Powder composition for rapid suspension

Abstract

The invention relates to a pulverulent composition which can be produced by bringing a powder which comprises at least one inorganic binder into contact with from 0.01 to 10% by weight, based on the total mass of the composition, of a liquid component comprising at least one copolymer which can be obtained by polymerization of a mixture of monomers comprising (I) at least one ethylenically unsaturated monomer which comprises at least one radical selected from the group consisting of carboxylic acid, carboxylic acid salt, carboxylic esters, carboxamide, carboxylic anhydride and carboximide and (II) at least one ethylenically unsaturated monomer having a polyalkylene oxide radical, where the liquid component contains at least 1% by weight of the at least one copolymer and at least 30% by weight of an organic solvent. Furthermore, a process for producing the liquid component, the use thereof and also specific copolymers are disclosed.

Claims

1. A pulverulent composition produced by bringing a powder which comprises at least one inorganic binder into contact with from 0.01 to 10% by weight, based on the total mass of the composition, of a liquid component comprising at least one copolymer obtained by polymerization of a mixture of monomers comprising (I) at least one ethylenically unsaturated monomer which comprises at least one radical selected from the group consisting of carboxylic acid, carboxylic acid salt, carboxylic esters, carboxamide, carboxylic anhydride and carboximide and (II) at least one ethylenically unsaturated monomer having a polyalkylene oxide radical, where the liquid component contains at least 1% by weight of the at least one copolymer and at least 30% by weight of an organic solvent; wherein said bringing into contact occurs prior to adding make-up water to the powder.

2. The pulverulent composition according to claim 1, characterized in that the composition contains from 5 to 99.5% by weight of the inorganic binder.

3. The pulverulent composition according to claim 1, characterized in that the inorganic binder is at least one binder selected from the group consisting of cement based on portland cement, white cement, calcium aluminate cement, calcium sulfoaluminate cement, calcium sulfate n-hydrate and latent hydraulic or pozzolanic binder.

4. The pulverulent composition according to claim 1, characterized in that at least 50% by weight of the at least one copolymer is present in dissolved form in the liquid component.

5. The pulverulent composition according to claim 1, characterized in that the monomer (I) or (II) comprises a random ethylene oxide-propylene oxide copolymer having a molecular weight of from 160 to 10 000 g/mol.

6. The pulverulent composition according to claim 1, characterized in that the proportion of the monomer (I) in the copolymer is from 5 to 95 mol %.

7. The pulverulent composition according to claim 1, characterized in that the ethylenically unsaturated monomer (I) is represented by at least one of the following general formulae from the group (Ia), (Ib) and (Ic): ##STR00005## where R.sup.1 and R.sup.2 are each, independently of one another, hydrogen or an aliphatic hydrocarbon radical having from 1 to 20 carbon atoms, Y is H, COOM.sub.a, COO(C.sub.qH.sub.2qO).sub.rR.sup.3, or CONH(C.sub.qH.sub.2qO).sub.rR.sup.3, M is hydrogen, a monovalent or divalent metal cation, ammonium ion or an organic amine radical, a is or 1, R.sup.3 is hydrogen, an aliphatic hydrocarbon radical having from 1 to 20 carbon atoms, a cycloaliphatic hydrocarbon radical having from 5 to 8 carbon atoms, or an optionally substituted aryl radical having from 6 to 14 carbon atoms, the indices q are, independently of one another, identical or different for each (C.sub.qH.sub.2qO) unit and are each 2, 3 or 4 and r is from 0 to 200, Z is O, or NR.sup.3, ##STR00006## where R.sup.4 and R.sup.5 are each, independently of one another, hydrogen or an aliphatic hydrocarbon radical having from 1 to 20 carbon atoms, a cycloaliphatic hydrocarbon radical having from 5 to 8 carbon atoms, or an optionally substituted aryl radical having from 6 to 14 carbon atoms, the radicals Q are identical or different and are each NH, NR.sup.3 or O, where R.sup.3 is as defined above, the radicals R.sup.6 are identical or different and are each (C.sub.nH.sub.2n)SO.sub.3H where n=0, 1, 2, 3 or 4, (C.sub.nH.sub.2n)OH where n=0, 1, 2, 3 or 4; (C.sub.nH.sub.2n)PO.sub.3H.sub.2 where n=0, 1, 2, 3 or 4, (C.sub.nH.sub.2n)OPO.sub.3H.sub.2 where n=0, 1, 2, 3 or 4, (C.sub.6H.sub.4)SO.sub.3H, (C.sub.6H.sub.4)PO.sub.3H.sub.2, (C.sub.6H.sub.4)OPO.sub.3H.sub.2 or (C.sub.nH.sub.2n)NR.sup.8.sub.b where n=0, 1, 2, 3 or 4 and b=2 or 3, R.sup.7 is H, COOM.sub.a, COO(C.sub.qH.sub.2qO).sub.rR.sup.3, or CONH(C.sub.qH.sub.2qO).sub.rR.sup.3, where M.sub.a, R.sup.3, q and r are as defined above, R.sup.8 is hydrogen, an aliphatic hydrocarbon radical having from 1 to 10 carbon atoms, a cycloaliphatic hydrocarbon radical having from 5 to 8 carbon atoms, or an optionally substituted aryl radical having from 6 to 14 carbon atoms.

8. The pulverulent composition according to claim 1, characterized in that the proportion of the monomer (II) in the copolymer is from 1 to 89 mol %.

9. The pulverulent composition according to claim 1, characterized in that the ethylenically unsaturated monomer (II) is represented by the following general formula ##STR00007## where p is an integer from 0 to 6, y is 0 or 1, v is an integer from 3 to 500, the indices w are, independently of one another, identical or different for each (C.sub.wH.sub.2wO) unit and are each an integer from 2 to 18, where R.sup.1, R.sup.2 are each, independently of one another, hydrogen or an aliphatic hydrocarbon radical having from 1 to 20 carbon atoms, and R.sup.3 is hydrogen, an aliphatic hydrocarbon radical having from 1 to 20 carbon atoms, a cycloaliphatic hydrocarbon radical having from 5 to 8 carbon atoms, or an optionally substituted aryl radical having from 6 to 14 carbon atoms.

10. The pulverulent composition according to claim 9, characterized in that, in the general formula (II), p is an integer from 0 to 4, v is an integer from 5 to 500, the indices w are, independently of one another, identical or different for each (C.sub.wH.sub.2wO) unit and are each 2 or 3.

11. The pulverulent composition according to claim 1, characterized in that the organic solvent is at least one solvent selected from the group consisting of ethyl acetate, 1-methoxy-2-propyl acetate, ethanol, i-propanol, n-butanol, 2-ethylhexanol, 1-methoxy-2-propanol, ethylene glycol, propylene glycol, acetone, butanone, pentanone, hexanone, methyl ethyl ketone, butyl acetate, amyl acetate, tetrahydrofuran, diethyl ether, toluene, xylene and higher-boiling alkylbenzenes, polyethylene glycol ethers and polypropylene glycol ethers and random ethylene oxide-propylene oxide copolymers having an average molar mass in the range from 200 to 2000 g/mol, monoethylene, diethylene or triethylene glycol, monopropylene, dipropylene or tripropylene glycol, methylpolyalkylene, ethylpolyalkylene, propylpolyalkylene, butylpolyalkylene and higher alkylpolyalkylene glycol ethers having 1, 2, 3 or more ethylene glycol and/or propylene glycol units, glycerol ethoxylates having a molecular weight of from 200 to 20 000 g/mol, pentaerythritol alkoxylates, ethylene carbonate, propylene carbonate, glyceryl carbonate, glycerol formal and 2,3-O-isopropylideneglycerol.

12. The pulverulent composition according to claim 1, characterized in that the organic solvent is n-butyl acetate.

13. The pulverulent composition according to claim 1, characterized in that the composition is a factory dry mortar, a bricklaying mortar, render mortar, mortar for composite thermal insulation systems, renovation mortar, joint grout, tile adhesive, thin bed mortar, screed mortar, embedding mortar, injection mortar, knifing filler, sealing slurry or lining mortar.

Description

EXAMPLES

Example 1

Preparation of the Polycarboxylate Ether

(1) 385 g of water, 350 g (0.12 mol) of polyethylene glycol-41-3000-hydroxybutylmonovinyl ether (20% of PO, random) are placed in a 1000 ml four-necked flask provided with thermometer, pH meter and reflux condenser.

(2) This mixture is cooled to 15 C. 0.5 g of 2% strength FeSO.sub.4*18H.sub.2O solution and 42.4 g (0.59 mol) of 99% strength acrylic acid are then added. 1.8 g of mercaptoethanol and 5 g of Brggolit FF6 are then added. A pH of about 4.6 is then established. After a mixing time of 2 minutes, 2.5 g of 50% strength H.sub.2O.sub.2 solution are added. After a short time, the polymerization commences and the temperature increases steadily. After about 2 minutes, the reaction reaches the temperature maximum of about 42 C. and a pH of 4.2. After a further 5 minutes, the mixture is brought to pH=5.5 by means of 30 g of 20% strength NaOH solution. This gives a slightly yellowish, clear aqueous polymer solution having a solids content of 51% by weight.

Example 2

Production of the Polycarboxylate Ether Solution in Methylpolyethylene Glycol 500

(3) 588 g of the 51% strength aqueous polycarboxylate ether solution from example 1 are weighed into a 2000 ml round-bottomed flask. 700 g of methylpolyethylene glycol 500 (Pluriol A 500 E from BASF SE) are added. The water is then taken off at 70 C. and 40 mbar by means of a rotary evaporator. At a water content of less than 1% by weight, the evaporation is stopped and the mixture is cooled. The resulting solution is slightly opalescent and has an active compound content of 30% by weight.

Example 3

Production of the Polycarboxylate Ether Solution in Propylene Carbonate

(4) 980 g of the 51% strength aqueous polycarboxylate ether solution from example 1 are weighed into a 2000 ml round-bottomed flask. 500 g of propylene carbonate are then added. The water is then taken off at 70 C. and 40 mbar by means of a rotary evaporator. At a water content of less than 1% by weight, the evaporation is stopped and the mixture is cooled. The resulting solution is slightly opalescent and has an active compound content of 50% by weight.

Example 4

Production of the Polycarboxylate Ether Solution in Methylpolyethylene Glycol 500/Glyceryl Carbonate

(5) 980 g of the 51% strength aqueous polycarboxylate ether solution from example 1 are weighed into a 2000 ml round-bottomed flask. 500 g of methylpolyethylene glycol 500 (Pluriol A 500 E from BASF SE)/glyceryl carbonate mixture (7:3) are then introduced. The water is subsequently taken off at 75 C. and 100 mbar by means of a thin film evaporator. At a water content of less than 2% by weight, the evaporation is stopped and the mixture is cooled. The resulting solution is slightly opalescent and has an active compound content of 50% by weight.

Use Example 1

(6) The following pulverulent composition as test formulation (99.80% by weight) using 0.20% by weight of PCE plasticizer (at make-up water values of about 18% by weight based on 100% by weight of dry mortar) serves for determining the mixing rate:

(7) TABLE-US-00001 Starting material Manufacturer Function % by wt. Omyacarb 6AL Omya GmbH Filler 10.00 Omyacarb 20 BG Omya GmbH Filler 15.00 Omyacarb 130 AL Omya GmbH Filler 26.43 Milke Classic Heidelberg Inorganic binder 30.00 Cement AG Ciment Fondu Kerneos Inc. Inorganic binder 10.00 Ca(SO).sub.4 (anhydrite) CAB 30, Lanxess Inorganic binder 6.00 AG Vinnapas 5023L Wacker Organic binder 2.00 Tartaric acid UD Chemie GmbH Retarder 0.12 Lithium carbonate Chemmetall GmbH Accelerator 0.10 Vinapor DF 9010 F BASF Construction Antifoam 0.15 Polymers GmbH 99.80

(8) 299.4 g of the pulverulent composition is treated with 2 g (0.67% by weight based on the dry mortar weight) of a solution from Example 2 (corresponding to 0.2% by weight of dispersant and 0.47% by weight of solvent). To assess the mixability, 300 g of the treated pulverulent composition are placed in a beaker and stirred at 500 revolutions per minute by means of a three-blade axial stirrer. The liquid (54 g of water corresponding to 18% by weight based on the dry mortar weight) is then added and the time after which the fresh mortar visually has a homogeneous consistency is measured. This test mixture requires 8 seconds until a homogeneous consistency is achieved while stirring continually (at 500 revolutions per minute).

(9) An identical pulverulent composition in the case of which the identical dispersant (0.6 g corresponding to 0.2% by weight based on the dry mortar weight) is added in powder form serves as comparison. This homogenized mixture is likewise stirred at 500 revolutions per minute by means of an axial stirrer. The liquid is then added. 54 g of water and 1.4 g of methylpolyethylene glycol 500 (Pluriol A 500 E from BASF SE) serve as liquid. This mixture then contains, as in the use example according to the invention, 0.6 g of plasticizer and 1.4 g of solvent in addition to the powder mixture. After addition of the liquid, the mortar requires 16 seconds until a homogeneous consistency is achieved.

Use Example 2

Pulverulent Composition

(10) TABLE-US-00002 Starting material Manufacturer Function % by wt. Omyacarb 6AL Omya GmbH Filler 10.00 Omyacarb 20 BG Omya GmbH Filler 15.00 Omyacarb 130 AL Omya GmbH Filler 26.48 Milke Classic Heidelberg Inorganic Binder 30.00 Cement AG Ciment Fondu Kerneos Inc. Inorganic Binder 10.00 Ca(SO).sub.4 (anhydrite) CAB 30, Lanxess Inorganic Binder 6.00 AG Starvis 3003 F BASF Construction Sedimentation 0.15 Polymers GmbH Inhibitor Vinnapas 5023L Wacker Organic Binder 2.00 Tartaric acid UD Chemie GmbH Retarder 0.12 Lithium carbonate Chemmetall GmbH Accelerator 0.10 Vinapor DF 9010 F BASF Construction Antifoam 0.15 Polymers GmbH 100.00

(11) 300 g of the pulverulent composition is treated with 2.0 g (0.67% by weight based on the dry mortar weight) of a solution from example 2 (corresponding to 0.20% by weight of dispersant and 0.47% by weight of solvent). To assess the mixability, 300 g of the treated pulverulent composition are placed in a beaker and stirred at 500 revolutions per minute by means of an axial stirrer. The liquid (63 g of water corresponding to 21% by weight based on the dry mortar weight) is then added and the time after which the fresh mortar visually has a homogeneous consistency is measured. This test mixture takes 9 seconds until a homogeneous consistency is achieved.

(12) An identical pulverulent composition in the case of which the identical dispersant (0.6 g corresponding to 0.20% by weight based on the dry mortar weight) has been added in powder form serves as comparison. This homogenized mixture is likewise stirred at 500 revolutions per minute by means of an axial stirrer. The liquid is then added. 63 g of water and 1.4 g of methylpolyethylene glycol 500 (Pluriol A 500 E from BASF SE) serve as liquid. This mixture then contains, as in the use example according to the invention, 0.6 g of plasticizer and 1.4 g of solvent in addition to the powder mixture. After addition of the liquid, the mortar requires 18 seconds until a homogeneous consistency is achieved.

Use Example 3

Refractory Mortar

(13) Pulverulent Composition

(14) TABLE-US-00003 Starting material Manufacturer Function % by wt. Omyacarb 6AL Omya GmbH Filler 10 Omyacarb 20 BG Omya GmbH Filler 15 Omyacarb 130 Omya GmbH Filler 27 AL CA 270 Almatis GmbH Inorganic Binder 11 CTC 50 Almatis GmbH Filler 37 100

(15) 300 g of the pulverulent composition is treated with 2.0 g (0.67% by weight based on the dry mortar weight) of a solution from example 2 (corresponding to 0.20% by weight of dispersant and 0.47% by weight of solvent). To assess the mixability, 300 g of the treated pulverulent composition are placed in a beaker and stirred at 500 revolutions per minute by means of an axial stirrer. The liquid (62 g of water corresponding to 22% by weight based on the dry mortar weight) is then added and the time after which the fresh mortar visually has a homogeneous consistency is measured. This test mixture takes 5 seconds until a homogeneous consistency is achieved.

(16) An identical pulverulent composition in the case of which the identical dispersant (0.6 g corresponding to 0.20% by weight based on the dry mortar weight) has been added in powder form serves as comparison. This homogenized mixture is likewise stirred at 500 revolutions per minute by means of an axial stirrer. The liquid is then added. 66 g of water and 1.4 g of methylpolyethylene glycol 500 (Pluriol A 500 E from BASF SE) serve as liquid. This mixture then contains, as in the use example according to the invention, 0.6 g of plasticizer and 1.4 g of solvent in addition to the powder mixture. After addition of the liquid, the mortar requires 9 seconds until a homogeneous consistency is achieved.

Use Example 4

(17) 32.92 kg of stucco plaster (-calcium sulfate hemihydrate) are sprayed with 987.57 g of a solution of a polycarboxylate ether in methylpolyethylene glycol 500 (active compound content 10% by weight) produced by a method analogous to example 2 in a Ldige mixer. The polycarboxylate ether solution is metered by means of an airless pump from Graco. The entry pressure is about 1.5 bar and the metering rate is about 320 ml/min. The metered addition commences at an initial temperature of 27 C. and ends at a temperature of 39 C. During the metered addition, the Ldige mixer is operated at a rotation rate of 188 rpm and the cutter head is set to the setting 2. The amount of polycarboxylate ether solution sprayed in is determined by means of a flow meter. To observe the mixing process, the front lid is replaced by a Plexiglas lid. After the metered addition, stirring is continued for a further 10 minutes to give a homogeneous mixture.

(18) To assess the mixability with water, 103 g of the treated stucco plaster are initially homogenized with 100 g of ground limestone (Omyacarb 6AL) and placed in a beaker. While mixing the pulverulent constituents at 200 revolutions per minute by means of an axial stirrer, the make-up water (58 g) is added. The time after which the fresh mortar visually has a homogeneous consistency is subsequently measured. This mixture according to the invention requires about 4 seconds for this.

Comparative Example

(19) An identical composition composed of 100 g of stucco plaster ((3-calcium sulfate hemihydrate) and 100 g of ground limestone (Omyacarb 6AL) to which the identical dispersant (0.3 g) has been added in powder form serves as comparison. While mixing the pulverulent constituents at 200 revolutions per minute by means of an axial stirrer, the liquid component consisting of make-up water (58 g) and solvent (2.7 g of methylpolyethylene glycol 500) is added. Accordingly, 0.3 g of plasticizer and 2.7 g of solvent are present in addition to the stucco plaster and the ground limestone in the mixture, as in the first example. This reference mixture takes about 7 seconds to reach a homogeneous consistency.