Hardening accelerator composition

Patent metadata

Field	Value
Publication number	US-9598315-B2
Application number	US-201414651774-A
Country	US
Kind code	B2
Filing date	Jan 27, 2014
Priority date	Jan 25, 2013
Publication date	Mar 21, 2017
Grant date	Mar 21, 2017

Abstract

The invention relates to a process for the preparation of a hardening accelerator composition by reacting a calcium source selected from calcium hydroxide, calcium oxide with a water-soluble silicate compound in the presence of at least one water-soluble polymeric dispersing agent and the hardening accelerator composition obtainable by said process. The composition has a low content of anions and of alkali cations and is therefore broadly applicable in building material mixtures.

First claim

The invention claimed is:

1. A process for the preparation of a hardening accelerator composition, the process comprising:
reacting, in water, a calcium source selected from the aroup consisting of calcium hydroxide and calcium oxide with a water-soluble silicate compound in the presence of at least one water-soluble polymeric dispersing agent,
wherein the at least one water-soluble dispersing agent comprises an anionic group and/or an anionoaenic group, and further comprises a polyether side chain, and
wherein the water-soluble silicate compound is of a formula m SiO 2 .n M 2 O; M is selected from the group consisting of Li, Na, K and NH 4 ; m and n are molar numbers; and a ratio of m:n is from 2.5 to 4.

2. The process according to claim 1 , wherein the calcium source and the water-soluble silicate compound are added to an aqueous solution of the water-soluble polymeric dispersing agent.

3. The process according to claim 1 , wherein:
i) the calcium source is present in an amount of from 0,01 to 75% by weight of calcium hydroxide or calcium oxide;
ii) the water-soluble silicate compound is present in an amount of from 0.01 to 75% by weight;
iii) the water-soluble dispersing agent is present in an amount of from 0.001 to 60% by weight; and
iv) the water is present in an amount of from 24 to 99% by weight of water.

4. The process according to claim 1 , wherein ratio of m:n is from 2.5 to 3.8.

5. The process according to claim 1 , wherein the water-soluble silicate compound is used in powder form.

6. The process according to claim 1 , wherein the dispersing agent is a copolymer which includes at least one structural unit having a formula selected from the group consisting of formulas (Ia), (Ib), (Ic), and (Id):

wherein R 1 is H or branched or unbranched C 1 -C 4 alkyl, CH 2 COOH or CH 2 CO—X—R 3 ; X is NH—(C n H 2n ) or O—(C n H 2n ) wherein n is 1, 2, 3 or 4, wherein the nitrogen atom or the oxygen atom is bound to the CO group, or X is a chemical bond;
R 2 is OM, PO 3 M 2 , or O—PO 3 M 2 ; with the proviso that X is a chemical bond, if R 2 is OM;
R 3 is PO 3 M 2 , or O—PO 3 M 2 ;

wherein R 3 is H or branched or unbranched C 1 -C 4 alky;
n is 0, 1, 2, 3 and 4;
R 4 is PO 3 M 2 , or O—PO 3 M 2 ;

wherein R 5 is H or branched or unbranched C 1 -C 4 alkyl;
Z is O or NR 7 ;
R 7 is H, (C n H 2n )—OH, (C n H 2n )—PO 3 M 2 , (C n H 2n )—OPO 3 M 2 , (C 6 H 4 )—PO 3 M 2 , or (C 6 H 4 )—OPO 3 M 2 ;
n is 1, 2, 3 or 4; and

wherein R 6 is H or branched or unbranched C 1 -C 4 alkyl;
Q is O or NR 7 ;
R 7 is H, (C n H 2n )—OH, (C n H 2n )—PO 3 M 2 , (C n H 2n )—OPO 3 M 2 , (C 6 H 4 )—PO 3 M 2 , or (C 6 H 4 )—OPO 3 M 2 ;
n is 1, 2, 3 or 4; and
wherein each M independently is H or a cation equivalent.

7. The process according to claim 1 , wherein the dispersing agent is a copolymer which comprises at least one structural unit of a formula selected from the group consisting of formulas (IIa), (IIb), (IIc), and (IId):

wherein R 10 , R 11 and R 12 are independently of one another, H branched or unbranched C 1 -C 4 alkyl;
E is branched or unbranched C 1 -C 6 -alkylene, cyclohexylene, CH 2 —C 6 H 10 , 1,2-phenylene, 1,3-phenylene, or 1,4-phenylene;
G is O, NH or CO—NH, or E and G together form a chemical bond;
A is C x H 2x where x=2, 3, 4, 5 or CH 2 CH(C 6 H 5 );
n is 0, 1, 2, 3, 4 or 5;
a is an integer from 2 to 350;
R 13 is H, branched or unbranched C 1 -C 4 alkyl, CO—NH 2 or COCH 3 ;

wherein R 16 , R 17 , and R 18 are each independently is H or branched or unbranched C 1 -C 4 alkyl;
E is branched or unbranched C 1 -C 6 -alkylene, cyclohexylene, CH 2 —C 6 H 10 , 1,2-phenylene, 1,3-phenylene, or 1,4-phenylene;
A is C x H 2x where x is 2, 3, 4, 5 or CH 2 CH(C 6 H 5 );
L is C x H 2x with x=2, 3, 4, 5 or CH 2 —CH(C 6 H 5 );
a is an integer from 2 to 350;
d is an integer from 1 to 350;
R 19 is H or branched or unbranched C 1 -C 4 -alkyl;
R 20 is H or branched or unbranched C 1 -C 4 -alkyl; and
n is 0, 1, 2, 3, 4 or 5;

wherein R 21 , R 22 and R 23 independently of each other are H or branched or unbranched C 1 -C 4 -alkyl;
W is O, NR 25 or N;
Y is 1, if W is O or NR 25 , and Y is 2, if W is N;
A is C x H 2x with x=2, 3, 4, 5 or CH 2 CH(C 6 H 5 );
a is an integer from 2 to 350;
R 24 is H or branched or unbranched C 1 -C 4 -alkyl;
R 25 is H or branched or unbranched C 1 -C 4 -alkyl; and

wherein
R 6 is H or branched or unbranched C 1 -C 4 -alkyl;
Q is NR 10 , N or O;
Y is 1, if Q is O or NR 10 , and Y is 2, if Q is N;
R 10 is H or branched or unbranched C 1 -C 4 -alkyl;
A is C x H 2x with x is 2, 3, 4, 5 or CH 2 CH(C 6 H 5 ); and
a is an integer from 2 to 350.

8. The process according to claim 1 , wherein the dispersing agent is a polycondensation product comprising structural units (III) and (IV), wherein:

wherein T is substituted or unsubstituted phenyl or naphthyl or substituted or unsubstituted heteroaryl with 5 to 10 ring atoms, of which 1 or 2 atoms are heteroatoms, which are selected from N, O and S;
n is 1 or 2;
B is N, NH or O, with the proviso that n is 2, if B is N and with the proviso that n is 1, if B is NH or O;
A is C x H 2x with x is 2, 3, 4, 5 or CH 2 CH(C 6 H 5 );
a is an integer from 1 to 300;
R 25 is H or branched or unbranched C 1 -C 10 -alkyl, C 5 -C 8 -cycloalkyl, aryl, or heteroaryl with 5 to 10 ring atoms, of which 1 or 2 atoms are heteroatoms, which are selected from N, O and S;
wherein structural unit (IV) is selected from structural units (IVa) and (IVb):

wherein D is substituted or unsubstituted phenyl or naphthyl or substituted or unsubstituted heteroaryl with 5 to 10 ring atoms, of which 1 or 2 atoms are heteroatoms, which are selected from N, O and S;
E is N, NH or O, with the proviso that n is 2, if E is N and with the proviso that n is 1, if E is NH or O;
A is C x H 2x with x is 2, 3, 4, 5 or CH 2 CH(C 6 H 5 );
b is an integer from 1 to 300;
M is independently H or a cation equivalent;

wherein V is substituted or unsubstituted phenyl or naphthyl which is optionally substituted by one or two groups selected from R 8 , OH, OR 8 , (CO)R 8 , COOM, COOR 8 ,

Assignees

• Basf Se

Inventors

• Hesse Christoph
• Nicoleau Luc

Classifications

• C04B28/02 Primary

  containing hydraulic cements other than calcium sulfates · CPC title

• C04B28/065

  Calcium aluminosulfate cements, e.g. cements hydrating into ettringite · CPC title

• C04B28/16

  containing anhydrite {, e.g. Keene's cement} · CPC title

• C04B2103/14

  Hardening accelerators · CPC title

• C04B28/14

  containing calcium sulfate cements {(gypsum-paper plates E04C)} · CPC title