Two-component composition

FR3152808A1Pending Publication Date: 2025-03-14BOSTIK SA(FR)
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Patent Information

Application Number
FR2023009524
Authority / Receiving Office
FR · FR
Patent Type
Applications
Current Assignee / Owner
Filing Date
2023-09-11
Publication Date
2025-03-14
Patent Text Reader

Abstract

The invention relates to a two-component composition comprising: a component A comprising at least one polyisocyanate; and a component B comprising at least one polyol; component A and / or component B further comprising at least one polyvinyl chloride (PVC) filler, said filler having a viscosity at a 5 s⁻¹ velocity gradient greater than or equal to 10 Pa·s, the viscosity being measured at 23°C for a diisononyl phthalate (DINP) / filler mixture, the weight ratio of which is 0.6, after 2 hours of aging at 23°C. The invention also relates to the use of the two-component composition according to the invention. Furthermore, the invention relates to a method for assembling substrates implementing the two-component composition according to the invention. Finally, the invention relates to an article comprising the two-component composition according to the invention. Figure for the abstract: none
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Description

[0182] - bringing the substrates into contact.

[0183] The two-component composition according to the invention is as described above, including the preferred embodiments and characteristics.

[0184] It is understood that, during the coating step and the contacting step, the two-component composition according to the invention is in the uncured state.

[0185] The substrates may be the same or different.

[0186] The substrates concerned are very varied and are, for example, inorganic substrates such as concrete, metals and / or alloys (such as aluminum alloys, steel, non-ferrous metals and galvanized metals), and / or organic substrates such as wood and / or plastics (such as PVC, polycarbonate, PMMA, polyethylene, polypropylene, polyesters, epoxy resins). Article

[0187] The present invention also relates to an article comprising the two-component composition according to the invention (cured or not), said composition binding at least two substrates of said article.

[0188] The two-component composition according to the invention is as described above, including the preferred embodiments and characteristics.

[0189] The article can be obtained by the method of assembling substrates according to the invention (including preferred embodiments and characteristics).

[0190] The substrates are preferably as described above for the substrate assembly method according to the invention.

[0191] All the embodiments described above can be combined with each other. the others. In particular, the various aforementioned constituents of the composition, and in particular the preferred modes, can be combined with each other.

[0192] The following examples are given purely for illustrative purposes of the invention and should not be interpreted as limiting its scope. Examples Example 1: Ingredients and measurement methods Ingredients used

[0193] The following ingredients were used:

[0194] - NCO polymer: polymer obtained from 4,4'- and 2,4'-diphenylmethane dii- isocyanate (MDI) and polyether diol, having an isocyanate content (%NCO) by weight of about 19% relative to the total weight of the polymer;

[0195] - Siliporite® SA 1720 (by ARKEMA): synthetic zeolite of type A having a pore diameter of 3 Å, charge;

[0196] - Bis-urea / DIDP: obtained by reaction of n-butylamine and 4,4'-MDI in DIDP, rheology agent,

[0197] - Polymer polyol 1: polyurethane having a number-average molar mass of about 3450 g / mol, obtained from castor oil, polyether triol and a mixture of 4,4'- and 2,4'-MDI with an NCO / OH molar equivalent ratio of about 0.2;

[0198] - 2-ethyl-1,3-hexanodiol, low molar mass polyol (146 g / mol);

[0199] - Polymer polyol 2: liquid polybutadiene with hydroxyl terminations having a number-average molar mass of approximately 2900 g / mol and a hydroxyl number between 44 and 51 mg KOH / g of polybutadiene;

[0200] - BYK 081 (by BYK Chemie): non-aqueous emulsion polysiloxane (propylene glycol), deboiling agent;

[0201] - MIKHART 10 (by Provençale SA): ground calcium carbonate having a size of average particles of 10 pm, charge,

[0202] - HAKUENKA® CCR-S10 (by OMYA): coated precipitated calcium carbonate fatty acids with an average particle size of 80 nm, charge,

[0203] - THIXATROL® AS 8053 (by ELEMENTIS): micronized amide wax having a average diameter less than 5 pm, rheology agent;

[0204] - RUETASOLV DI (by HM Royal): diisopropylnaphthalene having a point boiling point of 290-300°C, solvent;

[0205] - Lacovyl® PE1402H (by KEM ONE): PVC powder (homopolymer) produced by an emulsion polymerization process, having a viscosity at a speed gradient of 5 s 1 equal to 16.0 Pa.s, the viscosity being measured at 23°C according to standard EN ISO 3219:1993 for a mixture by weight PVC 100 / diisononyl phthalate 60 after 2 hours aging at 23°C, load;

[0206] - Lacovyl® PB 1302 (by KEM ONE): PVC powder (homopolymer) produced by a micro-suspension polymerization process, having a viscosity at a speed gradient of 5 s 1 equal to 3.3 Pa.s, the viscosity being measured at 23°C according to standard EN ISO 3219:1993 for a mixture by weight PVC 100 / diisononyl phthalate 60 after 2 hours of aging at 23°C, load. Preparation of bis-urea

[0207] Two solutions are prepared:

[0208] - a solution A of n-butylamine in diisodecyl phthalate (DIDP), consisting of 17.17% by weight of n-butylamine and 82.83% by weight of DIDP, the percentages being on the total weight of solution A, then

[0209] - a solution B of 4,4'-MDI in DIDP, consisting of 29.46% by weight of 4,4'-MDI in 70.54% by weight of DIDP, the percentages being on the total weight of solution B.

[0210] The 2 solutions A and B are heated to 100°C, then introduced, each under a pressure of 100 bar, into a reactor, in which they are continuously sprayed onto each other in a ratio A / B = 50.1 / 49.9 by weight, corresponding to a molar ratio n-butylamine / MDI equal to 2. The reaction is immediate and the temperature of the reactor reaches 140°C at the end of manufacture.

[0211] At the reactor outlet, a stable dispersion of 23.3% by weight (relative to the total weight of the dispersion) in the DIDP of a bis-urea of ​​formula:

[0212] The Brookfield viscosity of the suspension measured at 23°C is 15 Pa.s. Measurement methods

[0213] The density of components A and B is measured according to ISO 2811-1.

[0214] Tensile strength and Young's modulus were measured in accordance with ISO 37 (2012), at a constant speed of 100 mm / min.

[0215] In particular, the following conditions were applied:

[0216] A standard dumbbell-shaped test piece (H2), type 2, as illustrated in international standard ISO 37 (2012) is used. The narrow part of the dumbbell used has a length of 20 mm, a width of 4 mm and a thickness of 2 mm.

[0217] To prepare the dumbbell, the composition to be tested (previously packaged in a cartridge) is extruded into a Teflon mold, and is left to harden for 14 days under standard conditions (23°C and 50% relative humidity).

[0218] The principle of measurement consists of stretching in a tensile machine (for example Zwick Roell 2.5KN), whose movable jaw moves at a constant speed equal at 100 mm / min, a standard test piece and to record:

[0219] - the tensile strength (in MPa) which is the tensile stress at which produces the rupture of the test piece (also called TS for Tensile Strength in English), and

[0220] - Young's modulus (expressed in MPa) which is the slope of the tangent at the origin of the curve showing the tensile stress as a function of the elongation of the specimen.

[0221] The measurement is carried out at 23°C or at 40°C, is repeated for 5 test pieces, and the corresponding average of the results obtained is calculated.

[0222] Example 2: Preparation and properties of a composition according to the invention and of comparative compositions

[0223] Each of the compositions consists of a component A and a component B.

[0224] Component A is identical for all compositions and is prepared by mixing the ingredients indicated in Table 1 at room temperature (about 23°C) and under vacuum (about -90kPa), the percentages being percentages by weight of the total weight of component A.

[0225] [Tables 1] Component A NCO Polymer 79.6% Siliporite® SA 1720 5% Bis-urea / DIDP 15.4%

[0226] Component A has a density equal to 1.15.

[0227] Components 1B-3B are prepared by mixing the ingredients indicated in the Table 2 at room temperature (approximately 23°C) and under vacuum (approximately -90kPa), the percentages being percentages by weight of the total weight of component B.

[0228] [Tables2] Component IB (comp.) 2B (inv.) 3B (comp.) Polymer polyol 1 15.5% 15.5% 15.5% 2-ethyl-1,3-hexanodiol 14.2% 14.2% 14.2% Polymer polyol 2 5% 5% 5% Siliporite® SA 1720 3% 3% 3% BYK 081 0.3% 0.3% 0.3% MIKHART 10 45.5% 8.5% 8.5% HAKUENKA® CCR-S10 8.5% 8.5% 8.5% THIXATROL® AS 8053 3% 3% 3% RUETASOLV DI 5% 5% 5% Lacovyl® PE1402H - 37% - Lacovyl® PB 1302 - - 37%

[0229] Component IB has a density equal to 1.53 while components 2B and 3B have densities equal to 1.22.

[0230] Compositions 1-3 are then obtained by mixing component A respectively with component IB, 2B or 3B, using a SpeedMixer™ mixer at room temperature (approximately 23°C), in a volume ratio equal to 1.

[0231] Their mechanical properties are then evaluated in accordance with Example 1, and the results are shown in Table 3 below.

[0232] [Tables3] Composition 1 (comp.) 2 (inv.) 3 (comp.) Tensile strength at 23°C (MPa) 16.8 27.5 22 Young's modulus at 23°C (MPa) 984 957 750 Tensile strength at 40°C (MPa) 8 14.7 6.4 Young's modulus at 40°C (MPa) 338 929 550

[0233] Replacing the majority of the ground calcium carbonate in comparative composition 1 with a PVC filler makes it possible to reduce the density of the composition. Indeed, components 2B and 3B have a lower density than component IB.

[0234] In addition, replacing the majority of the ground calcium carbonate in Comparative Composition 1 with Lacovyl® PE1402H (PVC filler) significantly increases the tensile strength at both 23°C and 40°C, as well as the Young's modulus at 40°C, while maintaining a high Young's modulus at 23°C. (comparison with composition 2 according to the invention).

[0235] On the other hand, if Lacovyl® PB 1302 is used instead of Lacovyl® PE1402H, the tensile strength at 23°C and 40°C, as well as the Young's modulus at 23°C and 40°C, decrease (comparative composition 3 vs. composition 2 according to the invention). In addition, the Young's modulus at 23°C and 40°C and the tensile strength at 40°C decrease significantly compared to the composition not comprising PVC filler (comparative composition 1).

[0236] Thus, the use of Lacovyl® PE1402H (PVC filler having a viscosity at a speed gradient of 5 s 1 equal to 16.0 Pa.s) makes it possible to obtain a lighter adhesive than a conventional composition mainly comprising carbonated fillers, while giving it high tensile strength and Young's modulus both at 23°C and at 40°C.

[0237] Furthermore, the properties of composition 2 according to the invention allow its use as a semi-structural adhesive.

[0238] Consequently, composition 2 according to the invention can be used to obtain semi-structural assemblies which are not only lighter, but also more resistant to mechanical stresses, including when the ambient temperature increases significantly (for example, in summer or during transport or storage).

Claims

Claims

1. Two-component composition comprising: - a component A comprising: • at least one polyisocyanate; and - a component B comprising: • at least one polyol; component A and / or component B further comprising at least one polyvinyl chloride (PVC) filler, said filler having a viscosity at a speed gradient of 5 s 1 greater than or equal to 10 Pa.s, the viscosity being measured at 23°C for a diisononyl phthalate (DINP) / filler mixture, the weight ratio of which is equal to 0.6, after 2 hours of aging at 23°C.

2. A two-component composition according to claim 1, wherein the at least one polyisocyanate is a polyurethane polyisocyanate.

3. A two-component composition according to claim 1 or 2, wherein the at least one polyol comprises two polymer polyols and a low molecular weight polyol.

4. A two-component composition according to any one of claims 1 to 3, wherein the at least one PVC filler is a PVC homopolymer.

5. Two-component composition according to any one of claims 1 to 4, in which the at least one PVC filler is obtained by an emulsion polymerization process.

6. A two-component composition according to any one of claims 1 to 5, further comprising at least one rheology agent in component A and / or component B.

7. A two-component composition according to any one of claims 1 to 6, further comprising at least one filler in component A and / or component B.

8. Use of the two-component composition according to any one of claims 1 to 7 as an adhesive.

9. Method for assembling substrates comprising: - coating, on at least one surface of the substrates to be assembled, the two-component composition according to any one of claims 1 to 7, then - bringing the substrates into contact.

10. An article comprising the two-component composition of any one of claims 1 to 7, said composition binding at least two substrates of said article.

Citation Information

Patent Citations

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    WO2018172651A1

  • Polyurethane-based composition

    WO2019193279A1

  • Two-component polyurethane structural adhesive with improved properties

    WO2022129731A1