RU2723118C2 - Method and equipment for production of conductive fibers and filaments - Google Patents

Abstract

FIELD: production of composite materials.SUBSTANCE: invention relates to production of conductive fibers and elementary threads from natural or polymer fibers in form of fibrous composite material for use in textile industry and construction. Method includes a stage of knitted fabric manufacturing by means of a knitting machine, which is then subjected to preliminary activation. Further, the tissue is treated in a sonochemical reactor, where nanoparticles are applied to the tissue surface using an ultrasonic homogenizer. Fabric is dried and prevents connection of contact points in fabric by vibration system. Then follows the chemical metallisation of the fabric with the neutralization sequence, chemical activation, chemical metallisation, oxidation-reduction reaction and chemical neutralization. In Conclusion of conductive knitted fabric of drawn wrinkled knitting yarn, it is heated, calibrated and wound on a spool as the finished product.EFFECT: higher softness and flexibility of thread, which leads to greater versatility in use.8 cl, 6 dwg

Description

FIELD OF THE INVENTION

Method and corresponding equipment for the manufacture of conductive fibers and filaments of natural or polymer fibers in the form of a fibrous composite material for use in the textile industry and construction.

State of the art

The manufacture of conductive polymer fibers by incorporation or layering of carbon has long been known in the art. Thus, for example, DE 698 30 847 T2 describes, inter alia, a method for creating a macroscopic molecular structure from thin tube carbon molecules, the method comprising the following process steps: at least about 10 ⁶ thin tube carbon molecules, mainly of the same length from 50 to 500 nm, combined by means of a device for interfacing with a substrate coated with a material. The substrate consists of gold, mercury, and indium and tin oxide.

DE 11 2013 005 811 T5 describes a method for manufacturing fibers coated with carbon nanostructures. In this method, two-dimensional structures are given increased electrical conductivity. The electrically conductive structures include a substrate of a plurality of fibers with a predetermined interfiber aperture and a plurality of carbon nanostructures, respectively, covering the fibers, at least partially with the formation of bridges perpendicular to the specified apertures between adjacent fibers to create a continuous carbon nanostructure.

In all of these solutions, modified polymers are used as the substrate. Natural fibers do not use.

Disclosure of invention

The objective of the invention is to propose a method and appropriate equipment for implementing the method of manufacturing conductive fibers and filaments of natural or polymer fibers in the form of a fibrous composite material. The equipment of this invention and the associated method provide the possibility of manufacturing both natural and polymer fibers of a conductive material used as a basis for a conductive fabric.

Compared to the material of copper conductors, the fibrous material according to this invention has significantly higher softness and flexibility and, therefore, greater versatility in use.

The proposed equipment includes the following main nodes with the possibility of their addition to other nodes to optimize the method according to this invention. A knitting machine for the manufacture of knitted fabric from natural or polymer fiber, a sonochemical reactor with main units, an ultrasonic homogenizer, an ultrasonic transducer with a flat emitter, a magnetron, a flat emitter and a drying chamber with a vibration system, several series-installed bathtubs for chemical and galvanic metallization, connected to a common bath, an autoclave for processing fibers, a drum for ultrasonic heating and calibration of fibers after separating fibers from a fabric and a coil for winding finished and processed fibers or threads, as well as a control system for all parts of the equipment, in particular, to give the necessary electrical parameters for knitted fabric.

The method according to this invention includes the following process steps: the manufacture of knitted fabric, which is then subjected to a pre-activation bath, degreasing with an alkaline solution or an acid solution, depending on the material of the fibers; then the fabric is pulled through tension pulleys in a sonochemical reactor through a colloidal solution or suspension, the suspension being made by an ultrasonic homogenizer and continuously pumped into a sonochemical reactor and piped back into an ultrasonic homogenizer, and in an ultrasonic homogenizer, the fabric is subjected to ultrasound over the entire width and through vibrations are applied to the surface of the tissue nanoparticles, which are then fixed by a magnetron in and on the fibers of the fabric; after the ultrasonic homogenizer, the fabric is passed through the drying chamber, and it is preferably dried by the inductive method, in which the vibration system further prevents the contact points of the fabric from connecting; then follows chemical metallization with a sequence of neutralization, activation, chemical metallization, redox reaction, chemical neutralization, moreover, the fabric passes through the tension rollers through, from and to individual sections under the influence of a vibrosystem; then follows the galvanic metallization of the fabric with immersion in the electrolyte, followed by galvanic neutralization. The fabric is carried along the tension rollers through absorbent coated drums and a vibration system, acting simultaneously as cathodes in the galvanized metallization zone. The fabric thread is then pulled out of the fabric, heated and calibrated in a drum and wound on spools as a final product. All technological steps, in particular the creation of electrical parameters, are monitored and continuously regulated by means of control and regulation elements.

Brief Description of the Drawings

An embodiment of the invention with a method and corresponding parts of the equipment is disclosed in more detail by the example of the drawings, which depict:

Figure 1 is a sequence diagram of the technological stages of the manufacture of conductive fibers and filaments,

- a sequence diagram of the technological stages of thermal stabilization and calibration of fibers and filaments;

Figure 2 image of tissue in a bound state;

Figure 3 diagram of a sonochemical reactor with an ultrasonic homogenizer, an ultrasonic transducer with a flat emitter, a magnetron and a drying chamber with a vibrosystem;

4 is a diagram of a galvanic metallization of a fabric with a total of seven sites (neutralization, activation, chemical metallization, redox reaction, neutralization, electrolyte bath, neutralization) and

FIG. 5 is a sequence diagram of the final technological steps — pulling the thread from the fabric, calibrating and heat stabilizing the thread, winding the finished thread onto a spool.

The method is described below in conjunction with the necessary parts of the equipment.

The implementation of the invention

The method is based on the production of knitted fabric 1 or woven strips. To this end, using knitting machine 38, natural and polymer fibers are processed to produce knitted fabric 1 or woven strips. The fabric 1 in the bath 39 is subjected to preliminary activation, degreasing with an alkaline solution or an acid solution. Appropriate solutions are used depending on the type of fiber material.

Then the fabric 1 through the tension rollers is pulled through the bath 17 of the sonochemical reactor (Figure 3) through the colloidal solution 5 or suspension. The suspension is made in an ultrasonic homogenizer 2, 3, 4 and continuously pumped into the bath 17 of the sonochemical reactor. Ultrasonic homogenizer 2, 3, 4 consists of a tank 4 for a colloidal solution, an ultrasonic generator 2 and an ultrasonic transducer 3. A tank 4 for a colloidal solution has a branch to the filtration system 6 with a filter and a pump and an input to the cooling system 15. The ultrasonic generator operates in the range from 1000 to 2000 W and 20 kHz. A colloidal solution contains various nanoparticles of substances selected depending on the required properties of the finished yarns, for example silver, carbon, copper, nickel or other metals. The sizes of nanoparticles are up to 200 nm. The concentration of nanoparticles is up to 70 g / l.

The colloidal solution 5 made in the ultrasonic homogenizer 2, 3, 4 is pumped through the filter of the filtration system 6 to a sonochemical reactor. The solution 5 circulates in the common system through a pipe 10 connected to the cooling system 15 with a control valve 9. The temperature of the solution 5 is measured in a sonochemical reactor and in an ultrasonic homogenizer 2, 3, 4 and adjusted using the cooling system 15 to an appropriate preset temperature. The cooling system 15 operates on the basis of semiconductor thermocouples (Peltier elements).

In the bath 17, the fabric 1 is subjected to ultrasound from the ultrasonic transducer 13 by means of plane-emitters 14 over the entire width of the fabric, and due to this, nanoparticles are applied to the surface of the fabric 1 by cavitation and vibration in the range from 100 to 500 W. In conclusion, the fabric 1 is pulled through the magnetron 8. The magnetron 8 operates with an installed power of up to 900 watts and fixes nanoparticles in the fibers of fabric 1.

At the end of the bath 17, the fabric 1 passes through the vibrating system 16, and outside the bath 17 the fabric 1 is passed through the drying chamber 12, and drying is carried out, preferably by induction, and the additional vibrating system 16 prevents the contact points of the fabric 1 through its vibration. As final technological steps 4, chemical metallization 40 of fabric 1 in a common bath 18 is followed with a sequence of neutralization / purification of, for example, polyester material in a weak solution of hydrochloric acid with intensive circulation in bath 22 as section I, chemical activation of, for example, polyester material with immersion in a solution of palladium chloride (PdCl2) and tin chloride (SnCl4) with intensive circulation in bath 23 as section II, chemical metallization and chemical promotion, for example, with AgNO3 in absorbent-coated drums and vibration in bath 24 as section III, oxidatively reduction reaction in bath 25 as a part IV, chemical neutralization in the bath 26 as section V, the fabric 1 being tensioned by rollers 7, some of which are located inside the bathtubs, and some are located from the bathtub to the bath, pass through, from and into the baths 22, 23, 24, 25, 26, and in the baths 24, 25, the fabric 1 is exposed to an additional three or four drums (19) with an absorbent coating and a vibration system.

In conclusion, galvanic metallization of fabric 40 by electrolyte 1 in bath 27 as section VI followed by galvanic neutralization in bath 28 as section VII follows. Here, the fabric 1 is also passed through the tension rollers 7 through the drums 20 with an absorbent coating and a vibration system, while the drums simultaneously serve as a cathode in the galvanic metallization area and anode 21 (in section VI). The fabric 1 leaves section VII as a conductive knitted fabric 30. If necessary, rinsing with distilled water is carried out before each technological step of the chemical treatment.

There is also the possibility of chemical deposition of an additional metal layer. To do this, use an additional bath with a solution of potassium oxide, potassium hydroxide with the addition of ethylene diamine, oxalic acid, lactic acid and silver oxide. Finally, wrinkled yarn 31 is drawn from conductive knitted fabric 30, heated and calibrated in reels 32, and then wound as a final product onto spool 34. Spool 34 is designed to wind finished processed yarns / filament yarns thereon. Calibration in the drum 32 is possible simultaneously through several parallel grooves.

All technological steps and, in particular, the formation of electrical parameters are controlled and regulated by the control system 36 and the adjustment system 36.

Legend List

1 - knitted fabric, knitted woven stripes

2 - ultrasonic generator

3 - ultrasonic transducer

4 - capacity for colloidal solution

2 to 4 - ultrasonic homogenizer

5 - colloidal solution, suspension

6 - filtration system (filter and pump)

7 - idler rollers, guide rollers

8 - magnetron

9 - valve

10 - pipeline

11 - semiconductor thermocouple (Peltier element)

12 - drying chamber

13 - ultrasonic transducer with a flat emitter

14 - flat emitter

15 - cooling system

16 - vibration system

17 - bath sonochemical reactor

18 - bath with separation of chemical metallization and galvanic metallization

19 - drums with absorbent coating and vibration in the zone of chemical metallization

20 - drums with absorbent coating and vibration as cathodes in the area of galvanic metallization

21 - anode

22 - section I, bath chemical neutralization

23 - section II, chemical activation bath

24 - section III, chemical metallization bath

25 - plot IV, bath redox reaction

26 - plot V, bath chemical neutralization

27 - section VI, bath with electrolyte

28 - plot VII, galvanic neutralization bath

29 - liquid surface

30 - conductive, knitted fabric

31 - unwound, woven thread or wrinkled fiber

32 - drum ultrasonic heating and calibration

33 - thread or calibrated and non-wrinkled fibers

34 - reel for winding finished processed threads / filament yarn

35 - tension rollers

36 - control system for the electrical parameters of knitted fabric

37 - autoclave

38 - knitting machine

39 - pre-activation bath

40 - chemical and galvanic metallization.

Claims (39)

1. A method of manufacturing conductive fibers and filaments of natural or polymer fibers in the form of a fibrous composite material, characterized by the following process steps: - manufacturing by means of a knitting machine (38) of knitted fabric (1) from natural or polymer fibers, which is then subjected to preliminary activation in a bath (39), degreasing with an alkaline solution or an acid solution depending on the material of the fibers; - then the fabric (1) is pulled through the tension rollers (7) through the bath (17) of the sonochemical reactor through a colloidal solution (5) or suspension, the suspension being made in an ultrasonic homogenizer (2, 3, 4) and continuously pumped into the bath (17) and again, through the pipe (10), they are led back to the ultrasonic homogenizer (2, 3, 4), and in the bath (17) the fabric (1) is subjected to ultrasound over the entire width and, through cavitation and vibration, nanoparticles are applied to the surface of the fabric (1), which then fix the magnetron (8) in and on the fibers of the fabric (1); - after the bath (17), the fabric (1) is passed through the drying chamber (12), and it is dried, preferably by the inductive method, in which the vibration system (16) further prevents the contact points of the fabric (1) from being connected; - followed by chemical metallization of the tissue (1) with the sequence of neutralization in the bath (22), chemical activation in the bath (23), chemical metallization in the bath (24), redox reaction in the bath (25), chemical neutralization in the bath (26) ), and the fabric (1) along the tension rollers (7) passes through, from and to the bathtubs (22, 23, 24, 25, 26), and in the bathtubs (24, 25), the absorbent drums additionally act on the fabric (1) coating and vibration system (19) and then follows the galvanic metallization of the fabric (1) with immersion in the electrolyte in the bath (27) followed by galvanic neutralization in the bath (28) with the fabric (1) passing the tension rollers (7) through the drums (20) with absorbent coating and vibration system, which act simultaneously as cathodes in the galvanized metallization zone; - finally, from the conductive knitted fabric (30), the wrinkled knitting thread (31) is pulled, heated and calibrated in drums (32) and wound on a spool (34) as the final product, and all technological steps, in particular the creation of electrical parameters, are controlled and are regulated by a control and regulation system (36). 2. A method of manufacturing a conductive fiber according to claim 1, characterized in that the colloidal solution (5) made in the ultrasonic homogenizer (2, 3, 4) is pumped through the filter of the filtration system (6) to a sonochemical reactor, while the colloidal solution (5) is circulated in the cooling pipe (10) and cooling system (15) back to the ultrasonic homogenizer (2, 3, 4), moreover, the temperature of the colloidal solution (5) is measured in a sonochemical reactor and in an ultrasonic homogenizer (2, 3, 4) and adjusted using the cooling system (15) to the corresponding preset temperature. 3. A method of manufacturing a conductive fiber according to claim 1, characterized in that The magnetron (8) operates with an installed power of up to 900 watts. 4. A method of manufacturing a conductive fiber according to claim 1, characterized in that calibration in the drum (32) is carried out simultaneously in several parallel grooves. 5. Equipment for the manufacture of conductive fibers and filaments for implementing the method according to any one of paragraphs. 1–4, characterized in that the set of equipment includes - a knitting machine (38) for the manufacture of knitted fabric (1) from natural or polymer fibers, - a pre-activation bath for tissue degreasing (1), a sonochemical reactor bath (17) with the main components: an ultrasonic homogenizer (2, 3, 4), an ultrasonic transducer with a flat emitter (13), a magnetron (8), a flat emitter (14) and a drying chamber (12) with a vibrosystem (16), - several baths (22, 23, 24, 25, 26) of chemical metallization and baths (27, 28) of galvanic metallization, combined into a common bath (18), - an autoclave (37) for processing fibers, a drum (32) for ultrasonic heating and calibration of fibers after they are pulled from conductive knitted fabric (30) and a coil (34) for winding finished processed threads or filament yarns, as well as a system (36) for controlling all parts of equipment, in particular, to ensure the specified electrical parameters of knitted fabric (30). 6. Equipment according to claim 5, characterized in that The ultrasonic homogenizer (2, 3, 4) consists of a container (4) for a colloidal solution with a branch to the filtration system (6) with a filter and a pump and an entrance to the cooling system (15), and an ultrasonic one is installed in the container (4) for the colloidal solution a generator (2) and an ultrasonic transducer, the ultrasonic transducer being precisely tuned and operating with a power of 100 to 500 W with a frequency of up to 40 kHz. 7. Equipment according to claim 5 or 6, characterized in that bathtubs (22, 23, 24, 25, 26) of chemical metallization, including: section I - bath (22) chemical neutralization, section II - bath (23) chemical activation, section III - bath (24) chemical metallization and promotion, section IV - bath (25) of the redox reaction, section V - bath (26) chemical neutralization, equipped with tension rollers (7), some of which are located inside the bathtubs (22, 23, 24, 25, 26), and some are located from the bath to the bath, and are equipped with three or four drums, respectively, in section III and section IV (19) with absorbent coating and vibration system. 8. Equipment according to any one of paragraphs. 5-7, characterized in that baths (27, 28) of galvanic metallization consist of: section VI - bath (27) of an electrolyte with a cathode (20) and anode (21), and Section VII - galvanic neutralization bath (28) with tension rollers (7) inside the bathtubs (27, 28) and drums (20) with an absorbent coating and a vibration system, which simultaneously serve as a cathode in the galvanic metallization section and an anode (21) in section VI.

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