Polymer binding agent for covers prone to swelling during heating

FIELD: copolymers meant for usage in polymer binding agents for covers prone to swelling during heating.

SUBSTANCE: copolymer is described for usage in binding agent or as polymer binding agent in covers prone to swelling during heating, including a mixture of Newton copolymer and network copolymer, selected from a group including thixotropic and pseudo-plastic copolymers, while aforementioned Newton and network copolymers consist of links of substituted styrene and substituted acrylate and contain links of at least p-methylstyrene and 2-ethylhexylacrylate, with grammolecule ratio of p-methylstyrene and 2-ethylhexylacrylate ranging from 100/0 to 50/50. Also described is the cover prone to swelling during heating and method for producing the same, which cover includes polymer binding agent, foam-forming substances, carbon-forming substances and other normally used admixtures, featuring aforementioned copolymer as polymer binding agent.

EFFECT: optimized creation of coal and improved isolating properties of cover.

3 cl, 2 tbl, 8 dwg, 4 ex

 

The present invention relates to copolymers intended for use in a polymeric binder or polymeric binder for flame retardants, more specifically, the intumescent when heated coatings, characterized by excellent performance in relation to fire resistance.

The intumescent composition when heated coatings are well known state of the art. An outstanding characteristic of swelling upon heating of the coatings is that they can be applied to substrates such as metal, wood, plastic, graphite and other materials, in the form of a coating, characterized by a relatively low film thickness. When exposed to fire, heat or flame swelling through the floor to expand in thickness, creating an insulating layer of coal and expanded coal.

The most commonly used intumescent when heated coatings contain four major components, sometimes referred to as "reactive pigments", dispersed in a matrix binder. Reactive pigments include

(1) inorganic acid or a material which generates acid at temperatures in the range from 100 to 250°such as, for example, ammonium polyphosphate, which generates phosphate to the slot;

(2) a carbon source, such as a material containing a few atoms of hydrogen, carbon-rich, also called hydrate of carbon, such as pentaerythritol or dipentaerythritol;

(3) an organic amine or amide, such as, for example, melamine; and optional

(4) halogenated material, which upon decomposition releases gaseous chloride-hydrogen acid.

The main mechanism of expansion when heated presumably involves the formation of carbonized coal in the reaction of dehydration formed between an acid and a material containing multiple replaceable hydrogen atoms. In the formation of coal can participate Amin, but first and foremost it is described as a foaming agent for the formation of the insulating foamed carbon. Since the insulating coal stops the spread of fire and remains on the substrate under conditions of a serious fire, it provides superior fire protection and thermal protection in comparison with coatings that are related to non-flammable type.

Numerous patents and publications described swelling upon heating of the composition containing one or more polymeric materials in combination with a phosphate-containing materials and carbonization or forming carbon materials.

In the patent EP 090206 intumescent composition when heated coatings may contain as a film-forming binder vinyltoluene/acrylate copolymers or styrene/acrylate polymers.

In the patent US 3654190 swelling when heated floor contains solid vinyltoluene/butadiene copolymer, associated with chlorinated natural rubber, acts as formers of coal.

In the patent EP 0342001 polymeric binder for intumescent when heated coating includes a copolymer formed from the first monomer, the vast number and the second monomer in small numbers, in fact the second monomer is thermally unstable co monomer, which is preferably a Monomeric aldehyde, such as acrolein.

In international patent WP 01/05886 polymer binder in the form of an emulsion plays the role of the foaming agent when the composition allow to dry; polymeric binder may be a styrene/acrylate copolymer.

Paint industry is in search of a fire-retardant coating that will not only satisfy the requirements for fire protection, but which also would be desirable coating properties. Reactive pigments used in the composition of the intumescent through the floor, by themselves, insufficient to provide the desired coating properties. For example, the intumescent when heated floor should ensure that all operational features, the istics of, expected from commonly used coating, plus the additional benefit from the availability of fire protection. Introduction as properties of fire resistance and good properties of the coating in a single system in a simple way does not work. Combinations of additives, such as additives, components of the intumescent composition when heated coating, often as a result can produce a composition having as poor coating properties, and poor flame retardant properties.

It was found that for the functioning of swelling upon heating of the coating are critical chemical and physical properties of the binder. On the one hand, the binder should not soften or melt excessively quickly in order to make possible the formation of a stable coal. On the other hand, the viscosity of the binder is correlated with the diffusion and formation of coal.

So for swelling during heating of the coatings, it is desirable to provide a polymeric binder, which could reduce the spread of flame on the early stages of a fire and which has made its contribution to the improvement of education and coal expansion when heated at a late stage of fire.

It was shown that the combination of the linear polymer and crosslinked polymer as a binder for intumescent when heated coating makes possible optimization is their education coal and improve the insulating properties of the coatings.

Moreover, the inventors have found that the more the copolymer will contain styrene, the greater the degree of interaction with phosphorus will be negative. In contrast, the more the copolymer will contain p-methylstyrene (PMS), the greater the degree of interaction with phosphorus will be positive, thereby providing a good expansion when heated.

They also found that the swelling properties when heated compositions corresponding to the invention correlate with the ability of the copolymer to react with phosphorus and with the presence of p-methylstyrene (PMS) and 2-ethylhexyl acrylate (EHA).

In accordance with this invention provides a copolymer designed for use in a polymeric binder or polymeric binder in swelling when heated, the coating comprising a mixture of Newtonian copolymer and reticulated copolymer, these Newtonian and net copolymers consist of chains of substituted styrene and substituted acrylate and include at least parts of p-methylstyrene (PMS) and 2-ethylhexyl acrylate (EHA).

The invention also provides in another aspect of swelling when heated, fire-retardant coating containing the above-mentioned polymer binder, and a method of obtaining such coverage.

Net SOP the materials chosen in the group, including thixotropic pseudoplastic-type copolymers and copolymers.

The value adopted in the present invention, the Newtonian copolymers denote copolymers, which give the profile Newtonian viscosity when dissolved in the solvent, i.e. the viscosity is independent of shear; thixotropic copolymers denote copolymers, giving solutions in the solvent reduces the viscosity at shear, returning to its original condition when standing in the presence of a time-dependent, pseudoplastic-type copolymers are copolymers which give the solution a viscosity reducing shear, when dissolved in a solvent.

It was found that the ratio of PMS and AGE should be in the range of from 100/0 to 50/50, preferably to be equal to 90/10, preferably 80/20, and more preferably 75/25.

The copolymers used as the polymeric binder, corresponding to the invention can additionally include links of other substituted styrene, such p-tert-butylstyrene (PCBS), and/or other substituted acrylates, such isobutylacetate (IBMA).

Examples of suitable Newtonian copolymers include Pliolite VTAC-L, Pliolite VTAC-H, Plioway ECH, Plioway Ultra 200, Plioway EC1, all trademarks of the company ELIOKEM.

Examples of suitable mesh copolymers include Pliolite AC3H, Plioway ECL, Plioway Utra G20, Plioway EC-T, all trademarks of the company ELIOKEM.

Newtonian and net copolymers receive as a result of polymerization, while the polymerization is conducted in bulk, in solution, in suspension or in emulsion. The best way is to obtain in the conventional emulsion polymerization.

After that, the composition of the polymeric binder can be by conventional techniques, such as, for example, mixing with commonly used systems reactive pigments, dispersing agents, plasticizers, defoamers, thickeners, chlorinated paraffin solvents and other additives commonly used for this type of desirable swelling when heated coatings (waxes, fillers, fibers, chemicals, preventing deposition and the like).

In accordance with the invention, the best method of obtaining mentioned polymeric binder includes a step (a) dissolving the Newtonian and/or reticulated copolymers in solvent or in water, (b) optionally adding a chlorinated paraffin, (C) homogenizing the mixture and add supplements.

Swelling during heating of the coating corresponding to the invention, preferably contain as a foaming agent ammonium salt of phosphoric acid and/or polyphosphonate, more preferably ammonium polyphosphate.

Intumescent coating corresponding to the invention preferably contain carbohydrate as uglerodsesola substances, preferably pentaerythritol, dipentaerythritol, tripentaerythritol and/or polycondensate pentaerythritol.

Swelling during heating of the coating corresponding to the invention may contain halogen or may not contain halogen.

Swelling during heating of the coating corresponding to the invention, used in the form of material applied with a brush, applied by spray or applied by roller coating, designed to protect a variety of surfaces, preferably steel, wood, electrical cables and pipes.

Swelling during heating of the coating corresponding to the invention may be compositions of water-based or solvent-based.

Swelling during heating of the coating corresponding to the present invention can be used in applications for flooring roofing to prevent the ignition and spread of flame, for use on non-combustible substrates, such as structural steel in buildings, girders and the like, vessels or storage tanks, to protect them from loss of strength when it gets into the region of very high temperatures, when the fire is.

The following examples and drawings are provided for illustration of the invention using the composition of the intumescent coating containing a binder corresponding to the present invention.

Figure 1 shows thermal stability of Newtonian copolymer containing only one copolymer PMS/EGA (75/25), ammonium polyphosphate (APP) or a mixture of both components with the composition of 60/40 (calculated and experimental values).

Figure 2 shows thermal stability of Newtonian copolymer containing only styrene/acrylic copolymer, ammonium polyphosphate (APP) or a mixture of both components with the composition of 60/40 (calculated and experimental values).

Figure 3 shows thermal stability of the copolymer containing cross-linked copolymer containing only one copolymer PMS/EGA (75/25), ammonium polyphosphate (APP) or a mixture of both components with the composition of 60/40 (calculated and experimental values).

Figure 4 shows thermal stability of the copolymer containing only one cross-linked styrene/acrylic copolymer, ammonium polyphosphate (APP) or a mixture of both components with the composition of 60/40 (calculated and experimental values).

Figure 5 illustrates the differences between theoretical and experimental weight loss in TGA for mixtures with the composition of 60/40 for the hypoxia copolymers PMS/EGA (50/50, 75/25 and 100/0) and RDA (curves Δ(T)).

Figure 6 shows thermal insulation on aluminum plates with swelling upon heating the coatings obtained using Newtonian or cross-linked copolymers, these copolymers contain links only PMS/EGA (75/25) or PMS/AGO/acrylic links or a styrene/acrylic links.

Figure 7 illustrates thermal insulation on aluminum plates with swelling upon heating the coatings obtained using a copolymer containing a mixture of Newtonian and cross-linked polymers, or by using a commercial styrene/acrylic copolymer.

Figure 8 illustrates the intensity values of heat release (RHR), measured using the cone calorimeter after exposure in the form of 35 kW/m2for swelling during heating of the coatings obtained using the cover 1, cover 2 or cover 4 of example 2.

Example 1: Temperature resistant polymer binder

1.1.Measurement

thermal stability of various compositions were measured according to the method of thermogravimetric analysis.

Thermogravimetric analyses (TGA) were carried out with 10°C/min in synthetic air or nitrogen (flow rate: 5 × 10- 7m3/with that brand of Air Liquide) when using a microbalance Setaram MTB 10-8. In each case the mass of the specimen used is recorded equal to 10 mg samples (powder mixture) was placed on the open cups made of quartz glass. The accuracy of temperature measurements was 1.5°With the entire range of temperatures. Curves of the mass difference between the experimental and theoretical curves of TGA was calculated as follows:

Mpoly(T): TGA curve for copolymers,

Madd(T): TGA curve for the RDA,

Mexp(T): TGA curve for copolymer/ARR,

Mthe(T): TGA curve calculated in the linear combination of TGA curves for the copolymer and the RDA,

Mthe(T): × Mpoly(T) + y MARR(T)

Δ(T): the curve of the mass difference:

Δ(T) = Mexp(T) - Mthe(T).

Curve Δ(T) makes possible the observation of a gradual increase or decrease thermal stability of the polymer associated with the presence of additives.

1.2.Results

TGA curves illustrated in figures 1 to 5.

Increase heat resistance is obtained in the case of a copolymer PMS/AGO (figure 1) in comparison with the styrene/acrylic (C/a) copolymer (figure 2).

Similar results were obtained in the case of cross-linked copolymers (figures 3 and 4).

The difference between theoretical and experimental curves weight loss Δ(T) in figure 5, obtained for copolymers PMS/EGA with different ratios, shows that the resistance increases with the content of the substituted styrene (PMS).

Example 2: obtain the swelling is ri heated paints

Received various compositions. The first series of dyes was obtained without the use of chlorinated paraffin to visualize the impact of the nature of the polymeric binder to the material behavior under fire. A second series of ink was obtained with the use of chlorinated paraffin.

Paint was obtained with the use of a linear polymer PMS/AGO, cross-linked polymer PMS/EGA, linear polymer, crosslinked polymer and/or comparative commercial copolymer With/A.

The copolymer was dissolved in the solvent under the action of strong shear, then added chlorinated paraffin where it was needed and after homogenization was dispersible pigments in the order described below.

The compositions illustrated in table 1.

2.1.Paint without the use of chlorinated paraffin:

Paint A1: Newtonian copolymer PMS/EGA (75/25).

Paint A2: Newtonian cross-linked copolymer PMS/EGA (75/25).

Paint B1: Newtonian PMS/AGO/acrylic copolymer (50/14/36).

Paint B2: Newton stitched PMS/AGO/acrylic copolymer (50/14/36).

Paint C1: Newtonian styrene/EGA/acrylic copolymer (50/14/36).

Paint C2: Newtonian cross-linked styrene/EGA/acrylic copolymer (50/15/36).

2.2.Paint with the use of chlorinated paraffin:

The compositions illustrated in table 2.

Example 3: Evaluation of thermal and acoustic is ASCII

3.1.Measurement

Temperature profiles were determined through measurement of resistance using a cone calorimeter. The insulating property of swelling upon heating of the coating was tested by conducting measurement of the temperature of the substrate with the coating is subjected to a heat flux equal to 35 or 75 kW/m2. On aluminium panels 100 × 100·4 mm was applied intumescent through the floor (800 g/m2and left them to dry for 48 hours at 50°C. the Samples in accordance with ASTM 1356-90 and ISO 5660 device Stanton Redcroft Cone Calorimeter was subjected to a heat flux equal to 35 or 75 kW/m2, (50 kW/m2corresponds to the heat produced during a fire: in accordance with the work of V. Babrauskas, Fire and Mat(1984), 8(2), 81).

The heat release rate (RHR) is a selection of heat flow per time for the surface of the sample, and it is measured using calorimetry oxygen consumption. Data (TSS (total allocation), TCO2(the total allocation of CO2), TSV (the total amount of smoke emission) and THR (total heat)) was calculated using the developed by the applicants of the software.

3.2.Results

They are illustrated in figures 6 and 7.

The charts in figure 6 show that thermal and acoustic is Alecia better when the binder consists of a combination of linear and crosslinked polymers (paint A2, B2 and C2). When using this combination of polymers, the temperature measured on the back side of the plate with the coating, was significantly lower in comparison with what occurs in the case of a linear polymer as sole binder. The coating is particularly effective when the polymers are only from PMS and AGA coating (A2) or associated with additional substituted acrylate (B2).

Figure 7 shows that after 30 minutes of exposure in the form of 35 kW/m2the temperature on the back side of the plate remains stable at around 310°if coverage is obtained using a combination of Newtonian and cross-linked polymers, i.e. approximately 110°below the temperature measured for the case of the comparative binding/A.

Example 4: the swelling Behavior when heated coatings under fire

It was determined for paints containing chlorinated paraffin, and it is shown in figure 8.

All curves looked similar way, with the first major peak corresponded to the formation of swelling upon heating patterns, after it was followed by the second minor peak or plateau, corresponding to the destruction of the foam and education ostad is, which is stable at high temperatures.

The intensity of heat release (RHR) maximum for the composition containing comparative commercial styrene/acrylic copolymer (200 kW/m2). She is small for the compositions containing the copolymers of substituted styrene/AGA, respectively, 139 kW/m2for PMS copolymer/EGA and 54 kW/m2for PMS copolymer/PTBS/EGA. For comparison, the measured RHR obtained for the case of commercial paints solvent-based Unitherm 38091, and it was equal to 186 kW/m2.

Volumes of smoke emission, the value of allocation of co and CO2and full heat dissipation are shown in table 2, where good performance polymers substituted styrene/EGA (inks 1 to 3) were compared with corresponding characteristics for Unitherm 38091.

Low values for smoke emission, emissions of CO and CO2obtained for the copolymer as a binder corresponding to the invention protect the environment.

1. The copolymer for use in a polymeric binder or polymeric binder in swelling when heated, the coating comprising a mixture of Newtonian copolymer and reticulated copolymer selected from the group comprising thixotropic pseudoplastic-type copolymers and copolymers, these Newtonian and net copoly the career consist of chains of substituted styrene and substituted acrylate and contain links, at least, p-methylstyrene (PMS) and 2-ethylhexyl acrylate (EHA), at a molar ratio of p-methylstyrene (PMS) and 2-ethylhexyl acrylate from 100/0 to 50/50.

2. The copolymer according to claim 1, where the molar ratio of p-methylstyrene and 2-ethylhexyl acrylate equal to 90/10, preferably 80/20, and more preferably 75/25.

3. The copolymer according to claim 1 or 2, additionally containing parts of p-tert-butylstyrene (PCBS) and/or isobutylacetate (IBMA).

4. The copolymer according to any one of claims 1 to 3, where the copolymers of the mixture produced by carrying out emulsion polymerization.

5. Swelling upon heating the coating comprising a polymeric binder, foaming agents, uglerodsesola substances and other commonly used additives, characterized in that as the polymeric binder is a copolymer according to claims 1-4.

6. Swelling upon heating the coating according to claim 5, where the foaming substance is ammonium salt of phosphoric acid, operaterrassen substance chosen from the group comprising pentaerythritol, dipentaerythritol, tripentaerythritol and polycondensate pentaerythritol.

7. Swelling upon heating the coating according to any one of pp.5 and 6, which receive water-based or solvent-based.

8. The method of obtaining swelling during heating of the coating according to any one of pp.5-7, including the state (a) the solution of the Oia Newtonian and net copolymers in solvent or in water, in the condition of strong shear, (b) optionally adding a chlorinated paraffin, (C) homogenizing the mixture and add additives, (d) applying the mixture to the surface in the form of a coating.



 

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45 cl, 8 tbl

FIELD: chemistry.

SUBSTANCE: elastomeric polymer moulding composition can be used for making capacitor insulating layers, medical devices and fuel element seals. An elastomeric polymer moulding composition is described, which contains an elastomeric polymer, which can be cured by peroxide, is completely soluble (i.e. does not contain gel), does not contain divinyl benzene and extracting impurities. Material made based on the said composition is safe during production and use. The composition is an alternative to XL-10000 based compositions (butyl rubber, partially cross linked with divinyl benzene).

EFFECT: increased effectiveness of the composition.

7 cl, 1 tbl, 5 ex, 2 dwg

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