The way bezelektrodnogo application of metallic coating on the surface of the aromatic polyamide and the product of aromatic polyamide with metal coating

 

(57) Abstract:

Usage: betalactamase the metal coating on the surface of the aromatic polyamide. Essence: as a product using the composition, comprising from 70 to 98 wt.% aromatic polyamide and 2-30 wt.% polyvinylpyrrolidone, in the coating process, the surface of the product with an aqueous solution containing the activating cations tin, washing the surface, immersing the washed surface in an aqueous solution containing cations of the applied metal additive reductant and the formation of the coating. 2 C. and 10 C.p. f-crystals, 4 PL.

The invention relates to a method of Bezeichnung of applying metal coating to the surface of the aromatic polyamide in which the metal is strongly linked with the base of the aromatic polyamide and forms vysokotempovaya surface. Aromatic polyamide includes a small amount of polyvinylpyrrolidone as an additional polymer that improves the quality of the coating, adhesion and consequently the conductivity of the metal coating.

Betalactaminam metal coating is osisnie the metal coating is generally well known. One of the challenges to successfully achieve bezelektrodnogo of applying metal coating consisted in obtaining good adhesion between the substrate and the metal coating. Although for some applications and for some products it is quite sufficient can be a simple sealing, good adhesion of the metal coating is essential for those threads, since the metal coating must withstand the force impact of the additional processing.

Known method of applying a metallic coating on the surface of articles made of polymer, in which the metal cations electrostatically associated with the polymer in a nonaqueous system and thereby restored to the metal (international application WO 90/00634 from 25.02.90).

However, the known method required the use of nonaqueous solutions for the application of the metallic coating and electrostatic attraction for the binding of cations to obtain semiconductor materials that did not give a durable metal coating with high strength and modulus.

The technical result of the invention is to provide a method electrodeless deposition of the metal coating on the surface of the aromatic polinaut strength, the module and the electrical conductivity.

This technical result is achieved in that in the method bezelektrodnogo application of metallic coating on the surface of the aromatic polyamide as a product of the aromatic polyamide used a product made from a composition comprising from 70 to 98 wt.% aromatic polyamide and optionally from 2 to 30 wt.% polyvinylpyrrolidone, in the coating by the following stages:

the surface treatment of the product with an aqueous solution containing the activating cations tin;

washing the surface to remove unreacted activating cations tin;

immersing the washed surface in an aqueous solution containing cations of deposited metal, the additive of the reducing agent in an aqueous solution containing cations of deposited metal for recovery of metal cations and the formation of the coating.

The product of the aromatic polyamide may be a link.

In addition, the metal forming the coating may be selected from the group consisting of silver, copper and Nickel, and a reducing agent may be formaldehyde, and the process can be carried out in the presence of ammonium hydroxide, awlays the t 10000 to 40000.

As the aromatic polyamide can be used aromatic poly-para-amide or poly-para-phenyleneterephthalamide.

The technical result is also achieved due to the fact that the product of the aromatic polyamide coated with a metal coating made of a material containing 70-87% wt. aromatic polyamide and additionally 2-30 wt.% polyvinylpyrrolidone.

The product may be in the form of threads.

The metal coating may be selected from the group comprising silver, copper and Nickel, and aromatic polyamide may be poly-para-phenyleneterephthalamide.

Long ago there appeared a necessity of conducting aramid threads, which would have a durable metal coating, and the need is particularly acute for threads, which have high strength and modulus.

Yarn of aramides, in particular para-aramids, hard covered with a firmly adhering metal coating. Processing and pre-treatment of the surface of aramid threads essentially did not give satisfactory results.

The invention provides a method bezelektrodnogo covering yarn of aramides to get covered IU ravidasis and firmly adhering.

Used in the invention threads include the additional amount of polyvinylpyrrolidone (RUHR), distributed throughout the structure of the thread. There is reason to believe that the presence of the RUHR contributes in some way to create places for the bonding of the metal in the process bezelektrodnogo cover the threads. The reason for the improved adhesion is not fully understood.

Under the "aramid" is meant a polyamide in which at least 85% of the amide linkages(-CO-NH) are attached directly to two aromatic nuclei. Appropriate aramid yarn described in Mah-Made Fiber-Science and Technology, Vol. 2, Section "Fiber-Forming Aromatic Polyamids", p.297, W. Black et al., Inferscience Publishers, 1968. Aramid yarn is also described in U.S. patent 4172938; 3869429; 3819587; 3673143; 3354127 and 3094511.

With aramid you can use supplements, and how it was established, with aramid can connect up to 10 wt.% another polymeric material or can be used copolymers with up to 10 percent of other diamine instead of the diamine of the aramid or as much as 10% other twohorned instead of twohorned or aramid.

Para-aramids are the primary polymer in the filaments of this invention and poly/p-phenyleneterephthalamide (ECD-T) is the preferred para-aramid. Under ECD-T implies e copolymers, obtained by mixing small amounts of other diamines with p-phenylenediamine and small amounts of douglashamilton with terephthaloyl-chloride. In General, other diamines and other dualranger can be used in quantities of up to 10 mol. % p-phenylenediamine or terephthaloylchloride or even a few more, referring only to other diamines and dualranger had no reactive groups which would interfere in the polymerization reaction. ECD-T means also copolymers obtained by mixing other aromatic diamines and other aromatic douglashamilton, such as 2,6-Naftali-chloride or chloro - or dichlorotetrafluoroethane, taking into account the fact that other aromatic diamines and aromatic dualranger were present in quantities which would ensure obtaining anisotropic spinning additives. Receiving PEG-T is described in U.S. patent N 3869429; 4308374 and 4698414.

The RUHR is additive polymer in the filaments of this invention. Under the RUHR is meant a polymer that is obtained in the linear polymerization monomer units of N-vinyl-2-pyrrolidone with or without the inclusion of small amounts of copolymeres that can prisutstvie.

It was found that the RUHR almost any molecular weight can be used in the practice of the invention. You can use the RUHR with a molecular weight in the range from 5000 up to 500000, and they all, to some extent, will contribute to the realization of the invention. The RUHR with a molecular weight of from 10000 to 40000 is the preferred, and most preferred is the RUHR molecular weight 10000-24000. The RUHR with a molecular weight of less than 5000 unfit for reception of a strong connection with the para-aramid RUHR combination and easily pulled from the thread. The RUHR with a molecular weight of above 100000 causes an increase in demand for the metal in the case of a minimum level of conductivity. The reason for this increase in demand for the metal is not installed.

Used in the invention, the yarn can be spun by the way, according to the European patent N 401740 from 12.12.1990, which mix anisotropic mixture of acid solvent, para-aramid in the RUHR is heated and extruded through a spinning device in the/through the coagulating layer and/and through the water coagulating bath. The elements of this method using only PEG-T is described in U.S. patent N 3767756 from 23.10.1973. Used in this thread invention can be used to ateneu threads regulated or changed depending on the number of the RUHR, which is included in the thread. As mentioned, the RUHR can be present in amounts of from 2 to 30 weight. % based on the weight ECD-So the Lower limit is the limit of feasibility, although the advantages of the invention are achieved with any concentration of the RUHR, and these benefits are difficult to measure at concentrations of less than 2 wt.%.

The upper limit is the concentration at which begins the destruction of certain qualities due to the presence of excess RUHR. It should be recognized that the RUHR cannot be called the prevailing or even the main component forming material, and that, despite his presence in the threads in combination with PEG-T, get threads with wonderful and totally unexpected improvements, and that at the same concentration RUHR, because at concentrations above mentioned, some quality threads become unacceptable. It should be assumed that if more than 30 wt.% RUHR in relation to ECD-T RUHR irreversibly leached from the thread in the coagulation bath during processing.

Yarn of para-aramid/RUHR combination can be coated by the method of the invention in accordance with the following General process.

Water activation bath is prepared, ispolsu para-aramid yarn are immersed in a bath and stirred for faster activation. Then the thread is removed from the activation of the bath and washed until then, until the wash water will not remain the activating cations.

Washed and activated filament placed in another water bath, which will be clad bath and which may include surface-active agent to ensure complete wetting. Surfactant is preferred, but optional, and when used should be non-ionic and should be used in concentrations of from 1 to 5 g per 1 liter of the bath.

In thread type metal complex solution is to form a cladding baths. Complex metal solution is prepared by dissolving the appropriate amounts of metal salts, e.g. silver nitrate in water followed by addition of ammonia until then, until the solution becomes pale straw color and will not have pH=8-9,5, preferably 9. The appropriate amount of metal salt is that amount which will provide the desired weight of the reduced metal in the function plateruena metal thread. For example, it is desirable to prepare "40% reduction in tub", silver nitrate, to obtain the recovered silver in the number, composition is a wide range of metal concentrations. As will be seen in the examples, the preferred cladding baths range from 30 to 45% silver. It was found that the most effective and most preferred are baths with 35-40% silver.

Total clad baths should be such that the concentration of silver nitrate was less than 10 g/l Established that the metal complex solutions that have excessive concentration of metal cations can form rather not containing metal granules than tightly adhering metal coating.

Clad bath immersed in her threads stirred at a moderate pace for 10-20 min to ensure close-to-equilibrium system, and then in a bath add formaldehyde as reducing agent. Typically, the formaldehyde is added in the form of a 37 wt.% aqueous solution and in a quantity to obtain a molar ratio of silver from 1.1-1 to 2/1 or more.

The formaldehyde can be added all at once or gradually over time. For example, it is established that it is expedient to add the formaldehyde 10%-governmental portions over 1 h or so. The stirring is preferably continued until, while in the analysis clad baths will not receive the stitching.

All of the above stages can be performed with different baths at temperatures from 10 to 60oC and preferably 20-40oC.

Instead of complex solutions of silver for the deposition of other metals can be applied to other solutions. Nickel, copper, gold, etc. can be applied in the same way. If it is desirable or required for additional surface activation, you can use a bath having a low concentration (2-5%) of silver, after which you can apply complex solutions other clad metals. Nickel bath may include 0,2 Nickel chloride and 0.2 molar hypophosphite sodium pH brought ammonia to 9-9,5. Copper bath may include 30 g/l of copper sulfate, 100 g/l Rochelle salt (potassium tartrate sodium) and 50 g/l of 37% formaldehyde solution brought with sodium hydroxide the pH to 11-12.

Testing methods.

The resistivity. The resistivity of the filaments can be defined in ohms per inch thread or in the case of weaving or knitting yarns in ohms per square. The absolute values for each determination are the questions of the size of yarn and fabric structure in addition to the number of clad material and the continuity of the cladding.

reimut to the filaments at a distance of one inch.

To determine Ohm per square on a textile fabric ohmmeter probes, which have a length of one inch, pressed tightly in parallel and at a distance of one inch.

In any case, the resistivity is expressed in ohms, which are read by the reading ohmmeter.

The adhesion of the metal. Adhesion clad metal is measured on the fabric of the clad strands rubbing plated surface to determine the ease with which the metal is removed from the substrate. The degree of adhesion can be measured in a subjective way by rubbing clad products by hand to determine the degree of abrasion of the metal compared to the control material.

Objective methods for measuring adhesion is not sufficiently developed. Was elected the so-called "test abrasion, developed and supplied by the certificate American associan of textiles Chemist & Colourist (A. ATS) to determine the color stability at colouring. When tested for abrasion, specified as ATSS test method 116-1983 for carrying out controlled tests on the tested tissue, apply a rotating vertical procmeter. The results of the abrasion test are presented in a scale of 1-5 with 5 to provide the e preferred examples all parts are by weight, if not specified otherwise.

Example 1. a 10-foot coils from multiple threads, as indicated below, soaked each for 20 min in a solution of 45.6 g of tin chloride in 400 ml of water with pH, brought with HC to 1.5. Each skein was washed with water and then placed in a solution of 6.8 g of silver nitrate, 3 ml of nitric acid and 5.5 g of 37% aqueous formaldehyde, 400 ml of water to which was added ammonium hydroxide to achieve a pH=9.

Silver, spontaneously planirovanie on each thread, and the threads were washed and inspected. All the threads in the test were 1000 filament - 1500 denier. One thread was made of filaments 85% ECD-T and 15% of the RUHR (40 000) and one strand of filaments 75% PEG-T and 25% of the RUHR. The control thread was 100% ECD-So

Although all the threads had some degree of electrical conductivity, plating was badly stuck to the treads (easily erased) and well adhering to the thread containing the RUHR (difficult erased).

The method that was used for bezelektrodnogo coating aramid surfaces in the following examples according to the invention is as follows.

The thread described in the specific example of the type was associated in the bundles. 500 g of this skein soaked in the ribs, it was used a sufficient amount of formaldehyde. The molar ratio of formaldehyde to silver may be from 1.2 to 2 or more.

Example 2. The thread of 85% poly(p-phenyleneterephthalamide) (PEG-t), and 15% of the RUHR (40000 MB) with 1000 filaments and 1500 denier, as Hank was planirovali the method according to the invention in 40% silver bath as described above. Threads were twisted, as indicated in example 1, the previously mentioned European patent N 401740.

For comparison was planirovali thread of 100% PEG-T with 1000 filaments and 1500 denier, in the form of the rolls, applying the same procedure as described above, and also in a known manner. All comparative tests were carried out in 40% silver tub.

ECD-T thread has planirovali also the method described in German patent N 1197720. ECD-T surface activated by immersion for 3 minutes in a bath of colloidal palladium, washed, soaked for 2 min and 5% sodium hydroxide solution and washed. Then the thread was planirovali 40% silver bath, applying the same procedure as described above. A bath of colloidal palladium was prepared by pouring together equal volumes of 0.2 molar solution of palladium chloride, and then setting the pH with HCl to less than 1.

the adhesion of the plating was "Cracking-test", as explained above.

Example 3. As an additional test of the improved adhesion between the filament and substrate lakirovannym metal filament of the invention, processed as in example 2, and thread made of 100% PEG-T was planirovali the way described above, and clad filament conducted through the device, in which the filament extends through the die plate to be concluded in thermoplastic material, and then these threads in the package were dissected to obtain the pallet for subsequent forming process. An example of such a device is described in U.S. patent N 4312917, and the method is called "Patrizia".

thermoplastic material was nylon 6,6, temperature range processing was 265-295oC, and settings of the machine was such that when placed in the matrix product amounted to about 35% by weight of the filaments. Processing clad threads this way went smoothly, and Packed the product was cut into coils with a length of about 0.25 inch. Processing threads only from ECD-T was difficult, because the clad metal was peeled off from the thread and let extrusion binder resin. A number of the Packed product was nevertheless collected and tested for comparison with the pallet Packed filaments according to the invention.

Example 4. A group of strands of PEG-T with a different number RUHR (40000 MB) planirovali the method according to the invention, as described above, and tested for resistivity. Clad bath for this example consisted of 25% silver.

Clad filaments were tested for resistivity. The results are shown in table.2.

Threads were twisted to achieve concentrations RUHR listed in table.2.

For control and comparison threads only from ECD-T, without the RUHR, was also planirovali in the same conditions.

From this example we see that the mean range of concentrations of the RUHR, useful for obtaining clad filaments according to the invention. Although it may seem that thread, which has 12% of the RUHR, and have a much lower resistance than give the thread with higher and lower Konya. Advantages of the invention are achieved in a wide range of concentrations of the RUHR, from 3 to 30%, and the preferred concentration range is 9-15%.

As a subjective test, the adhesion of the silver coating of the filaments of this example was used up manually, the results were recorded. Silver is difficult erased with threads that had the contents of the RUHR, and very easy to control threads, not comprised of the RUHR.

Example 5. In accordance with the procedure above, ECD-T threads, comprising 15% of the RUHR (40000 MB) planirovali silver in baths having a number of different concentrations of silver.

Clad filaments were tested for resistivity. The results are shown in table.3.

The thread with the highest conductivity was obtained using baths that contained silver in concentrations of from 25 to 55%. The bath concentrations less than 20% and more than 60% plating is ineffective to obtain a conductive coating. Threads with the most high resistivity had a silver coating that have been washed with very great difficulty, which means the highest adhesion of the silver coating to the substrate filament.

Example 6. In Sohotel in the bath with a concentration of silver of 50%.

Clad filaments were tested for resistivity. The results are shown in table.4.

Thus, in the practice of the invention are acceptable to a wide range of molecular weights for the RUHR. Because of the limits of solubility, i.e., the excess solubility at very low molecular weights and excessive solution viscosity at very high molecular weights, the practical range of molecular weights for the RUHR is 5000-500000. The preferred range is 10000-24000.

In this example, the silver is very difficult erased clad with threads.

1. The way bezelektrodnogo application of metallic coating on the surface of the aromatic polyamide, characterized in that as a product of the aromatic polyamide used a product made from the composition comprising 70 to 98 wt. aromatic polyamide and an additional 2 to 30 wt. polyvinylpyrrolidone, in the coating process perform the following steps: processing the surface of the product with an aqueous solution containing the activating cations tin, washing the surface to remove unreacted activating cations tin, immersion surfaces washed in an aqueous solution, sodetel, for recovery of the metal cations and the formation of the coating.

2. The method according to p. 1, characterized in that the product of the aromatic polyamide is a thread.

3. The method according to p. 1, characterized in that the metal forming the coating, selected from the group consisting of silver, copper and Nickel.

4. The method according to p. 1, characterized in that the reducing agent is formaldehyde, and the process is carried out in the presence of ammonium hydroxide, which is the pH regulator.

5. The method according to p. 1, characterized in that the use of polyvinylpyrrolidone (mol.m. 10000 40000.

6. The method according to p. 1, characterized in that the aromatic polyamide used aromatic polyaramid.

7. The method according to p. 1, characterized in that the aromatic polyamide used polyparaphenyleneterephtalamide.

8. The product of the aromatic polyamide coated with a metallic coating, wherein the product is made from a material containing 70-98 wt. aromatic polyamide and additionally 2-30 wt. polyvinylpyrrolidone.

9. The product under item 8, characterized in that it is made in the form of threads.

10. The product under item 8, characterized in that the metal coating is to ensure polyamide is polyparaphenyleneterephtalamide.

12. The article on p. 11, wherein the metal is silver.

 

Same patents:

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27 cl, 4 tbl, 4 ex

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24 cl, 4 tbl, 1 ex

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31 cl, 21 dwg, 5 tbl, 18 ex

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22 cl, 3 dwg, 9 tbl, 20 ex

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1 ex

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1 tbl

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1 tbl, 10 ex

Polymer composition // 2383569

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EFFECT: increased stiffness of melt at simultaneous reduced pressure during processing and insignificant load on engine, simplification of moulded items production.

6 cl, 1 ex, 2 tbl

FIELD: chemistry.

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7 cl, 3 tbl, 18 ex, 8 dwg

FIELD: metallurgy.

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EFFECT: facilitates preparation of complex phosphonic electrolytes and solutions of specified composition and concentration not containing undesirable impurities, it also facilitates upgraded processibility of the method of preparation of electrolytes and solutions, and expands an arsenal of existing methods of preparation of nitrilotri-(methylenphosphonates) electrolytes and solutions for coating with metals and alloys.

5 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention refers to methods formation of component coating by chemical conversion for dielectrics, semiconductors and electronegative metals (iron, aluminium, titanium and their alloys), as well as combined ceramic-metal materials and can be used in radio engineering industry, in instrument engineering and for manufacturing of printed-circuit boards and decoration of wax, plastisol and other products. The first version of the method involves component surface processing in sorption stabilising solution in ratio as follows, g/l: SiO2 - (35-45)×10-3, Al2O3 - (0.5-10)×10-3, MgO - (0.5-10)×10-3, HF - (0.5-1)×10-3, water - the rest. It is followed with sensitisation, activation in solution containing palladium chloride and hydrochloric acid, and metal plating. The second version of the method involves sensitisation of component surface in sorption stabilising solution in ratio as follows, g/l: SiO2 - (35-45)×10-3, Al2O3 - (0.5-10)×10-3, MgO - (0.5-10)×10-3, HF - (0.5-1)×10-3, water - the rest.

EFFECT: improved plating quality ensured with higher catalytic activity of processed surface and reduced palladium content in solution for activation.

2 cl, 8 tbl, 8 ex

FIELD: technological processes.

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EFFECT: invention provides for production of metalised dispersed woven and nonwoven materials using simplified technology, with simultaneous cheapening and provision of production safety due to use of proposed ingredients and their certain ratio.

2 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to chemical application of metal coating. The procedure consists in bringing substrate into contact with a bath containing a surface active substance, reducer and metal chosen from a group Ag, Cu, Pd and Co. Also temperature of the bath is higher, than temperature of dimness of solution present in the bath in form of at least two phases. The bath contains water solution of silver salt, substituted alkylene-oxide compound, boric acid, reducer and complex former. The procedure includes silicon surface etching, immersion of silicon surface into the above described bath, leaving silicon surface till silver coating forms on it and extracting silicon surface coated with silver from the bath.

EFFECT: increased visual reflex and electrical conductivity.

34 cl, 2 ex

FIELD: metallurgy.

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EFFECT: method makes it possible to produce high-quality tin coatings with increased corrosion resistance on parts of copper or its alloys.

3 cl, 6 ex

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