Reinforcement threads and composites, having higher fire resistance

FIELD: chemistry.

SUBSTANCE: present invention relates to threads which can reinforce organic and/or inorganic materials. The threads are coated with a lubricating composition. The lubricating composition contains at least one bonding agent selected from silanes such as aminosilanes or epoxysilanes, and at least one additive capable of having an effect on the thread/matrix boundary surface(s) in order to improve fire resistance of the composite. The additive may be selected from the following: nitrates such as potassium nitrate (KNO3) and guanidine nitrate; alcohols selected from dipentaerythritol, tripentaerythritol, ethoxylated pentaerythritol, propoxylated pentaerythritol, ethoxylated/propoxylated pentaerythritol, sorbitol or derivatives thereof; phosphorus derivatives or derivatives of phosphoric acid, organophosphorus compounds, phosphates of cyclic esters, guanidine phosphate, 1,2,3-dioxaphosphorinane or ammonium pyrophosphate.

EFFECT: high fire resistance of the composite material.

15 cl

 

The present invention relates to filaments (or fibers)that can strengthen organic and/or inorganic materials, as well as to the resulting hardened products (or composites), and these reinforcing threads and these composites have improved fire resistance. The present invention relates also to compositions used for coating these fibers and the method of production of these threads.

The present invention relates in particular to the amplified glass yarns, which can be obtained by mechanical stretching at high speed (up to several tens of meters per second) of streams of molten glass flowing from the holes located at the base of the nozzle or nozzles. These threads extend in the form of filaments that before you merge them into the threads of the cover composition, called a sizing intended, in particular, to protect the filaments from abrasion, to make possible the binding threads with a hardening matrix (organic and/or inorganic material, or materials), etc.

Although glass yarns possess remarkable properties, which are detected in the received composite products, but they have a negative impact in regard to the fire resistance of these composites, making it easier in some cases the spread of fire inside of these composites. Introduced in m is trico classic substances, giving fire, do not allow at present to eliminate this effect, because the values of fire resistance to be achieved in this case, remain insufficient, in particular, they are below the level achieved in the absence of reinforcement threads.

The present invention is directed to solving this problem, and it was found that the addition of a sizing composition of the component, which in itself is not necessarily recognized flame retardant agent, but which modifies the surface of the partition matrix/fiber obtained in the composites, thus preventing ignition or accelerating self-extinguishing, improves the fire resistance of the composite, at the same time without compromising its properties (in particular, mechanical) or laying reinforcing threads.

Thus, the present invention is primarily composition, in particular, a sizing composition used for coating reinforcing fibers, in particular glass, characterized in that it contains at least one additive that can change (or modify) the surface section of the filament/matrix to improve the fire resistance of the composite material matrix/reinforcing fibers, in particular, preventing fire and/or accelerating self-extinguishing, and while maintaining the mechanical properties of the composite or laying of threads.

Delay vos is laminine and/or acceleration of fire extinguishing are the result of at least one phenomenon, taking place mainly on the surface of the partition filament/matrix and preferably leading to reduction of heat transfer on the boundary surface, in particular, because of the formation of the carbon layer, and, not wishing to be bound by any theory regarding possible modes of action, it is assumed that the additive is, for example, a donor of carbon or acts as an oxidizing agent, breaking the chains of the matrix on the boundary surface and contributing to the formation of a mesh structure, or interacting with fire-retardant agent in the matrix, etc.

The additive or additives capable of modifying the surface of the partition filament/matrix to improve the fire resistance of the composite filament/matrix (without compromising, however, the mechanical properties or laying) can be chosen in particular from:

- nitrates such as potassium nitrate (KNO3) or guanidine nitrate;

- alcohols and their derivatives such as pentaerythritol and its derivatives, in particular, dipentaerythritol, tripentaerythritol, ethoxylated pentaerythritol, propoxycarbonyl pentaerythritol, ethoxylated/propoxycarbonyl pentaerythritol or sorbitol (or D-glucit); and

derivatives of phosphorus or phosphoric acid, organophosphorus compounds, phosphates, cyclic ethers or organophosphonates such as ammonium polyphosphate, guanidine phosphate, 1,2,3-dioxaphosphinan and the and ammonium pyrophosphate,

moreover, the additive or additives are preferably selected from nitrates, such as potassium nitrate (KNO3) or guanidine nitrate (preferably nitrate is potassium nitrate), and/or alcohols (and their derivatives) type of sorbitol or derivative pentaerythritol, preferably (in particular, when the reinforcing fiber is planned to be cut) of ethoxylated pentaerythritol, propoxyethanol pentaerythritol, ethoxylated/propoxyethanol pentaerythritol and sorbitol, and particularly preferably from ethoxylated pentaerythritol and sorbitol.

Additives, selected according to the invention, typically are not part of the products, which are traditionally considered to agregates, and not have, for example, no effect on combustion, if you only enter them, in particular, in the same content in the same matrix and not on the fiber. As mentioned above, their effect is mainly on the surface of the partition matrix and threads (in particular, on the surface of the section sizing/warp and/or matrix)), and these compounds may affect, if necessary, to the specified surface of the partition matrix and/or a flame retardant in the matrix and/or with other components of the sizing.

It should be noted that the composition according to the invention is beneficial not contains red phosphorus, antimony oxide and halo is animowany compounds, since these latter, among other things, cause harm to the environment.

Preferably, the additive or additives capable of modifying the surface of the section threads/Maritsa, according to the invention can dissolve or form a dispersion or emulsion in water and/or in (the rest of) the songs. Since the composition according to the invention is generally water composition, the content of solid components of the composition in this case is preferably from 1 to 20 wt.% from the composition (i.e. the composition comprises from 80 to 99 wt.% water), in particular from 2 to 10 wt.%. In other embodiments of the composition according to the invention may not contain water or may contain other solvents.

The content of the additive or additives capable of modifying the surface of the partition matrix/fiber according to the invention is usually from 1 to 60%, preferably from 2 to 40% by weight of the solid components of the composition.

Composition (preferably a sizing) may also contain at least one agent education connection, allowing typically bind reinforcing fibers (in particular, fiberglass) with a hardening matrix. This agent education communication can be selected in particular from silanes, titanates and zirconates, and preferably selected from silanes (in particular, from aminosilanes, epoxysilane etc). The share attributed the non-agent in this case is preferably from 1 to 50 wt.%, favorably 2 to 20 wt.%, and particularly preferably from 5 to 15 wt.% from the dry extract of the composition.

The composition may also contain at least one adhesive agent (film-forming), and this tool usually affects the ability of the threads to laying (rigidity, cohesion between the filaments and so on), and the agent selected, for example, polyurethanes, epoxy resins, acrylic copolymers, polyvinyl acetate and polyolefin emulsions, and the share of the adhesive agent or agents is optionally (when they are present) from 10 to 90%, preferably from 20 to 80%, by weight of the solid komponentov composition. Preferably, the composition comprises at least one adhesive agent capable of bonding additive according to the invention with the surface of the thread to keep it on the surface section of the filament/matrix, and the beneficial agent is a polyurethane selected in particular so badly to dissolve in the matrix or not to diffuse (too much) to the surface of the partition. It could be, for example, of polyurethane, which is scheduled to sew after application of the composition on the thread (for example, during the operation of drying), and the polyurethane is samoszhimayuschimsya (in particular, containing functional groups that can be crosslinked such as isocyanate groups in the polymer is ETUI), or is mixed with a crosslinking agent (component, for example, of the order of 2-50 wt.% a mixture of polyurethane/a crosslinking agent such as polyisocyanate or polymermodified, and these cross-linking groups may blocked by a blocking agent (which can be unlocked, for example, heat treatment) such as caprolactam or the oxime of butanone.

If necessary, you can use several different adhesive agents (in particular, polyurethanes) or the same adhesive agent carrying out several functions, for example, you can use at least one adhesive agent, contributing, in particular, to achieve good mechanical properties (and/or needed to keep the additive and possibly other components on the threads, as can be seen from the preceding), and possibly at least one other bonding agent, capable of protecting and/or facilitate the laying of the reinforcement threads.

Finally, the composition according to the invention (in particular, a sizing) may contain at least one other agent (typically, up to 20 wt.% from its solid components), and the agent selected, for example, lubricants (for example, ethoxylated esters of fatty alcohol), emulsifiers or Surfactants (e.g. ethoxylated (20 moles) of stearyl alcohol), antistatic agents, phenagesic the lei, of wetting, textile agents, etc.

As already mentioned, the composition typically contains at least one solvent, in particular water. If necessary, some active ingredients may already be in solution or dispersion in a solvent when they are added to the mixture prior to forming the composition, and/or the solvent or solvents may be added to the mixture after the active components, in order to obtain the viscosity and the ratio, usually required to be applied to the threads.

The preferred sizing composition according to the invention has, for example, the following structure.

Components% weight. solid components of the composition
Organosilanols agent education communication(s)1-50
Polyurethane adhesive agent(s)10-90
KNO31-60
Grease(and)0-20

The present invention relates also to the amplifying threads (favorably to glass)coated with the above composition, and these threads can be in various forms such as continuous the main thread, cut yarn, braids, tapes, mats, etc.

The proportion of the applied composition (or loss by fire) is favorably from 0.1 to 3%, preferably from 0.2 to 1.5% by weight of the filaments.

The composition according to the invention can be applied in one or several stages on the filaments (before the formation of threads) and/or amplification of the thread. The composites obtained from these threads usually contain at least one organic material and reinforcing filaments, and at least part of the reinforcing yarns is a yarn according to the invention.

The present invention relates also to a method for production of glass strands coated with the composition according to the invention, according to which the pull (with speeds from a few meters to tens of meters per second) multiple threads of molten glass flowing from a variety of holes located at the base of one or more nozzles, in the form of one or several bundles of continuous filaments(diameter, comprising typically from 5 to 24 μm), then combine the filament in one or more threads, which are collected on a moving basis, and this method is the location on the surface filamento (during extrusion and before collecting the filaments in the thread) at least part of a sizing composition according to the invention, and if necessary, thread covered the entire composition. is th not later than the collection of threads.

Threads can be collected in different ways; in particular, they can be cut, or after the formation of the mechanism serving to extrude or subsequent operations, as well as they can gather around a rotating basis (for more wrappings such as roving or rovings, ears, cakes etc) or also be distributed on moving conveyors (for example, for the formation of mats or films). If necessary, the threads can be dried (e.g., infrared radiation, hot air, high frequency radiation, and so on), as the water may worsen a good adhesion between the fibers and harden the material, and/or can be subjected to heat treatment (at temperatures that can range, for example, up to 200°C), so that if it was possible to conduct the polymerization and/or the stitching of all or part of sizing.

Note that under the "glass" in the present invention refers to thread-based glass, it not only has threads formed entirely of glass filaments, but also the threads formed of glass filaments and organic filaments, in particular, thermoplastic filaments. In this latter case, when extruding glass filaments simultaneously ekstragiruyut and capture organic filaments (or simultaneously pulling the organic filaments, taken, for example, with the wrappings), when the eating of the trajectory, which are glass filaments and organic filament (or filaments), converge to each other before these filaments are connected in at least one composite yarn seized mechanically.

The object of the present invention is also a composite material containing at least one organic material and at least those threads, which is defined above.

Organic material is favorably thermoplastic material is selected, in particular, polyamides, thermoplastic polyesters such as polybutylene terephthalate (pbtf was honored with) or polyethylene terephthalate (PET), polyolefins, Polyacetals, polycarbonates, etc.

In the composition form of the matrix used to produce a composite material by molding, may also include (in addition to a hardening of the matrix and reinforcement threads) at least one fire-retardant agent (for example, cyanuric such as cyanurate melamine, and/or organophosphorus agent, as the melamine pyrophosphate, and/or may include fillers, in particular, to improve the mechanical strength and/or to stabilize the dimensions of the composite (for example, mineral fillers of the type of mica, talc and so on).

The composition is moldable matrix according to the invention can favorably have the following structure:

from 20 to 95 wt.% the organic is their substances;

from 1 to 60%, in particular from 5 to 40%, preferably from 10 to 30% (by weight) of at least one flame retardant funds;

from 1 to 60 wt.%, preferably from 10 to 40 wt.%, oily fibers according to the invention; and

- from 0 to 50 wt.% inorganic/mineral fillers.

The following example illustrates the present invention, however, does not limit its scope.

Preparing a sizing composition having the following composition by mixing in water in its different components.

Component% weight. solid components of the composition
Aminosilane manufactured by the company "GE Silicone under the name And 110010
Polyurethane with cross-linking agent, manufactured by Bayer under the name of Baybond PU130 (input in the form of an aqueous dispersion with a dry extract content of 30 wt.%)67
KNO320
Polyoxyethylene (20 moles) of stearyl alcohol3

Received one or more glass strands by pulling the filaments of molten glass from the die and the sizing of the above composition is bosilca to connect the filaments in the strands.

The obtained filament was then immediately cut under villeroi, then cooked capable of forming a composition having the following composition.

Componentwt.%
The matrix consisting of polyamide 6 (Ultramid B3, manufactured by BASF)50
Fire-retardant agent melamine pyrophosphate (manufactured Buddenheim called Budit 311 MPP)25
Cut greasy fiber25

Then, on the basis of the above-described form of the composition, obtained composite molded product by extrusion and then injection molding.

Then there was each of the following tests: test for Flammability with limited oxygen content (LOI) (according to ISO 4589-2/1996F), testing with an infrared emitter (according to the standard NFP 92-505) and test cone calorimeter (ASTM E1354). The experiment is carried out on samples made in accordance with this example (below results "fiber KNO3") and the comparative samples, obtained by replacing the filaments of this example, the threads that were samakovlis the same composition, but without KNO 3(below is the results of "standard threads"). The results are shown in the following table.

TestThe standard threadThread with N
The limiting oxygen index, ISO 4589-2/1996F%25,628,2
IR emitter, NFP92-505Time to ignition (s)30170
The average time to ignition (s)4118
Cone calorimeter, ASTM E1354Peak HRR (kW/m2)306203

The LOI test is to determine the concentration of oxygen in a mixture of oxygen/nitrogen, which allows you to support combustion of the material within a specified period of time (180 seconds) or a specified length (50 mm). The results of this test show that in the case of products according to the invention harder to sustain combustion. Also, in the case of tests with infrared emitter seems I have owned, that takes much more time to have ignited the products according to the invention, and that they stew is also much faster. Finally, the test cone calorimeter shows that the energy released during combustion, much less in the case of products according to the invention.

In addition, the following table shows that these improvements are not due to deterioration of the mechanical properties of the composites obtained values of mechanical strength are of the same order as in the use of filaments of example and comparative threads (the values of the limit of the tensile strength obtained according to ISO 527-2, and the values of impact strength in the trials by Sharlee according to ISO 179-1).

Thread comparisonThread with KNO3
Ultimate tensile strength (MPa)149,4to 150.1
Impact test on Charpy (kJ/m2)78,678,4

Amplification strands and composite products made according to the invention can be used in various applications, for example, in the field of electric connected the th, upon receipt of electric and electronic components, etc.

1. Amplification strands coated with a sizing composition, wherein the sizing composition comprises at least one agent of education selected, in particular silanes, such as aminosilane or epoxysilane, and at least one additive can affect the surface and section of the strands/matrix to improve the fire resistance of the composite, and an additive selected from:
- nitrates such as potassium nitrate (KNO3) or guanidine nitrate;
- alcohols selected from dipentaerythritol, tripentaerythritol, ethoxylated pentaerythritol, propoxyethanol pentaerythritol, ethoxylated/propoxyethanol pentaerythritol, sorbitol, or derivatives thereof;
derivatives of phosphorus or a derivative of phosphoric acid, organophosphorus compounds, phosphates, cyclic ethers, guanidine phosphate, 1,2,3-dioxaphosphorinanes or ammonium pyrophosphate.

2. Reinforcing filament according to claim 1, characterized in that the sizing composition does not contain red phosphorus, antimony oxide and halogenated compounds.

3. Reinforcing filament according to claim 1 or 2, characterized in that the sizing composition comprises at least one bonding agent selected from polyurethanes, epoxy resins, acrylic copolymers, polyvinyl acetate and poly is latinovich emulsions.

4. Reinforcing filament according to claim 1 or 2, characterized in that the sizing composition comprises at least one adhesive agent, such as polyurethane, is capable of bonding additive to the surface of the filaments, so that it remains on the surface of the partition filament/matrix.

5. Reinforcing filament according to claim 1 or 2, characterized in that the sizing composition comprises at least two different polyurethane adhesive agent.

6. Reinforcing filament according to claim 1 or 2, characterized in that the sizing composition has the following composition:

Componentswt.% solid components of the composition
Organosilane(s)1-50
Polyurethane(s)10-90
KNO31-60
Grease(and)0-20

7. The method of producing glass yarns according to which pull many threads of molten glass flowing from a variety of holes located at the base of one or more nozzles, in the form of one or several bundles of continuous filaments, and then connect the filaments in one or more threads that collect on driving the I basis moreover, this method consists of applying to the surface of the filaments during extrusion and prior to the merger of the filaments into one or more filaments of at least part of a sizing composition, and the threads if necessary, cover the entire composition no later than the collection of fibers, characterized in that the sizing composition comprises at least one agent of education selected, in particular silanes, such as aminosilane or epoxysilane, and at least one additive can affect the surface and section of the strands/matrix to improve the fire resistance of the composite, and an additive selected from:
- nitrates such as potassium nitrate (KNO3) or guanidine nitrate;
- alcohols selected from dipentaerythritol, tripentaerythritol, ethoxylated pentaerythritol, propoxyethanol pentaerythritol, ethoxylated/propoxyethanol pentaerythritol, sorbitol, or derivatives thereof;
derivatives of phosphorus or a derivative of phosphoric acid, organophosphorus compounds, phosphates, cyclic ethers, guanidine phosphate, 1,2,3-dioxaphosphorinanes or ammonium pyrophosphate.

8. The method according to claim 7, characterized in that the sizing composition does not contain red phosphorus, antimony oxide and halogenated compounds.

9. The method according to claim 7 or 8, characterized in that the sizing composition sod is RIT at least one adhesive agent, selected from polyurethanes, epoxy resins, acrylic copolymers, polyvinyl acetate and polyolefin emulsions.

10. The method according to claim 7 or 8, characterized in that the sizing composition comprises at least one adhesive agent, such as polyurethane, is capable of bonding additive to the surface of the filaments, so that it remains on the surface of the partition filament/matrix.

11. The method according to claim 7 or 8, characterized in that the sizing composition comprises at least two different polyurethane adhesive agent.

12. The method according to claim 7 or 8, characterized in that the sizing composition has the following composition:

Componentswt.% solid components of the composition
Organosilane(s)1-50
Polyurethane(s)10-90
KNO31-60
Grease(and)0-20

13. Moldable composition comprising at least one of the filaments, as they are defined in one of claims 1 to 6.

14. Moldable composition according to item 13, characterized in that it contains at least one fire-retardant agent and/or at least one fill the ü.

15. Moldable composition according to one of PP-14, characterized in that it has the following composition:
from 20 to 95 wt.% organic substances;
from 1 to 60%, in particular from 5 to 40%, and preferably from 10 to 30 wt.% at least one fire retardant tools;
from 1 to 60 wt.%, preferably from 10 to 40 wt.% oily fibers according to the invention; and
- from 0 to 50 wt.% inorganic/mineral fillers.



 

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15 cl

FIELD: chemistry.

SUBSTANCE: radiation-curable primary coating composition contains an oligomer, a diluent monomer; a photoinitiator; an antioxidant; and an adhesion promoter; wherein said oligomer is the reaction product of: a hydroxyethyl acrylate; an aromatic isocyanate; an aliphatic isocyanate; a polyol; a catalyst; and an inhibitor. Said oligomer has number-average molecular weight ranging from at least 4000 g/mol to less than or equal to 15000 g/mol; and wherein said catalyst is selected from a group comprising dibutyl tin dilaurate; metal carboxylates, sulphonic acids; catalysts based on amines or organic bases, zirconium and titanium alkoxides and ionic liquid salts of phosphonium, imidazolium and pyridinium.

EFFECT: obtaining a hardened film of said radiation-curable primary coating composition.

6 cl

FIELD: chemistry.

SUBSTANCE: radiation-curable secondary coating composition contains a mixture of secondary coating oligomers which is mixed with a first diluent monomer; a second diluent monomer; an optional third diluent monomer; an antioxidant; a first photoinitiator; a second photoinitiator; and, optionally, a slide-enhancing additive or a mixture of slide-enhancing additives; wherein said mixture of secondary coating oligomers contains: α) Omega-oligomer; and β) Upsilon-oligomer; wherein said Omega-oligomer is synthesised from reaction of α1) hydroxyl-containing (meth)acrylate; α2) isocynate; α3) polyether polyol; and α4) tripropylene glycol; in the presence of α5) a polymerisation inhibitor; and α6) a catalyst; to obtain an Omega-oligomer; wherein said catalyst is selected from a group comprising copper naphthenate, cobalt naphthenate, zinc naphthenate, triethylamine, triethylenediamine, 2-methyltriethylenediamine, dibutyl tin dilaurate, metal carboxylates, sulphonic acids, catalysts based on amines or organic bases, zirconium and titanium alkoxides and ionic liquid salts of phosphonium, imidazolium and pyridinium; and wherein said Upsilon-oligomer is epoxy diacrylate. The method of applying the coating onto an optical fibre involves operation of a glass drawing column to obtain optical glass fibre; applying a radiation-curable primary coating composition onto said optical glass fibre; optional exposure of said radiation-curable primary coating composition to radiation in order to cure said coating; applying a radiation-curable secondary coating composition in paragraph 1 onto said optical glass fibre; and exposing said radiation-curable secondary coating composition to radiation in order to said coating.

EFFECT: obtaining optical fibre and a conductor having a cured secondary coating.

6 cl

FIELD: chemistry.

SUBSTANCE: radiation curable primary coating composition contains at least one urethane-(meth)acrylate functional oligomer and a photoinitiator, wherein the urethane-(meth)acrylate functional oligomer is a product of reaction of hydroxyethyl acrylate, a mixture of 2,4-toluene diisocyanate and 2,6-toluene diisocyanate, isophorone diisocyanate and polyether polyol in the presence of a catalyst and an inhibitor, where the urethane-(meth)acrylate functional oligomer contains (meth)acrylate groups, at least one polyol backbone chain and urethane groups, where 15% or more of the urethane groups are derivatives of one of 2,4- and 2,6-toluene diisocyanate or both, where at least 15% of the urethane groups are derivatives of isophorone diisocyanate, and where said urethane-(meth)acrylate functional oligomer has number-average molecular weight from at least 4000 g/mol to at least 15000 g/mol; and where the cured film of the radiation curable primary coating composition has equilibrium modulus of elasticity, measured as indicated in the description, which is equal to at least 1.2 MPa. The invention also relates to a method of coating glass optical fibre, involving (a) using a glass drawing column to obtain glass optical fibre, preferably at linear velocity between 750 m/min and 2100 m/min; (b) applying the radiation curable primary coating composition onto the surface of the optical fibre; and (c) optional exposure to radiation to cure said radiation curable primary coating composition. The cured primary coating composition on the optical fibre and conductor has the following properties after initial curing and after one month at 85°C and 85% relative humidity:A) % RAU from 84% to 99%; B) in-situ modulus of elasticity between 0.15 MPa and 0.60 MPa; and C) Tc of the tube -25°C to - 55°C.

EFFECT: improved coating characteristics.

13 cl, 2 tbl

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