Mortar composition based on isocyanate amine adducts, multi-component resin system, method for the fastening of construction elements and use of the multi component resin system for the fastening of construction elements

Abstract

A multi-component resin system can be used for producing a mortar composition based on isocyanate amine adducts for the chemical fastening of construction elements. A mortar composition based on isocyanate amine adducts can be produced from the multi-component resin system. A corresponding method can be used for the chemical fastening of construction elements in mineral substrates, using the mortar composition based on the isocyanate amine adducts.

Claims

1: A multi-component resin system, containing: at least one isocyanate component (A), and at least one amine component (B), wherein the at least one isocyanate component (A) comprises at least one aliphatic and/or aromatic polyisocyanate having an average NCO functionality of 2 or more, wherein the at least one amine component (B) comprises at least one amine which is reactive to isocyanate groups and has an average NH functionality of 2 or more, wherein the multi-component resin system is free of polyaspartic acid esters, and the at least one isocyanate component (A) and/or the at least one amine component (B) comprises at least one filler and at least one rheology additive, and wherein a total filling level of a mortar composition produced by mixing the at least one isocyanate component (A) and the at least one amine component (B) is in a range from 30 to 80%, based on the g total weight of the multi-component resin system.

2: The multi-component resin system according to claim 1, wherein both the at least one isocyanate component (A) and the at least one amine component (B) comprise the at least one filler and the at least one rheological additive.

3: The multi-component resin system according to claim 2, wherein a filling level of the at least one isocyanate component (A) and a filling level of the at least one amine component (B) is from 10 to 70 wt. %, based in each case on a total weight of the at least one isocyanate component (A) and the at least one amine component (B), respectively.

4: The multi-component resin system according to claim 1, wherein the at least one isocyanate component (A) and the at least one amine component (B) are present in a quantity ratio in which the average NCO functionality to the average NH functionality is between 0.3 and 2.0.

5: The multi-component resin system according to claim 1, wherein the at least one isocyanate component (A) comprises at least one aromatic polyisocyanate selected from the group consisting of 1,4-phenylene diisocyanate, 2,4- and 2,6-toluylene diisocyanate, xylylene diisocyanate, hydrogenated xylylene diisocyanate, tetramethylxylylene diisocyanate, 1,5-naphthylene diisocyanate, diphenylene methane-2,4′- and -4,4′-diisocyanate, triphenylmethane-44′,4-triisocyanate, bis- and tris-(isocyanatoalkyl)-benzene, toluene, and xylene.

6: The multi-component resin system according to claim 1, wherein the at least one isocyanate component (A) comprises at least one aliphatic polyisocyanate selected from the group consisting of hexamethylene diisocyanate (HDI), trimethyl HDI (TMDI), pentane diisocyanate (PDI), 2-methylpentane-1,5-diisocyanate (MPDI), isophorone diisocyanate (IPDI), 1,3- and 1,4-bis(isocyanatomethyl)cyclohexane (H6XDI), bis(isocyanatomethyl)norbornane (NBDI), 3(4)-isocyanatomethyl-1-methyl-cyclohexyl isocyanate (IMCI), and 4,4′-bis (isocyanatocyclohexyl)methane (H12MDI).

7: The multi-component resin system according to claim 1, wherein the total filling level is in a range from 35 to 65 wt. %, based on the total weight of the multi-component resin system.

8: The multi-component resin system according to claim 1, wherein the at least one isocyanate component (A) and/or the at least one amine component (B) contain at least one adhesion promoter.

9: The multi-component resin system according to claim 1, wherein the at least one amine which is reactive to isocyanate groups is selected from the group consisting of 4,4′-methylene-bis[N-(1-methylpropyl)phenylamine], an isomer mixture of 6-methyl-2,4-bis(methylthio)phenylene-1,3-diamine and 2-methyl-4,6-bis(methylthio)phenylene-1,3-diamine, 4,4′-methylenebis(2,6-diethylaniline), 4,4′-methylenebis(N-sec-butylcyclohexanamine), 3,3′-diaminodiphenylsulfone, N,N′-di-sec-butyl-p-phenylenediamine, 2,4,6-trimethyl-m-phenylenediamine, and a mixture thereof.

10: The multi-component resin system according to claim 1, wherein the multi-component resin system is a two-component resin system.

11: A mortar composition, produced by mixing the at least one isocyanate component (A) and the at least one amine component (B) of the multi-component resin system according to claim 1.

12: A method, comprising: chemically fastening a construction element in a borehole, with the mortar composition according to claim 11.

13: A method of improving temperature resistance of a chemical anchor, comprising: curing the mortar composition according to claim 11, to obtain the chemical anchor.

14: The method according to claim 13, wherein the chemical anchor has improved pull-out strength at 80° C.

15: A method, comprising: chemically fastening a construction element in a borehole, with the multi-component resin system according to claim 1.

16: A method of improving temperature resistance of a chemical anchor, comprising: mixing the multi-component resin system according to claim 1, to obtain a mortar composition, and curing the mortar composition, to obtain the chemical anchor.

17: The method according to claim 16, wherein the chemical anchor has improved pull-out strength at 80° C.

Description

EXAMPLES

Components Used:

[0083] 4,4′-methylene-bis[N-(1-methylpropyl)phenylamine] (from ABCR), aspartic acid. N,N′-(methylenedi-4,1-cyclohexanediyl)bis-,1,1′,4,4′-tetraethyl ester (as Desmophen NH 1420 from Covestro), a mixture of (6-methyl-2,4-bis(methylthio)phenylene-1,3-diamine and 2-methyl-4,6-bis(methylthio)phenylene-1,3-diamine (as Ethacure 300 Curative from Albermale), 4,4′-methylenebis(2,6-diethylaniline) (from TCI) and diethyltoluenediamine (as Ethacure 100 from Albermale) were used as the amine which is reactive to isocyanate groups in the amine component.

[0084] Hexamethylene-1,6-diisocyanate homopolymers (as Desmodur N 3600 and N 3900 from Covestro), hexamethylene-1,6-diisocyanate biuret oligomerization product (as Desmodur N 3200 from Covestro) and a mixture of hexamethylene-1,6-diisocyanate homopolymer and isophorone diisocyanate homopolymer (as Desmodur XP 2838 from Covestro) were used as isocyanates in the isocyanate component.

[0085] 3-aminopropyltriethoxysilane (as Dynasylan AMEO from Evonik) and 3-glycidyloxypropyltrimethoxysilane (as Dynasylan GLYMO from Evonik) were used as adhesion promoters.

[0086] Quartz powders (Millisil™ W3 and W12 from Quarzwerke Frechen) and quartz sand (F32 from Quarzwerke Frechen) were used as fillers and silica (Cab-O-Sil™ TS-720 from Cabot Rheinfelden) was used as a thickener.

COMPARATIVE EXAMPLES

[0087] Two commercially available mortar compositions are used as comparative examples: RE500V3 (Hilti, comparative example 1, epoxy resin mortar) and HY200A (Hilti, comparative example 2). The composition listed in the table below, which is based on EP 3 447 078 A1, is used as comparative example 3.

TABLE-US-00001 TABLE 1 Composition of comparative example 3 in wt. % based on EP 3447078 A1 Constituent Comparative example 3 Isocyanate component Hexamethylene-1,6- 24.4 diisocyanate homopolymer (N3900) Quartz powder (W12) 14.4 Silica 0.6 Amine component Aspartic acid, N,N′- 37.6 (methylenedi-4,1- cyclohexanediyl)bis-,1,1′,4,4′- tetraethyl ester Quartz powder (W12) 22.1 Silica 0.9 Isocyanate:amine ratio 1:1 Filling level in % 38

Examples According to the Invention

[0088] The compositions according to the invention of the isocyanate component and the amine component are shown in Tables 2 and 3 below.

TABLE-US-00002 TABLE 2 Compositions of the isocyanate component and the amine component [wt. %] for examples 1 to 7 according to the invention; use of different amines. 1 2 3 4 5 6 7 Iso- Hexamethylene- 38.9 39.6 36.4 37.7 37.9 33.4 39.0 cyanate 1,6-diisocyanate com- homopolymer ponent (N3900) Quartz powder 22.9 24.2 21.4 22.2 22.3 19.6 23.0 (W12) Silica 0.9 1.0 0.9 0.9 0.9 0.9 0.9 Amine 4,4′-methylene- — — 12.8 6.1 — 22.9 — com- bis[N-(1- ponent methylpropyl) phenylamine] (6-methyl-2,4- 23.1 23.4 12.8 18.2 19.2 — 21.9 bis(methylthio) phenylene- 1,3-diamine/2- methyl-4,6- bis(melhylthio) phenylene- 1,3-diamine (DMTDA) 4,4′-methyl- — — — — 4.8 5.7 — enebis(2,6- diethylaniline) Diethyltoluene- — — — — — — 1.1 diamine (DETDA) Quartz powder 13.5 11.2 15.1 14.3 14.2 16.9 13.5 (W12) Silica 0.7 0.5 0.6 0.6 0.6 0.6 0.6 Isocyanate: 1:1 1:1 1:1 1:1 1:1 1:1 1:1 amine ratio Filling level 38 37 38 38 38 38 38 in %

TABLE-US-00003 TABLE 3 Compositions of the isocyanate component and the amine component [wt. %] for examples 8 to 16 according to the invention; examples 8 to 10: variation of isocyanate; examples 11 to 14: variation of fillers and filling level; examples 15 and 16: addition of silane. 8 9 10 11 12 13 14 15 16 Iso- Hexamethylene- 40.3 — — — — — — — — cyanate 1,6-diisocyanate com- homopolymer/ ponent isophorone diisocyanate homopolymer (XP2838) Hexamethylene- — 40.1 — — — — — — — 1,6-diisocyanate biuret oligomerization product (N3200) Hexamethylene- — — 39.2 — — — — — — 1,6-diisocyanate homopolymer (N3600) Hexamethylene- — — — 31.4 25.1 38.9 38.9 39.3 38.3 1,6-diisocyanate homopolymer (N3900) Quartz sand — — — — — — 22.9 — — (F32) Quartz powder — — — — — 22.9 — — — (W3) Quartz powder 23.7 23.6 23.6 30.5 36.7 — — 22.4 21.4 (W12) Silica 1.0 1.0 1.0 0.9 0.9 0.9 0.9 0.9 0.9 Amine (6-methyl-2,4- 21.7 22.0 22.8 18.6 14.9 23.1 23.1 22.8 23.7 com- bis(methylthio) ponent phenylene-1,3- diamine/ 2-methyl-4,6- bis(methyithio) phenylene- 1,3-diamine (DMTDA) 3-amino- — — — — — — — 1.1 — propyl- trimethoxy- silane Quartz sand — — — — — — 13.6 — — (F32) Quartz powder — — — — — 13.6 — — — (W3) Quartz powder 12.8 12.9 12.9 18.0 21.8 — — 13.0 13.2 (W12) Silica 0.5 0.5 0.5 0.6 0.6 0.6 0.6 0.6 0.6 Isocyanate: 1:1 1:1 1:1 1:1 1:1 1:1 1:1 1:1 1:1 amine ratio Filling level 38 38 38 50 60 38 38 37 36 in %

Mortar Compositions and Dull-Out Tests

[0089] To produce the mortar compositions, the isocyanate component and the amine component were each first produced individually. For this purpose, the constituents shown in Tables 1 to 3 were added together and mixed with one another. The liquid isocyanate and amine components produced in this way were each mixed in a speed mixer (DAC-600 from Hauschild) for 30 seconds at 1500 rpm. The isocyanate component and the amine component were then combined with one another and mixed in a speed mixer for 30 seconds at 1500 rpm. The mortar composition obtained in this way was filled into a hard cartridge and injected into a borehole using an extrusion device.

[0090] The pull-out strength of the mortar compositions obtained by mixing the isocyanate component and the amine component according to the above examples was determined using a high-strength anchor threaded rod M12, which was doweled into a hammer-drilled borehole having a diameter of 14 mm and a borehole depth of 72 mm by means of the relevant mortar composition in C20/25 concrete. The boreholes were cleaned by means of compressed air (2×6 bar), a wire brush (2×) and again by compressed air (2×6 bar).

[0091] The boreholes were filled up, by two thirds from the bottom of the borehole, with the mortar composition to be tested in each case. The threaded rod was pushed in by hand. After curing, the mortar ring protruding from the borehole was cut off.

[0092] To determine the reference bond stress, after a curing time of 24 hours at a temperature of 23° C., the failure load was determined by centrally pulling out the threaded anchor rod with close support.

[0093] To determine the bond stress at 80° C., after a curing time of 24 hours at a temperature of 23° C., the concrete blocks were heated to 80° C. and held at that temperature for 24 hours. Immediately after removing the concrete slabs from the oven, the failure load at 80° C. was determined by centrally pulling out the threaded anchor rod with close support.

[0094] The bond stresses obtained with the mortar compositions are shown in Tables 4 to 6 below.

TABLE-US-00004 TABLE 4 Results of the determination of the reference bond stress at 23° C. after a curing time of 24 hours and the bond stress at 80° C. for comparative examples 1 to 3. Comparative Comparative Comparative example 1 example 2 example 3 Pull-out tests Bond stress [N/mm.sup.2] Reference 39 32 26.0 80° C. 16 25 1.8 Ratio 0.41 0.78 0.07

TABLE-US-00005 TABLE 5 Results of the determination of the reference bond stress at 23° C. after acuring time of 24 hours and the bond stress at 80° C. for comparative examples 1 to 7. 1 2 3 4 5 6 7 Pull-out tests Bond stress [N/mm.sup.2] Reference 23.5 24.4 29.9 26.1 24.8 27.2 25.0 80° C. 22.8 23.0 15.5 19.0 25.5 17.5 23.5 Ratio 0.97 0.94 0.52 0.73 1.03 0.64 0.94 * not determinable

TABLE-US-00006 TABLE 6 Results of the determination of the reference bond stress at 23° C. after a curing time of 24 hours and the bond stress at 80° C. for examples 8 to 16 according to the invention. 8 9 10 11 12 13 14 15 16 Pull-out tests Bond stress [N/mm.sup.2] Reference 18.2 25.6 22.7 25.5 26.6 22.6 20.4 23.5 26.0 80° C. 23.6 20.1 22.9 23.3 23.6 23.5 23.7 20.7 24.7 Ratio 1.30 0.78 1.01 0.92 0.89 1.04 1.16 0.89 0.95