is achieved by forming on their surface kurbinovo coverage in the complete absence of fluorine in the layer carbin, which is achieved due to the greater length and in more mild conditions of the process. It should also be noted that adhesion is a surface phenomenon (Chemical encyclopedia, vol. 1, publishing house "Soviet encyclopedia". M., 1988, p.54) and, accordingly, the degree of transformation of the whole of poly (vinylidene fluoride), in addition to the surface layer of the thread, carbin has little effect on the adhesion interaction between the surface of the fibers with the environment, in this case with platelets. In addition, kurbinovo PVDF coating on the threads allows its use in the manufacture of filters of different patterns - fabrics, knitted fabrics and other - (example 40 and 41 in table).

From the data given in the table, it is seen that in the whole range of proposed options (examples 1-38) process, the strength of the filament is higher than that of the prototype. The increased duration of the swelling of the fibres leads to decrease in strength as in the case of the use of dimethylformamide, and dimethyl sulfoxide (example 5, 14, 23 and 32) to values close to the values of the prototype. And with the reduction of the time of swelling of less than 1 h, the rate of adhesion of platelets is higher than that of the prototype (examples 4, 13, 31). The range of the claimed temperature is justified by the fact that the lower limit is determined by the solubility of potassium hydroxide sufficient to obtain kurbinovo cover, allowing to obtain an indication of the adhesion of platelets below the level of the prototype, and the upper limit is determined by the resistance kurbinovo coverage and strength characteristics of the yarns (examples 7, 16, 25 and 34). The processing time of less than 0.5 h leads to the results in the adhesion of platelets at the level of the prototype (examples 8,17, 26 and 35), and the increase in time over 4 hours reduces the strength up to values of the prototype (examples 11, 20, 29 and 38). The concentration range is determined by the solubility of potassium hydroxide in n-butanol and the-propanol when the claimed temperature treatment, providing properties of the obtained surgical materials in terms of adhesion of platelets is lower than that of the prototype (examples. 9, 10, 18, 19, 27, 28, 36 and 37), which is characterized by increased thromboresistant obtained materials.

Education coverage of carbin on the surface of the filaments allows to obtain more effective filter cloth for filtration of aggressive acidic gases by reducing the resistivity of the material, which reduces the static charge on the filter surface and, accordingly, accumulation of dust particles (example 39 and 40).

1. The method of obtaining PVDF thread with karbinovym coating processing of the original thread potassium hydroxide solution in an organic solvent, characterized in that original thread diameter from 0.07 to 0.90 mm previously subjected to impregnation in dimethylformamide or dimethyl sulfoxide within 1-4 h, then treated 15-17%solution of potassium hydroxide in n-butyl or n-propyl alcohol at 60-80°C.

2. The method according to claim 1, characterized in that the processing of 15-17%potassium hydroxide solution is conducted for 0.5 to 4.0 hours



 

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