Thermoplastic polyimide and its variant, the polyamide acid and its variant and hot-melt laminated film for coating wire

 

(57) Abstract:

Thermoplastic polyimide of the General formula I, where AG1, AG4contain at least one organic radical structures (a)-(C); R1, R2= N, CH3CH2CH3, phenyl (other designations, see p. 1 formula). New thermoplastic polyimide is characterized by a robust adhesive properties at low temperatures and good resistance to radiation. 5 C. p. F.-ly, 2 tab., 3 Il.

The invention relates to new thermoplastic polyimide, new Polynicotinate, which is a precursor of thermoplastic polyimide, and a new layered thermoplastic film, in particular, is suitable for coating elektroprovodnyh when enabled, the layer of welding agent containing a novel thermoplastic polyimide. More specifically, the invention relates to new thermoplastic composition characterized by a robust adhesive properties at low temperatures and good resistance to radiation and, in addition, the invention relates to a new Polynicotinate, which is a precursor of thermoplastic polyimide composition, and a new layered thermoplastic film, in particular, prodazhnymi adhesive properties. In particular, a new layered thermoplastic film has a definite impact on resistance to radioactive rays.

Thanks to the good heat resistance, satisfactory physical properties at low temperatures, good resistance to chemicals and satisfactory electric characteristics of the polyimide film is widely used for making various components electrical and electronic equipment. However, since the polyimide, which is used in the form of a film, as a rule, is insoluble and infusible, during wrapping metal wire polyimide film is usually on a polyimide film is applied layers (proslaivaet) thermoplastic resin.

In European patent application N 456515 as an adhesive can be essentially used in the resin composition.

This glue can be offered for use in the form of a lacquer, or varnish can be applied on a substrate such as a glass plate, stainless plate, and so on, to dry and then remove to get the elastic uncured adhesive film without a substrate (adhesive tape self-sustained type). This glue can be used for different purposes, and he finds, cha is a rotary binding metal foil, for example, copper foil or aluminum foil to the substrate, for example a metal plate, such as aluminum foil or plastic film, such as polyimide film.

For example, in European application N 154714 presents polyimide copolymer consisting of an aromatic bis(averagegrade) aromatic diamine and aliphatic diamine. This polyimide copolymer shows a wide range of glass transition temperatures while maintaining the desired flexibility and mechanical properties under tension. The glass transition temperature are suitable for many applications, in particular for injection molding. However, these polyimides have a high glass transition temperature exceeding 250oC.

In the aforementioned European application N 456515 presents the polyimides containing the repeating unit in the molecule, represented by several formulas, these polyimides have high solubility in organic solvents and a low softening temperature, and the resin composition containing the polyimide, show excellent properties, even when their utverjdayut at low temperature.

However, these polyimide compositions have a high temperature is authorized physics in the field of elementary particles, the proposed design of advanced accelerators for generating high energy. In order to reliably generate higher the energy necessary to generate extremely intense magnetic field using a magnet, able to receive and send a huge electric shock. In a lot of talk recently about the use of superconducting magnets, including superconducting wire. In many cases, for a superconducting wire using only the oxide containing copper. However, when applying an insulating coating on the superconducting wire is used, the adhesive of thermosetting resin, after carrying out heat treatment properties of the oxide components in superconductors easily changed, and the result is degradation of the physical properties of superconducting magnets. To prevent this, you need to use this type of adhesive that securely cures itself and coupled with the superconducting wire at low temperature.

In the initial stage of the above-mentioned accelerator accelerates the movement of elementary particles containing proton-proton and electron-electrons to cause them to collide with each other and their collapse before ... the STV radiation. For this reason, it is necessary that the insulating covering material and the intermediate adhesive superconducting magnet were extremely resistant to radiation.

Typically, to form a coating on superconductors operating at very low temperature, use a coating composed of layers of thermosetting resin and polyimide film. However, in this case, to otvetit epoxy resin, over a long period of time, apply a high temperature, which inevitably causes degradation in superconductors. In addition, the epoxy resin may not be quite resistant to radiation and, consequently, in the expectation that more radiation is generated in proportion to the empowerment of accelerators, it is desirable to continue developing a more effective adhesive to ensure sufficient adhesion at an exceptionally low temperatures and high resistance to radioactive rays.

Recently for the superconducting wires used hot-melt laminated film obtained from the polyimide and Polynicotinate. To prevent the superconducting who had been the less than 145oC.

When using hot-melt laminated film obtained from polyamide, which is a precursor of the above-mentioned polyimide, however, still faced with the above problems.

Solving the above technical problems could facilitate the use of such adhesive, which is capable of samootverzhenij at very low temperatures that could prevent unwanted degradation of superconductors. On the other hand, since such an adhesive quickly someotherdude at normal temperature, the lifetime of such adhesive in B-stage is so short that the adhesive may not be offered for sale for use in the form of laminated film.

Summary of the invention

Therefore, to fully resolve the aforementioned problems, the inventors have conducted comprehensive research to offer a new polyimide adhesive, able to provide reliable adhesion at low temperatures and good resistance to radioactive rays, a new thermoplastic polyimide, suitable for use as the adhesive film, and a new hot-melt laminated film suitable for forming coatings on provodniki in the process of thermal melting and combines outstanding softness and adhesive properties.

In General, the new thermoplastic polyimide, the invention depicted General formula (1) corresponding to given below the chemical structure.

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in which Ar1, Ar2, Ar4and Ar6each individually represent divalent organic radical, whereas Ar3and Ar5each individually represent a tetravalent organic radical, and in which L, m, t and n, each independently represent a positive integer of 1 or greater than 1, and L, m, n and t are expressed by the following formulas 1 n 15, t 1, 1 L 15, 1 m 15.

Among the components of the new thermoplastic polyimide component shown in the General formula (1) as Ar1represents at least one radical selected from the group of divalent radicals, the chemical structure of which is shown below.

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where R1, R2=H, CH3CH2CH3Ph

-H2C-CH2-,

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where R1, R2= H, CH3CH2CH3Ph.

Among the components of the new thermoplastic polyimide component shown in the General formula (1) as Ar2represents at least one radical selected from the group of divalent aromatic was radical polyimide component, shown in the General formula (1) as Ar3represents at least one radical selected from the group of tetravalent organic radicals, the chemical structure of which is shown below.

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Among the components of the new thermoplastic polyimide component, represented in the General formula (1) as Ar4choose from the group of divalent organic radicals, the chemical structure of which is shown below.

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R1R2=H, CH3CH2CH3Ph, R1R2=H, CH3CH2CH3Ph.

Among the components of the new thermoplastic polyimide component, represented in the General formula (1) as Ar5represents at least one kind radicals selected from the group of tetravalent organic radicals, the chemical structure of which is shown below.

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Among the components of the new thermoplastic polyimide component, represented in the General formula (1) as Ar6represents at least one kind radicals selected from the group of divalent aromatic radicals, the chemical structure of which is shown below

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In particular, the new thermoplastic polyimide, in addition, represent what Telenesti, mean divalent organic radical, whereas Ar5means tetravalent organic radical, and where L, n and t each denote a positive integer equal to 1 or greater than 1, and L, n and t are expressed by the following formulas: 1 L 15, 1 n 15, t 1.

In General, the new Polynicotinate, which is the predecessor of the new thermoplastic polyimide, the invention is represented by formula (3) below

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in which Ar1, Ar2, Ar4and Ar6each individually represent divalent organic radical, whereas Ar3and Ar5each individually represent a tetravalent organic radical, and where L, m, t and n, each independently represent a positive integer equal to 1 or greater than 1, and L, m, n and t are expressed by the following formulas: 1 L 15, 1 15 m, 1 n 15, t 1.

In particular, the new Polynicotinate, in addition, represented the General formula (4) below,

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in which Ar1, Ar2and Ar6each individually represent divalent organic radical, whereas Ar5means tetravalent organic radical, and where L, n and t each independently denote a positive integer, Rav is th layered film, suitable for formation of a coating on a conductive wire, conforming to the invention is distinguished by a new structure in which there are layers of polyimide film and welding agents, consisting mainly of a thermoplastic resin.

In accordance with another feature of thermoplastic resin of the new hot-melt laminated film suitable for forming a coating on a conductive wire and relevant to the invention, thermoplastic resin has a softening temperature below 220oC and consists only of a new thermoplastic polyimide described previously in any of the preceding sections.

In addition, another main feature of the polyimide film is that it contains at least one kind of acid dianhydride corresponding to the following formulas

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and at least one kind of diamine corresponding to the following formulas

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Essentially, a new layered thermoplastic film suitable for forming a coating on a conductive wire, in accordance with the invention contains a polyimide film, specifically it contains the film from the new polyimide, and a layer of welding agent, sotoyama the AI layer. Therefore, after winding the layered film superconducting wire, for example at the location of welding agent inside the superconducting wire wrapped layered film is thermally treated at a certain temperature above the softening temperature of the layer of welding agent. As the temperature exceeds the softening temperature of the layer of welding agent, the layer of welding agent contained in the layered hot-melt film is alloyed with the superconducting wire, when the temperature exceeds the maximum temperature of its softening 220oC. This, in turn, allows the inner wire to avoid the harmful effects of heat treatment and, thus, protects the wire from losses due to degradation. As mentioned above, a new layered thermoplastic film suitable for forming a coating on a conductive wire, in accordance with the invention with a view to making it excellent physical properties in common fields composed of polyimide films of new, different reliable heat resistance, high performance at a low temperature, long-term resistance to chemicals and special Elektricheskiye properties and melting at a low temperature. In particular, the new hot-melt laminated film perfectly suitable for forming coatings on superconducting wires.

Accordingly, a new thermoplastic polyimide represented by the above formulas (1) and (2), and proposed by the present invention, has excellent cut-through, reliable adhesion properties, low hygroscopicity and good resistance to radiation. Specifically, thanks to a new composition, thermoplastic polyimide, corresponding to the invention has a glass transition temperature between 100oC and 250oC, and furthermore, since thermoplastic polyimide may be contacted with the copper foil directly in the process of formation of the layered structure at a temperature exceeding the glass transition temperature, thermoplastic polyimide can be processed into a film suitable for use, yet remains in a state of polyimide. On the other hand, the new Polynicotinate represented by the above formulas (3) and (4) and acting as a precursor of thermoplastic polyimide, can be transformed into kidny component after direct application to the film-substrate and easily obey the invention, detects very low coefficient of hygroscopic approximately 1%, a variety of physical properties, including heat resistance, prevents degradation.

As is evident from the above advantages, in contrast to conventional adhesives based on epoxy resin new thermoplastic polyimide and polyamideimide corresponding to the invention, individually, demonstrate reliable adhesive properties at low temperatures and good resistance to radiation and, in addition, by effectively transforming them into film adhesive of the invention offers the ideal thermoplastic polyimide composition.

Moreover, as the new layered thermoplastic film, perfectly suitable for formation of a coating on a conductive wire, proposed by the inventor, is composed of a layer film of a new polyimide, characterized by special physical properties, such as temperature, operating characteristics at low temperature, chemical resistance and electric characteristics, and a layer of welding agent consisting mainly of a thermoplastic resin, when the wrap elektroprovodnyh such thermoplastic layered planet thermally fused to the wire in the temperature interval in which the physical properties of the wire can remain constant without any degradation. Therefore, when the superconducting wire are coated with a thermoplastic laminated film of the invention, the layered film can wrap the wire, melting, without prejudice to the properties of superconductivity inherent in the superconducting wire.

Further, as thermoplastic laminated film of the invention contains a layer VariAudio agent consisting mainly of a thermoplastic resin, manufacturers can commercially distribute layered film containing a layer of welding agent to facilitate stakeholders the process of working with wire by using a new layered film, and ultimately, improve performance.

Moreover, because the invention uses for the surface coating of insulating material containing a polyimide resin having adhesive properties and a glass transition temperature less than 220oC, from among thermoplastic polyimides represented by the General formulas (1) and (2), and the layer of welding agent containing polyimide, can be successfully implemented properties such as reliable adhesion at

Fig. 1 is a General explanation of the new method of applying the wire coating of thermoplastic laminated film proposed by the invention and which is suitable for formation of a coating on the wire.

Fig. 2 is a General explanation of another new method of applying the wire coating of hot-melt film proposed by the invention.

Fig.3 is a General explanation of another method of applying the wire coating of hot-melt film proposed by the invention.

Detailed description of the invention

Below are examples of thermoplastic polyimide, polyamidoimide, which is a precursor of polyimide, and a thermoplastic laminated film for formation of the coating on the wire, proposed by the invention, and methods for their preparation.

First, the following describes a method of obtaining a solution Polynicotinate, which is a precursor of polyimide corresponding to the present invention. First diamine represented the General formula (5), is dissolved or dispersed in an organic solvent in an atmosphere of inert gas such as argon or nitrogen.

H2N - Ar7- H2N (5)

where Ar7siloti, with the structure depicted General formula (6) given below

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or a solution of the diamine is added to a mixture of eveningtide acid and at least one kind of organic dianhydride tetracarbonyl acid, represented the General formula (7) below,

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located in the solid state and in solution in an organic solvent, and where Ar9present in General formula (7) denotes a tetravalent organic radical. And finally, get a solution Polynicotinate, which is a precursor of polyimide, and represented the General formula (4)

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in which Ar1, Ar2and Ar6each individually represent divalent organic radical, whereas Ar5means tetravalent organic radical, and where L, n, t is a positive integer equal to 1 or greater than 1, and L, n and t are expressed by the following formulas 1 L 15, 1 n 15, t 1.

Next, the following describes a method of obtaining a solution Polynicotinate, which is the predecessor of another polyimide corresponding to the invention. First, only one apigenin represented by the formula (8)

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or a mixture of EPIDEMIA and at least one of the diamines, the image is bound gas, such as argon or nitrogen, where Ar10present in General formula (8), means a divalent organic radical. Next, the solution is added to eveningtide acid, represented the General formula (6) above, or to the mixture of eveningtide acid dianhydride and organic tetracarbonyl acid in the solid state and in solution in an organic solvent. And finally, get a solution Polynicotinate, which is a precursor of polyimide, and represented the General formula (3) below

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in which Ar1, Ar2, Ar4and Ar6each individually represent divalent organic radical, whereas Ar3and Ar5each individually represent a tetravalent organic radical, and where L, m, n and t each independently represent a positive integer equal to 1 or greater than 1, and L, m, n, t is expressed by the following formulas: 1 L 15, 1 15 m, 1 n 15, 1 t 15.

Despite the fact that the reaction is regular in the sense of reversibility of the above-mentioned processes, first get the solution containing only evidenceid acid, represented above by formula (7), or at least one dianhydride of organicheskaia acid dianhydride and organic tetracarbonyl acid. In the resulting solution may be added or diamine represented by the above formula (6), or only apigenin depicted above General formula (5), or a mixture of EPIDEMIA and at least one kind of diamine represented by the above formula (6), as in the solid state and in solution or suspension in an organic solvent.

The above processes are preferably carried out at a temperature in the region -10oC to 50oC, preferably in the temperature range from -5oC to 20oC. the Time of reaction is from 0.5 to 6 hours. As a result of reactions get polyamide, depicted above General formulas (3) and (4), the precursor of thermoplastic polyimide, the proposed invention.

In order to carry out the reaction required to obtain solution Polynicotinate, you can use various organic solvents, including, for example, sulfoxidov, such as dimethylsulfoxide or diethylsulfoxide, formamide, such as N,N-dimethylformamide or N,N-diethylformamide, and acetamide, such as N,N-dimethylacetamide or N,N-diethylacetamide, etc. Any of these organic solvents may be used Eome, any of these polar solvent to obtain a mixture of solvents may be mixed with nerastvorim to Polynicotinate, such as acetone, ethanol, isopropanol, benzoylmethylecgonine or similar.

To obtain the polyimide of the polyimide solution, which is a precursor of thermoplastic polyimide, a solution of the polyamide, in essence, transform into imide thermal or chemical means. The next stage is the way to dehydration and close the loop component solution Polynicotinate, in other words - imidazole solution Polynicotinate described below.

When thermal solution of polyamidation imagesyour through the successive processes described hereinafter. First, a spray solution or put another way, on a substrate, such as an organic film made of PET, or on the platen, or to the conveyor belt. After the formation of the film it is dried so that it has become self-supporting. It is desirable that the drying process was carried out at a temperature slightly below the 100oC for 5 to 90 minutes.

The dried film is then further heated to complete the imide to complete the formation of the polyimide film containing the 100oC to 350oC, preferably from 150oC to 300oC. Although there are no restrictions in the rate of rise of temperature, it is desirable that the temperature was raised gradually until the maximum suggested above values. The duration of the heating process depends on the film thickness and the maximum temperature, which is used in the processing of the film. However, it is desirable that the heating process was carried out for 10 seconds to 30 minutes after reaching the maximum temperature. First film separated from the substrate, and then securing the ends of the film, carry out the above-mentioned process final heat. The resulting polymer has a very low coefficient of linear expansion.

The chemical method of implementation of imidazole solution Polynicotinate first to the solution Polynicotinate add selected dehydrating agent and a tertiary amine as catalyst, in excess of stoichiometric, and then the mixed solution is treated in the same way, which is used during thermal dehydration process, and finally get the film right polyimide.

Comparison of thermal and chemical obrabotki and a lower coefficient of linear expansion characteristic of polyimide, obtained by chemical treatment. However, the invention can also be implemented with a combination of thermal and chemical processing methods.

After the completion of imidization Polynicotinate depicted above General formula (3), get a new polyimide compound represented the General formula (1) below

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in which Ar1, Ar2, Ar4and Ar6each individually represent divalent organic radical, whereas Ar3and Ar5each individually represent a tetravalent organic radical, and where L, m, t and n, each independently represent a positive integer of 1 or greater than 1, and L, m, n and t are expressed by the following formulas 1 n 15, 1 L 15, 1 15 m, t 1.

As eveningtide acid represented by the above formula (6) may be used either arifianto selected from glycols or phenols. Specifically, the radical Ar8present in the above General formula (6), has one of the data structures below.

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Specifically, in order to obtain proportionate physical properties, it is desirable that the radical Ar8had mostly chemical structure is 3 CH2CH3Ph.

As the organic dianhydride tetracarbonyl acid can be used dianhydride any tetracarbonyl acid. The radical Ar9present in the above General formula (7) denotes a tetravalent organic radical and, more specifically, has the structure shown below.

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Dianhydride any organic tetracosanoic acids may be used either one by one or in various combinations with each other. Specifically, to obtain proportionate physical properties, it is desirable that the radical Ar9consisted mainly of at least more than one kind of organic dianhydride tetracarbonyl acid from the number having the structure indicated below.

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As Epidemiol depicted above General formula (8), by carrying out the invention can be used apigenine selected among containing glycolic or phenolic groups. Specifically, the radical Ar10present in the above-mentioned General formula (8), can be represented by one of the following structures

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Specifically, to obtain proportionate physical properties, it is desirable that the radical ArPh, R1, R2=H, CH3CH2CH3Ph.

As the radical Ar7present in the above General formula (5) of the diamine and which is essentially divalent organic radical, can be used any Ar7specific suitable chemical structures of which are given below.

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More specifically, it is desirable that the radical Ar7represented at least more than one kind of divalent organic radical, the structure of which is given below.

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In accordance with the invention, it is possible that thermoplastic polyimide represented by the General formula (1) and General formula (2) are using eveningtide acid represented by the General formula (6) in which the radical Ar8corresponds mainly Ar1or Ar4shown in the General formulas(1), (2), (3), (4), the glass transition temperature between 100oC and 250oC, the adhesive power when linking with copper foil and very low hygroscopic coefficient, equal to about 1%.

And it is also possible that the resistivity to radioactive rays when using the polyimides obtained through additional diag testvol mainly Ar3or Ar5shown in the General formulas(1), (2), (3), (4), was increased.

In the above General formula (1) from the main unit, contained in a new thermoplastic polyimide, there are number of repetitions l, m and n, each of which indicates a positive integer equal to 1 or more than 1. In particular, it is desirable to repeat the numbers l, m and n were equal to less than 15. This is because, if the number of repetitions exceeds 15 times the sum of the numbers of repetition of l and m, the result will be biased ratio in copolymerization and reducing the practical effect polymerization. More specifically, in this case it will be difficult to obtain the desired adhesive properties at low temperatures. The polymer may also contain links to various values of the number of repetitions l, m and n. However, especially desirable that the values of the numbers of repetition of l, m and n, respectively, have remained constant.

It is desirable that the number of repetitions t in main unit was the least integer greater than 1, equal to 15 or less than 15. Although restrictions on the molecular weight of the new thermoplastic polyimide absent, to maintain appropriate strength of the resulting polyimide, it is desirable that Brednikova molecular m is facing difficulties. To solve the problem, the molecular weight of the polyimide is measured indirectly. For example, when a polyimide synthesized from the obtained Polynicotinate, the molecular weight of the polyimide can be determined based on a value corresponding to the molecular mass of polyamidation.

Even in the case of new Polynicotinate depicted above General formula (3), it is desirable that the number of repetitions l, m and n have the main unit, each individually would be a positive integer equal to 1 or greater than 1. In particular, it is desirable that each of the numbers of repetition of l, m and n were less than 15. Single polymer molecule may contain links with different numbers of repetitions l, m and n. However, especially desirable that the amount of duplicate numbers l, m and n, respectively, remained constant. It is desirable that the number of repetitions t in main unit was positive integer greater than 1, equal to 15 or less than 15.

New polyimide corresponding to the invention, has a special cut-through, reliable adhesion at a low temperature, low hygroscopicity and good resistance to radiation. More specifically, with the new as the polyimide can be coupled with a polyimide film directly when layering it at a certain temperature, overlying the glass transition temperature. From the test results it is obvious that the new polyimide corresponding to the invention, detects a sufficiently low coefficient of hygroscopic - 1%, as determined when immersed in pure water at 20oC for 24 hours, and, in addition, it shows high resistance to radioactive rays.

Therefore, the invention facilitates the transformation of the new thermoplastic polyimide film. This, in turn, favors a reliable adhesion of the copper foil to a flexible PCB for wiring made of a new thermoplastic polyimide film without adhesive. When the process of adhesion, copper foil may be contacted with the other surface through the clutch can become loose layer on the other surface. New polyimide film is particularly suitable for the base, for example, boards for multi-wire installation.

In addition, the new thermoplastic polyimide film proposed by the invention, can also be used as an adhesive when using films, deprived of its own adhesive properties. In this case, since the new thermoplastic polyimide film can be applied exactly in in the retene, you can directly apply on plain film. After completing the process of imidazole to apply, you may be prompted new film containing the adhesive layer. Polynicotinate proposed by the invention, may be offered for use in the most different purposes, and specific restrictions on its use there.

As a new thermoplastic polyimide, as mentioned above, has various special features, the invention can offer a new hot-melt laminated film suitable for coating wire, consisting of a new film of a polyimide and a layer of welding agent, which mainly contains a thermoplastic polyimide resin.

In accordance with the invention, various thermoplastic polymers can be used for inclusion in the composition of hot-melt laminated film suitable for coating wire, both individually and as a mixture of different types of thermoplastic polymers, including, for example, polyimide resin having adhesive properties similar to those mentioned above, polyamide, polyesters, polyethylene, polyvinyl butyral, polyurethane, polyetherimide, etc. However, in order to obtain proportionate physical properties, preferred the East film, suitable for coating wire received in accordance with the invention, used for thermal splavki with superconductors, in order to prevent, for example, the superconducting wire from degradation, it is preferable that the softening temperature of the used thermoplastic resin was less than 145oC.

It is essential that the layer of welding agent includes and contains mainly the above-mentioned thermoplastic resin. However, the layer of welding agent may additionally contain other components, such as inorganic filler.

The layer of welding agent in accordance with the invention is formed accurately, so that the total thickness ranged from 1 μm to 50 μm, preferably from 5 μm to 20 μm. If the total thickness of the layer of welding agent exceeds the established limits, it can not only cause the protrusion of the layer of welding agent for the edge of the polyimide film base with their fusing tasks for each other, but will also impede the manifestation of a new polyimide film in the fullness of its special physical properties. On the other hand, if the total thickness of the layer of welding agent will be less than the above, have a look at the acquisition, receive a first fusing film dissolved Polynicotinate, and then through a process of dehydration and closing cycle, while dissolved Polynicotinate get the copolymerization reaction anhydrides of various acids, such as, for example, dianhydride pyromellitic acid, dianhydride biphenyltetracarboxylic acid, dianhydride benzophenonetetracarboxylic acid, etc. and various diamines, such as diaminodiphenyl ether, p-phenylenediamine or bis-(aminophenoxy)-propane.

In addition, can also be used casionally product, such as polyamideimide and polyetherimide. Polyimide film proposed by the invention is based on the concept of inclusion and quasimidi products. It is desirable that the polyimide film was composed of polyimide. In particular, preferably, when a polyimide film corresponding to the invention, includes at least one kind of acid dianhydride having the structure shown below,

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and at least more than one kind of diamine having the chemical structure indicated below,

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When using the acid dianhydride and diamine as materials obtained polyimide plenkov which X indicates a tetravalent organic radicals, presented in the chemical structure shown below,

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a Y indicates a divalent organic radicals represented by the chemical structure shown below,

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An example of a polyimide film represented by the General formula (5), is a film APICAL (a product and trademark of the firm Kanegafuchi chemical industry Co. Co., Ltd. ). Due to the fact that a polyimide film represented by the General formula (5), is particularly stable heat resistance and satisfactory physical properties at low temperature, the film is suitable for the insulation of the wires (e.g., superconducting wires).

The thickness of the polyimide film that can be applied is in the range from 5 μm to 150 μm. Preferred for practical use, the thickness of the polyimide is from 10 μm to 125 μm. In particular, when a coating of a polyimide film is applied on the wire, it is preferable that each layer of polyimide film had a thickness of from 10 μm to 75 μm. If the thickness is less than the lower specified limit, it will not only hamper the formation of the layered structure, but may also cause unwanted damage during operation. On the other hand, if the thickness exceeds UCCA, suitable for coating conductors carried out in the invention, consists of layers of new polyimide film and welding agent consisting mainly of a thermoplastic resin. The layer of welding agent layered thermoplastic film having a layered structure may be formed by coating on the surface of the polyimide film of a thermoplastic resin dissolved in the solvent first, and subsequent implementation of the drying process.

Practically, after application to a polyimide film coating of the solute in the solvent of thermoplastic resin is quite certain thickness in the process of drying, so that the actual thickness of dried layer would correspond to the actual thickness of the layer of welding agent. For example, a thermoplastic laminated film can be obtained by imidization solution Polynicotinate, which is a precursor of polyimide resin having good adhesion, after the preceding distribution process solution Polynicotinate on the entire surface of the polyimide film. In another method of forming the layer of welding agent, a thermoplastic resin, previously transferred to the op is nye for coating wire, also is formed by carrying out the series of processes described hereinafter. For example, first collect a layered design, with consistently polyimide film, polyimide resin with adhesive properties, the pre-formed film, and are able to exfoliate the sheet, and then the components of the layered structure shrink when heated to glue them, and finally peeling the sheet peel off, and get layered thermoplastic film suitable for coating wire.

The obtained thermoplastic laminated film corresponding to the invention, wound or before her wound, on the layer of welding agent have a gasket made of polyethylene terephthalate, polypropylene or polyethylene. Before using layered thermoplastic film corresponding to the invention, for coating lead wire width of the film in accordance with the necessity.

Usually the process of applying to the wire a new layered thermoplastic film corresponding to the invention, carried out as described hereinafter. For example, as shown in Fig. 1, is first layered thermoplastic film 10 preset width Speer is e, the layered film 10 is heated to a certain temperature to decompose the layer of welding agent and thermally fused polyimide film 16 with the wire 12. In addition, as shown in Fig. 2, the layered film 10 can also be wound on the wire 12, resulting in contact both edges of the wound laminated film 10 with each other without overlapping. In addition, as shown in Fig. 3, in accordance with another method of the width of the layered film 10 make somewhat larger than the outer cylindrical surface of the wire 12, so that the layered film 10 could wrap along the wire 12. Although in practice you can use any of these methods, it is most preferable to wind the layered film 10 on the wire, based on the method shown in Fig. 1.

Thus, the described thermoplastic polyimide, polyamidoimide and the new film, laminated film suitable for coating wire. However, it should be understood that the invention is not limited to only these typical variations of the invention described above and, for example, for coating can serve as a superconducting wire or it can be the most common wire, such as mucheyami, changes and modifications based on the knowledge of specialists, without deviating from the invention.

Hereinafter more fully described specific examples of the invention. However, the scope of the invention is not limited to the following further examples. The radicals Ar1-Ar6corresponding to the General formula(1), (2), (3) or (4), are shown in table 1.

Example 1

In a volumetric flask with a capacity of 50 ml was placed 2 g of dianhydride, ethylene glycol bis-trimellitic acid (abbreviated below TMEG) and 20 g of dimethylformamide (below abbreviated as DMF), and then the components were mixed by a stirrer until complete dissolution. Regardless of this sample in a three-neck flask with a capacity of 500 ml, fitted with a stirrer, was placed 8.6 g of 2,2-bis(4 - aminobenzyl-oxyfuel)propane (abbreviated below VVRR), 12.3 g of 2,2 - bis(4-(4-aminophenoxy)phenol)propane (abbreviated below of the WAR) and 240,4 g DMF. The components were mixed by a stirrer to dissolve, while replacing the air in the flask by nitrogen. Then the flask of Ladenburg ("spider") with a capacity of 100 ml was placed 19.3 g of solid 3,3',4,4'-dianhydride benzophenonetetracarboxylic acid (abbreviated below BTDA), then BTDA was added to the solution AVRR in a three-neck flask. Using 5 g of DMF, was transferred to utworow for 30 min, it was added to 16.4 g of solid of the WAR and continued stirring for another 30 minutes After you have added 15.2 g of solid TMEG and stirring for 30 min another exemplary solution TMEG kept in a volumetric flask with a capacity of 50 ml, simultaneously observing the change in solution viscosity in a three-neck flask. After the viscosity reached a maximum, the introduction of the solution prepared TMEG stopped. The mixture solution was stirred for 1 h, resulting in a solution Polynicotinate, which was used for the manufacture of the film. To this end, the acid solution previously subjected to imidization, and then used for production of laminated film. The authors investigated the physical properties of this film.

In a volumetric flask with a capacity of 100 ml was filled with 2 g of isoquinoline, 20 g of acetic anhydride and well mixed. This solution was added to the obtained polyimide solution and well mixed. After complete removal of the air mixture caused by the layer film of polyethylene terephthalate (PET), and the obtained laminated film was heated up to 80oC and kept at this temperature for 25 minutes Next, the PET film was separated and gradually raise the temperature from 150 to 200oC, at which the layer of the mixture to stand for 10 minutes to imidazole and education in the result, thermoplastic poliya ASTM) has defined the coefficient of hygroscopic obtained polyimide. The glass transition temperature was 210oC, and the coefficient of hygroscopic - a total of 1.25%. The results of the tests are presented in table 1.

Next, laid sequentially one on another polyimide film "APICAL" (a product and a registered business name "Kanegafuchi chemical industry Co. Ltd."), film of thermoplastic polyimide and a peelable sheet material. Components connected to one another at a temperature of 150oC at a speed packaging of 2.2 cm/min with the purpose of obtaining a hot-melt laminated film suitable for use as wire insulation. After removal of the peelable sheet from the obtained laminated film on its surface was placed a copper foil and glued it to the surface at 150oC speed bonding of 2.2 cm/min and as a result have produced a layered film with a coating of copper foil.

Authors using the test method according to JIS-K6481 determined the strength of the film strength at normal temperature, having a value of 1.2 kgf/see test Results are presented in table 1. In addition, using applied in electronic engineering and is designed for 2 MeV wire, the authors felt the film on the radiation resistance by irradiating the film Lu>The polyimide obtained in the described example, contains structural units represented by General formula (1). The molecular weight of the polyimide is 100000-150000.

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Example 2

First in the flask 1 (any) with a capacity of 500 ml are mixed together to 16.9 g of 2,2-bis-[4-(4-aminophenoxy)phenyl] propane (hereinafter called the WAR) and 25.4 g of dimethylformamide (DMF), and then the mixture is stirred until then, until complete dissolution. In addition, 1.0 g of the WAR and 10 g of DMF mix together in another flask 2 with a capacity of 50 ml, and the mixture is then stirred until complete dissolution. Apart from these mixtures 11.9 g of dianhydride 2,2-bis-(4-hydroxyphenyl)propane-di - benzoate-2,2', 3,3'-tetracarboxy acid (hereinafter referred to as an ESDA), 4.5 g of dianhydride pyromellitic acid (PMDA) and 25 g of DMF are mixed together in a three-neck flask with a capacity of 500 ml equipped with a stirrer, and then cooling the mixture of water with ice in a nitrogen atmosphere, the mixture is dissolved completely.

Next, with stirring, a solution of the WAR, previously obtained in a 50 ml flask 1, quickly poured into the three-neck 500-ml flask. After mixing the solution for 30 minutes, watching the viscosity of the solution in the three-neck flask with a capacity of 500 ml, the WAR of the solution stored in 50-ml flask 2, the pic is-ml flask 2 in a three-neck 500-ml flask cease. Then the resulting solution is stirred for one hour. Next, the mixed solution is added to 78.2 g of DMF, stirred thoroughly, and get the solution right Polynicotinate.

The solution Polynicotinate poured on the film of PET and then heated at 80oC for 25 minutes. Then heated polyamidation component is dried until then, until it becomes self-supporting. Then the dried film Polynicotinate prepare the chin from a PET film and then is fixed on the metal substrate. Then the film Polynicotinate subjected to a stepwise heat treatment at 150oC 200oC, 250oC and 300oC for 5 minutes at each stage. Then, for the final translation to film of thermoplastic polyimide thermally processed film Polynicotinate imagesyour. Then impose on one another conventional polyimide film "APICAL" (a product and trademark of Kanegafuchi Chemical Industry Co., Ltd.), termostatico polyimide film obtained in the result of implementation of the above processes, and a copper foil thickness of 35 μm in this order. Assembled construction roll at 300oC and velocity of 2.2 cm/min, And finally get the layered film with a layer of copper foil.

STI thermoplastic polyimide, obtained as described above, and determines that the glass transition temperature is 222oC, and the coefficient of hygroscopic equal to 1.13%. Then, in the same way as in example 1, determine the strength of raster layered film with a layer of copper foil, which is 2.0 kg/see the Results are given in table 1. Then, using electronic conductors with a capacity of 2 MeV, a layered film with a layer of copper foil is irradiated with radioactive rays in 5 MGy to check the resistance to this radiation. The results show that the resulting material is no discoloration or damage. The polyimide obtained in example 2, consists of the following repeating units represented by the General formula (2), and the molecular weight of the polyimide is about 100,000 to 150,000.

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Example 3

First carry out the copolymerization by adding 30 g of DMF, 22,7 g VAWR and 10.6 g of PMDA to the solution Polynicotinate obtained in example 1, and then obtain the solution of a copolymer of polyamidation. Next, in the same manner as in example 1, the obtained solution Polynicotinate imagesyour before obtaining a thermoplastic polyimide in the form of a film. Then, in the same way as in example 1, get hot-melt laminated square is Luigi.

In the same way as in example 1, determine the glass transition temperature and the coefficient of hygroscopic. In the result set that layered film with the copper layer has a glass transition temperature of 185oC and the coefficient of hygroscopic 1,45%. In addition, in the same way as in example 1, determine the strength of raster layered film with a layer of copper foil, which is 1.6 kg/see below, using electronic conductors with a capacity of 2 MeV, a layered film with a layer of copper foil is irradiated with radioactive rays in 5 MGy to check the resistance to such radiation. From the test results it becomes apparent that no discoloration layered film with a layer of copper foil or destruction of the material obtained. The polyimide obtained in example 3, consists of the following repeating units represented by the General formula (2):

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and molecular weight of the polyimide is about 100,000 to 150,000.

Example 4

First, 5.0 g of dianhydride of biphenol And bis-trimellitic acid (hereinafter referred to as an ESDA) and 50.0 g of DMF is mixed in a flask with a capacity of 50 ml, and the mixture is then stirred with a stirrer until complete dissolution. Regardless of the sample 8.6 g of 1,2-bis(4 - aminobenzylidene) the PP) and 260,8 g of DMF is mixed in a three-neck flask with a capacity of 500 ml, equipped with a mixer, and then the mixture was stirred in nitrogen atmosphere to dissolve the mixture. Then, 19.3 g of anhydride is 3,3',4,4'-benzophenonetetracarboxylic acid (hereinafter designated as BTDA) in solid form is added to baklazhanovyuyu flask with a capacity of 100 ml, and then BTDA is added to the solution AVRR in a three-neck flask. Then the residual ingredient BTDA, adhesively to the inner wall 100 ml flask packagenamespace type, using 5 g of DMF is reloaded into the three-neck flask. After stirring the mixed solution for about 30 minutes is added to 16.4 g of the WAR in the solid state, and the stirring continued for about 30 minutes After the addition of 21.3 g of an ESDA in the solid state and mixing for about another 30 min, the sample solution is stored in an ESDA 50-ml flask with study the actual solution viscosity in a three-neck flask. After confirmation of the achievement of the solution in the three-neck flask maximum viscosity stops the introduction of the resulting solution an ESDA. The mixed solution was stirred for 1 h, and finally, the result is a solution of polyamide acid.

In the same manner as described in example 1, the applicants received a thermoplastic polyimide in the form of a film. Then, the same conclusions and finally got the film, laminated with copper foil.

As shown in example 1, were determined as the glass transition temperature and the coefficient of hygroscopic obtained thermoplastic polyimide. It was shown that the glass transition temperature of thermoplastic polyimide equals 219oC, and the coefficient of hygroscopic - 1,33%.

In addition, the strength of raster obtained laminated copper foil film is estimated as 1.2 kg/see the Results are given in table 1. In addition, with the use of electronic wires having a capacity of 2 MeV, the irradiation of the laminated copper foil film radioactive radiation 5 MGy is determined resistance to radiation exposure. The results confirmed the absence of discoloration laminated copper foil film, and the destruction of the embedded material.

The polyimide obtained in this example 4, consists of the following repeating units represented by the General formula (1)

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Example 5

First, 5.0 g an ESDA and 50.0 g of DMF is mixed in a flask with a capacity of 50 ml, and the mixture is then stirred with a stirrer until complete dissolution. Regardless of the sample 5.7 g WAVRE and 7.4 g of 2,2-bis(4- (4-aminophenoxy) biphenyl (hereinafter about the camping stirred in a nitrogen atmosphere to dissolve the mixture. Then 8.7 g PMDA is added in the solid state baklazhanovyuyu flask with a capacity of 100 ml, and then BTDA is added to the solution WAVRE in a three-neck flask. Then the residual ingredient BTDA, adhesively to the inner surface of the wall 100 ml balaganapathy bulb, using 5 g of DMF is reloaded into the three-neck flask. After stirring the mixed solution for about 30 minutes is added to 16.4 g of the WAR in the solid state, and the stirring continued for about 30 minutes After the addition of 32.9 g of an ESDA in the solid state and mixing for about another 30 min, the sample solution is stored in an ESDA 50-ml flask with study the actual solution viscosity in a three-neck flask. After confirming that the three-neck flask reached the maximum viscosity of the solution, introducing the resulting solution TMEG stops. The mixed solution was stirred for 1 h, and finally, the result is a solution of polyamide acid.

In the same manner as described in example 1, the obtained thermoplastic polyimide in the form of a film. Then, in the same manner as described in example 1, the obtained hot-melt laminated film suitable for the insulation of the wires and, finally, the obtained laminated copper f is kopycinski obtained thermoplastic polyimide. Confirmed that the glass transition temperature of thermoplastic polyimide equals 223oC, and the coefficient of hygroscopicity of 1.28%.

Next, the strength of raster obtained laminated copper foil film, which is equal to 1.4 kg/see the Results are given in table 1. Further, with the use of electronic wires having a capacity of 2 MeV, the irradiation of the laminated copper foil film radioactive radiation 5 MGy, determined resistance to radiation exposure. The results confirmed the absence of discoloration laminated copper foil film, and the destruction of the embedded material.

The polyimide obtained in this example 5, consists of the following repeating units represented by the General formula (1)

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Comparative example 1

The basis of the examples for comparison is a thermoplastic polyimide containing BTDA and the WAR. First of 1.94 g of dianhydride 3,3',4,4'-benzophenonetetracarboxylic acid (BTDA) and 30 g of DMF are mixed in a flask with a capacity of 50 ml, and the mixture is then brought to a complete dissolution. Separately mix 51.8 g of the WAR and 310 g of DMF in a three-neck flask with a capacity of 500 ml equipped with a stirrer. Upon cooling, a mixture of water with ice and atmosphere Asy BTDA added to a solution of the WAR. Next, using 10.0 g DMF remains of BTDA with walls 100-ml flask is transferred into a three-neck flask with a capacity of 500 ml After stirring the mixture for 30 minutes, watching the viscosity of the solution in a three-neck 500-ml flask, in this three-neck 500-ml flask is gradually transferred to the solution of BTDA from a flask with a capacity of 50 ml After achieving the maximum viscosity a solution of BTDA stop. The solution is then stirred for one hour, and get finally the solution Polynicotinate. Then impose on one another conventional polyimide film "APICAL" (a product and trade name of Kanegafuchi Chemical Industry Co., Ltd.), the film is a thermoplastic polyimide obtained by the above described method, and a copper foil thickness of 35 μm in sequence, and then the components of the roll at 300oC and velocity of 2.2 cm/min And get finally the layered film with a layer of copper foil.

Next, in the same way as in example 1, determine the glass transition temperature and the coefficient of hygroscopic layered film with a layer of copper foil. The result revealed that the glass transition temperature is 238oC, and the coefficient of hygroscopic equal to 1.98%. Although check the strength of resdir the same way as in example 1, as in the layered film with a layer of copper is the water capacity of 2 MeV, the obtained laminated film with a layer of copper foil is irradiated with radioactive rays in 5 MGy to check the resistance to it. The results show that there is no discoloration of the layered film with a layer of copper foil or material failure.

Comparative example 2

Using a method identical to that described in example 1, get layered film with a layer of copper foil, replacing thermoplastic polyimide obtained by the method of the invention, a conventional adhesive based on epoxy resin "EPICOAT" 828 (product and trade name TUKA-Shell Co., Ltd.).

After analysis of the physical properties of the obtained laminated film with a layer of copper foil in the same manner as in example 1 revealed that the glass transition temperature is 178oC, and the coefficient of hygroscopic equal to 1.98%. In addition, in the same way as in example 1, check the strength of raster layered film with a layer of copper foil. However, due to the fact that the bonding process in the layered film does not occur, the results do not get. The results obtained are presented in table 1. After irradiation layered film with a layer of copper foil radioactive radiation in 5 MGy to check the resistance of the film to radiation, SL. termoplastici the polyimide represented by the General structural formula

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in which Ar1and Ar4present in General formula contain at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

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where R1, R2= H, CH3CH2CH3, phenyl,

in which Ar2and Ar6present in General formula contain at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

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in which Ar3and Ar5present in General formula 1 contain at least one organic radical selected from the group of tetravalent organic radicals having the following chemical structure:

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in which L, m, n and t are represented by formulas 1 L 15, 1 15 m, 1 n 15, t 1,

and having a molecular weight of more than 10,000.

2. Thermoplastic polyimide represented by the General structural formula 2

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in which Ar1present in General formula 2, contains at least one organic radical selected from the group of divalent organic radiolover,

in which Ar2and Ar6present in General formula 2, contain at least one organic radical selected from the group of divalent aromatic radicals having the following chemical structure:

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in which Ar5present in General formula 2, contains at least one organic radical selected from the group of tetravalent organic radicals having the following chemical structure:

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in which L and t are represented by the following formula: 1 L 15, t 1.

3. Polyamide acid represented by the General structural formula 3

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in which Ar1and Ar4present in General formula 3, contain at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

< / BR>
where R1, R2= H, CH3CH2CH3, phenyl,

in which Ar2and Ar6present in General formula 3, contain at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

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in which Ar3and Ar5present in General formula 3, the content is, has the following chemical structure:

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in which L, m, n and t are represented by the following formula: 1 L 15, 1 15 m, 1 n 15, t 1.

4. Polyamide acid represented by the General structural formula 4

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in which Ar1present in General formula 4, contains at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

< / BR>
where R1, R2= H, CH3CH2CH3, phenyl,

in which Ar2and Ar6present in General formula 4, contain at least one organic radical selected from the group of divalent organic radicals having the following chemical structure:

< / BR>
in which Ar5present in General formula 4, contains at least one organic radical selected from the group of tetravalent organic radicals having the following chemical structure:

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in which L and t are represented by the following formula: 1 L 15, t 1.

5. Hot-melt laminated film for coating a wire-containing film of polyimide on the basis of at least one acid dianhydride selected from compounds FA welding-based thermoplastic polymer, characterized in that the layer of welding agent-based thermoplastic polymer, it contains a layer of polyimide of the General formula 1 or 2 under item 1 or 2 with a softening temperature below 220oC.

Priority signs:

27.07.93 - p. 1;

25.12.92 and 27.07.93 - p. 2;

27.07.93 - p. 3;

25.12.92 and 27.07.93 - p. 4;

16.12.92 and 27.07.93 - p. 5.

 

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