The laminate of flat porous substrate with a coating and method for its manufacture

 

(57) Abstract:

Proposed a laminate of flat porous substrate with a coating comprising an adhesive powder, applied with the formation of non-adhesive at room temperature, the stable storage intermediate product, and a second substrate connected to the planar porous substrate at elevated temperature and pressure, and is coated on a porous substrate, the coating contains a combination of components: a thermoplastic polymer, at least one solid at room temperature epoxy resin and optionally at least one solid at room temperature, the prepolymer of epoxy resins and polyamines. In the production method of a laminate of flat porous substrate coating is fixed on the first substrate at the first elevated temperature by melting of the components. The connection of the substrates occurs by chemical crosslinking or by subsequent crosslinking of the components of the powder and subsequent cooling. 2 C. and 20 C.p. f-crystals.

The technical field to which the invention relates

The invention relates to a flat, closed or porous substrate with the coating and spacecam in the first stage, the adhesive powder is applied to the first substrate and at room temperature get nakleivalis, stable storage intermediate product, and the second stage is the connection of the first substrate with the second substrate at an elevated temperature and an elevated pressure to obtain a laminate.

Art

Known adhesive powder-based thermoplastic, which can be deposited on the bonding substrate and to form nakleivalis, stable storage intermediate product. The connection with the second substrate occurs when heated under pressure, and curing the adhesive layer is purely physical way when cooled. The disadvantage of this fusible and heat sealable adhesive is that the temperature stability of the formed adhesive layer is limited by the melting range of the used thermoplastic. In addition, some of the copolymers due to the low melting temperature and associated minor ability to crystallization reduces the resistance to hydrolysis and solvents.

Much better properties in terms of strength of adhesion, resistance to hydrolysis and the action of solvents can be achieved using adhesive materials on the basis of epoxides. One is in, subjected to tension when bending. Because they are two-component systems, they share another disadvantage, namely, that they should always be mixed in liquid or pasty form directly before gluing and then apply to join (at the bonding part). As a consequence, the possibility of storing or shipping materials, covered with adhesive. As a one-component system should be maintained mainly at low temperatures to maintain their suitability for use, or handle only at temperatures above 150oFor cross-linking (stitching). Sometimes the reaction proceeds sufficiently long, and the joined substrates are subjected to high thermal loads.

In U.S. patent 4117038 offered bystrootverdevayuschey adhesive powder based on epoxy resin, which can be applied to the porous substrate and to produce a laminate, in particular, for the production of skis. But in the method of manufacturing a laminate according to this patent requires pre-treatment of the porous substrate prior to applying the adhesive powder, and apply the adhesive powder is required before one pressed into the substrate, what complicates the process of manufacture. In addition, obtained, after drying and curing the above-mentioned solution or pressing, fragile coating has a bad connection with the substrate and this substrate with the coating is not adapted for convenient storage (e.g., twisted) and transportation, it is almost possible to use only within a particular production. In addition, the proposed in this patent, the adhesive based on epoxy resin does not have a sufficiently high elasticity, for example, required for winding the coil porous substrate coated with a coating of adhesive powder.

The invention

The objective of the invention is to provide a flat, closed or porous substrate with a coating and method thereof using the adhesive powder, which can be deposited on the first substrate, thus there is a strong connection with the substrate at room temperature, which is stable during storage. This is not bounding at room temperature and stable storage intermediate product must stick together with the second substrate as possible at a lower temperature and bottom of the I by creating adhesive powder, representing a combination of the following component parts. The powder consists of a thermoplastic polymer, the proportion of which is from 25 to 95 wt.%, and at least one solid at room temperature epoxy resin, the proportion of which is from 5 to 75 wt.%, and optionally at least one solid at room temperature, the prepolymer of epoxy resins and polyamines, which accounts for no more than 25 wt.%. In the first stage, when applying the adhesive powder on the first substrate occurs mainly physical binding of adhesive powder with the substrate, while the second stage is a mix of both substrates by chemical means through the formation of cross-linkages (linkage) between the components of the adhesive powder and subsequent cooling. A mixture of selected compounds allows to obtain nakleivalis, stable during storage substrate with an adhesive layer, which is deposited on the substrate at the first stage and connected with the substrate due to physical forces. After cooling, the adhesive layer remains potentially reactive. In the process of applying to the second substrate at a higher temperature compared to the process is the resulting product has a higher resistance to high temperature, as well as to the effects of gidroliznaya agents and solvents, as compared with the pure thermoplastic adhesives, and, in addition, has a higher elasticity compared to products containing adhesives based on epoxy resins. The reason for this is the crosslinking of the polymer with the epoxy resin. In addition, it was unexpectedly found that the crosslinking components begins at significantly lower temperatures. Depending on the composition of the adhesive powder, you can ensure that the stitching is already at 90oC. in Addition, the crosslinking reaction occurs within a very short time.

The proportion of thermoplastic polymer can vary over a wide range, preferably in the range of from 50 to 90 wt.%. The amount of epoxy resin is substantially less and is preferably from 10 to 50 wt.%. In the case of prepolymer its content is not more than 25 wt.%.

Suitable thermoplastic polymers include low-melting polyamide, complex, polyester, polyurethane and/or a vinyl copolymer with functional side groups comprising carboxy-, amino-, amido - and angiography. thermoplastic polymer may also be a mixture of polymers of nikoplai, including carboxy-, amino-, amido - and angiography. When this polymer is produced from a linear or branched monomers. The polyamide can be obtained from one or more of the following monomers:

- at least one at least bifunctional carboxylic acid,

- at least one at least bifunctional amine,

- at least one-aminocarbonyl acid,

at least one lactam.

Complex polyester can be obtained from one or more of the following monomers:

- at least one at least bifunctional carboxylic acid,

- at least one at least bifunctional alcohol,

- at least one-hydroxycarbonate acid,

at least one lactone.

Polyurethane can be obtained from diisocyanates, polyols and diols.

Epoxy resin that is solid at room temperature, preferably is the reaction product of epichlorohydrin with bisphenol a and/or the reaction product of epichlorohydrin with bisphenol f Epoxy resin may also be a multifunctional epoxide. For example, you can use epoxy novolak.

Solid at room is the basis of bisphenol a and polyamine and/or reaction products of epoxy resins based on bisphenol F and polyamine. Perhaps there prepolymer of epoxy resins and polyaminoamide based on polyamines and dimeric fatty acids.

Depending on the purpose and type of substrate to one possible embodiment of the invention is the mixing of adhesive powder with other additives. In this case, as additives should take into account low-melting resins and/or waxes with a melting point of less than 100oWith, preferably below 90oWith, and/or dyes and/or mineral and/or organic fillers. For example, as additives can be used in chemical products under the following trademarks: "LIGA STEARIN F, GESP. 10-12" (represents a saturated aliphatic monocellate with unbranched chain, the main part is palmitic and stearic acid; supplied by the company Peter Greven Fett-Chemie GMBH & CO KG, Germany); "LOROL WITH 18" (component - sterilely alcohol, octadecanol-1; supplied by the company BRENNTAG Chemiepartner GmbH, Germany); "LIGA Glycerin 99,5" (technological additive for plastics-based glycerin, supplied by the company Peter Greven Fett-Chemie GMBH & CO KG); "Aerosil R 972" (filler, the component parts of which are silane, the reaction products of dichlorodimethyl dioxide to the tee in the directories mentioned above firms. The proportion of such additives generally should not exceed 10 wt.%. The use of low-melting resins and/or waxes should primarily be taken into account when applying on the first substrate should be possible at lower temperatures. Dyes affect staining. Metal fillers affect the conductivity. Their share may be higher. Despite the special properties of low-melting resins or waxes, has is the fact that thermoplastic polymer or epoxy resin has a first melting point that is less than 130oWith, preferably less than 100oC and the softening temperature is from 50 to 90oC. this ensures the following: in the process of applying to the first substrate, the connection with the substrate occurs only due to the melting of the surface of thermoplastic polymer or epoxy resin, while the other components are not melted. Therefore, the melting point of the other or both of the other components must be higher than the first melting temperature thermoplastic polymer or epoxy resins. However, it turned out that to achieve the UD is considerably higher than the first melting temperature. Thus, using such an epoxy resin, a melting point of less than 130oWith, preferably less than 100oC. In this regard, it is essential the fact that the energy consumption for bonding both substrates is possible a small amount.

The temperature of the deposition process, in which the powder is deposited on a substrate, typically greater than 5 to 10oWith the melting point of the component with the lowest melting temperature. As mentioned above, it is also possible that the adhesive powder is fixed on the first substrate at the first elevated temperature due to melting additives. In this case, the binding of adhesive powder with the first substrate occurs only physical way. Chemical crosslinking occurs only when there is binding of both substrates to each other at a second elevated temperature, for example by hot pressing. This method is also characterized by stitching the main components, and thus receive a product with a higher stability and flexibility.

It should be noted that for the application of adhesive powders on the substrate or substrates are obtained is heat, for example, you can perform the coating and bonding in the high-frequency field, first of all, if the adhesive contains metal powder fillers.

In order to provide a uniform layer of adhesive on the substrate, the size of the granules of adhesive powder should be less than 200 microns, preferably less than 100 microns.

There is also a variant embodiment of the invention, in which the first stage to the second substrate also put adhesive powder, which allows to carry out the bonding process during the deposition of the layers.

Information confirming the possibility of carrying out the invention

Example 1.

In a vessel with a stirrer to prepare a powder mixture of thermoplastic is a polyamide, epoxy resin, prepolymer based polyamine and epoxy resin, wax and amorphous silicon dioxide. The mass fraction of these components are 64,6%, 27,6%, 5,3%, 2,0%, 0,5% respectively. As polyamide choose a product with the trade name Platamid H RA (represents an aliphatic high molecular weight copolymer based on polyamide; comes in powder form by the company ATOFINA Deutschland GmbH, Germany), and as the epoxy resin is a product under the name the products can be found in the directories mentioned above firms. Before mechanical mixing of the components of the powder mixture separately crushed to grain size less than 100 microns. Thus obtained mixture is stirred usual method with water and components of the paste comprising a dispersant, a solvent and a thickener to form a paste and brush applied on one side of the nonwoven material. Then dried at a temperature of 95oC. non-Woven material coated with an adhesive powder is characterized by good storage stability. Wound on the reel strips of nonwoven material is not glued to each other with adhesive powder is firmly glued to the top surface of the nonwoven material.

The obtained non-woven material is placed on wool material and both materials are subjected to processing under pressure and heat in the press of continuous operation. The temperature of extrusion is 120oC, pressure 3 bar and the processing time of 30 sec. Thus obtained laminate is extremely stable, which corresponds to the objectives of the invention.

Example 2.

Similarly, the obtained powder containing 62.5 wt.% polyamide, with 32.5 wt.% epoxy resin Epikote 1055 (solid the asty with 1 wt.% silicon oxide as an auxiliary agent and water, as well as with components of the paste. The paste should be applied on the nonwoven material at room temperature and dried in a furnace of continuous operation at 105oC. non-Woven material has good stability during storage. The process of applying layers is carried out at a temperature of extrusion, equal to 130oC. the resulting laminate is characterized by high temperature resistance and resistance to solvents.

1. Laminate, consisting of a flat porous substrate with a coating comprising an adhesive powder, applied with the formation of non-adhesive at room temperature, the stable storage intermediate product, and a second substrate connected to the planar porous substrate, wherein the planar porous substrate and the second substrate are connected at elevated temperature and pressure, and is coated on a porous substrate adhesive powder contains a combination of the following components, wt.% on the composition of the adhesive powder: low-melting polyamide complex polyester and/or polyurethane 25 - 95, at least one solid at room temperature epoxy resin 5 to 75, and optionally at least one solid at room temperature, the prepolymer of epoxied, a complex of the polyester and/or polyurethane is 50 to 90 wt.%, share at least one solid at room temperature epoxy resin is 10 to 50 wt.% and share at least one solid at room temperature, the prepolymer of epoxy resins and polyamines is not more than 25 wt.%.

3. Laminate under item 1 or 2, characterized in that as the low-melting polyamides, polyesters and/or polyurethanes it contains a mixture of polymers.

4. The laminate according to any one of paragraphs.1-3, characterized in that the low-melting polyamide, complex polyester and/or polyurethane derived from a linear or branched monomers.

5. The laminate according to any one of paragraphs.1-4, characterized in that as the low-melting polyamides, polyesters and/or polyurethanes it contains a polyamide derived from at least one of the monomers represented by at least one at least difunctional carboxylic acid, at least one at least difunctional an amine, at least one aminocarbonyl acid, at least one lactam.

6. The laminate according to any one of paragraphs.1-4, characterized in that as the low-melting polyamides, polyesters and/or polyure the necks least one at least difunctional carboxylic acid, at least one at least difunctional alcohol, at least one hydroxycarbonic acid, at least one lactone.

7. The laminate according to any one of paragraphs.1-4, characterized in that as the low-melting polyamides, polyesters and/or polyurethanes it contains a polyurethane derived from diisocyanates, polyols and diols.

8. The laminate according to any one of paragraphs.1-7, characterized in that the solid at a room temperature epoxy resin contains the reaction products of epichlorohydrin with bisphenol a, and/or the reaction products of epichlorohydrin with bisphenol F, and/or the reaction products of epichlorohydrin with novolak.

9. The laminate according to any one of paragraphs.1-7, characterized in that the solid at a room temperature epoxy resin contains a polyfunctional epoxides.

10. The laminate according to any one of paragraphs.1-9, characterized in that the solid at room temperature, the prepolymer of epoxy resins and polyamines contains the reaction products of epoxy resins based on bisphenol a and polyamines and/or reaction products of epoxy resins based on bisphenol F and polyamines.

11. The laminate according to any one of paragraphs.1-9, characterized in that the solid at room temperature, the prepolymer obtained from aboubou of PP.1-11, characterized in that the adhesive powder additionally contains other additives.

13. Laminate under item 12, characterized in that the additives it contains low-melting resins and/or waxes with a melting temperature of less than 100C, preferably less than 90, and/or dyes and/or mineral and/or organic fillers.

14. Laminate under item 11 or 12, characterized in that the proportion of all additives is not more than 10 wt.%.

15. Laminate under item 11 or 13, characterized in that the additives it contains metallic fillers.

16. The laminate according to any one of paragraphs.1-11, characterized in that the low-melting polyamide, complex polyester and/or polyurethane, or a component of at least one solid at room temperature epoxy resin has a first melting temperature than the melting temperature of the other two components and component less than 130C, preferably less than 100C, and the softening temperature of from 50 to 90.

17. Laminate under item 16, characterized in that the higher the second melting temperature, respectively, the other two components is less than 130C, preferably 100 C.

18. A method of manufacturing a laminate sing temperature by melting of the components mentioned adhesive powder, then the obtained intermediate product with a coating combined with the second substrate at a second elevated temperature, initiating chemical crosslinking, to form a laminate.

19. The method according to p. 18, characterized in that the connection of the intermediate product fixed on the floor with the second substrate is carried out by hot pressing.

20. The method according to p. 18 or 19, characterized in that the constituent components of the adhesive powder is selected with a granule size of less than 200 microns, preferably less than 100 microns.

21. The method according to any of paragraphs.18-20, characterized in that before connecting to the second substrate also put a coating of the specified components of the adhesive powder.

22. The method according to any of paragraphs.18-21, characterized in that the said coating is applied using a high-frequency field.

 

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1 ex

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