EP4003931A1 - Compositions de gypse - Google Patents

Compositions de gypse

Info

Publication number
EP4003931A1
EP4003931A1 EP20746576.6A EP20746576A EP4003931A1 EP 4003931 A1 EP4003931 A1 EP 4003931A1 EP 20746576 A EP20746576 A EP 20746576A EP 4003931 A1 EP4003931 A1 EP 4003931A1
Authority
EP
European Patent Office
Prior art keywords
gypsum
alkyl
weight
pbw
hydrogenpolysiloxane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20746576.6A
Other languages
German (de)
English (en)
Inventor
Max GIUDICI
Barbara CALLONI
Giuseppe PIRRONE
Alberto CESTONARO
Giovanni Floridi
Giuseppe Li Bassi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lamberti SpA
Original Assignee
Lamberti SpA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lamberti SpA filed Critical Lamberti SpA
Publication of EP4003931A1 publication Critical patent/EP4003931A1/fr
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/38—Polysaccharides or derivatives thereof
    • C04B24/383—Cellulose or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials

Definitions

  • the present invention relates to a method for producing waterproof gypsum products which comprises the use of gypsum compositions comprising an alkyl hydrogenpolysiloxane and a depolymerized carboxymethyl cellulose.
  • the invention also relates to gypsum compositions comprising an alkyl hydrogenpolysiloxane and a depolymerized carboxymethyl cellulose.
  • gypsum Certain properties of gypsum make it very popular for use in making industrial and building products. It is an abundant and inexpensive raw material which, through a process of dehydration and rehydration, can be cast, molded, extruded or otherwise formed into useful products. It is also non-combustible and relatively dimensionally stable.
  • gypsum wallboards also known as plasterboards, which consist of a rehydrated gypsum core sandwiched between multi-ply paper cover sheets, that are commonly used for interior wall and ceiling applications.
  • gypsum products such as wallboards, gypsum tiles, gypsum blocks, gypsum bricks, and the like, are largely hydrophilic and easily absorb water which causes problems of degradation in their thermal insulation and heat retaining properties, generation of cracks, changes in size, etc..
  • Many attempts have been made in the past to reduce the water absorption (waterproofing) of gypsum products by hydrophobization of the gypsum raw materials. These attempts include the addition to the gypsum compositions used for the preparation of gypsum products of water-repellent compounds such as metallic soaps, asphalts, waxes, resins and polysiloxanes, in particular alkyl hydrogenpolysiloxanes.
  • alkyl hydrogenpolysiloxanes to confer waterproofing properties in gypsum-based products is described, for example, in the patents US 3,455,710, EP 0 171 018 and US 5,814,411 among others.
  • H2 hydrogen gas
  • alkyl hydrogenpolysiloxanes are quite efficient water-repellent compounds, but, unfortunately, they are quite expensive and many efforts have been made to find compounds which allowed to reduce the amount of the hydrogen polysiloxanes that are required for giving appropriate waterproofing properties to the gypsum products.
  • Some polysaccharides and/or derivatives thereof are among the compounds described in the art which are able to improve the waterproofing effect of alkyl hydrogenpolysiloxanes
  • WO 99/50200 describes a method for damp-proofing gypsum plaster by adding to the plaster an alkyl hydrogenopolysiloxane and a galactomannan.
  • DE 10 220 659 relates to a composition for rendering gypsum water- repellent comprises an organosiloxane containing Si-bonded hydrogen atoms (hydrogenpolysiloxane) together with a starch ether.
  • US 2009/036572 discloses a method for waterproofing a gypsum-based product formed from a plaster-based composition comprising a linear or cyclic hydrogenpolysiloxane and a pregelified starch.
  • the addition of a specific depolymerized carboxymethyl cellulose markedly improves the performances of the alkyl hydrogenpolysiloxanes and provides to obtain waterproofing results superior to those obtained with other polysaccharides, thus allowing a further optimization of the production costs.
  • the depolymerised carboxymethyl cellulose of the invention is easily soluble in water and it can be provided in the form of pourable concentrated aqueous solutions, allowing faster and easier preparation of gypsum compositions compared to the prior art polysaccharides.
  • KOSi(OH) 2 (CH 2 ) 3 NH 2 KOSi(OH) 2 (CH 2 ) 3 NH 2
  • a hydroxybased cellulose Carboxymethyl cellulose is mentioned among the suitable hydroxybased cellulose, but no further specific information are provided and only hydroxyalkyl or alkyl hydroxyalkyl cellulose were used in the Examples.
  • the waterproofing mechanism of the metal salts of alkylsiliconates is completely different from that of the alkyl hydrogen siloxanes.
  • gypsum includes calcium sulfate hemihydrate, calcined gypsum, anhydrite, stucco and gypsum.
  • gypsum compositions comprising, based on 100 part by weight (pbw) of gypsum, a) from 0.005 to 2 pbw (active substance) of a depolymerized carboxymethyl cellulose (depolymerized CMC) having a weight average molecular weight comprised between 10,000 and 90,000 dalton (Da);
  • gypsum composition comprising, based on 100 pbw of gypsum :
  • the gypsum composition of the invention comprises, based on 100 pbw of gypsum :
  • the weight ratio of depolymerized CMC to alkyl hydrogenpolysiloxane is preferably from 10: 1 to 1 : 10, more preferably from 3: 1 to 1 : 3.
  • the gypsum suitable for the realization of the present invention can be, for example, plaster (CaS04 * l/2H 2 0) in the form of building plaster, plaster of Paris or insulating plaster, or other types of gypsum, such as floor gypsum, Keene's cement, phosphogypsum, FGD gypsum, anhydrite or mixtures of plaster and slaked lime.
  • the gypsum composition comprises more than 60 % by dry weight, preferably more than 80 % by dry weight, of gypsum.
  • the depolymerized CMC has a weight average molecular weight comprised between 15,000 and 50,000 Da, more preferably from 17,000 to 45,000 Da.
  • the molecular weight of the depolymerized CMC is determined by gel permeation chromatography using a 0.1 M aqueous solution of ammonium acetate as eluent and a pullulane standard kit (see Characterization Method).
  • the depolymerized CMC has a degree of substitution (DS) ranging from 0.4 to 1.6, more preferably 0.6 to 1.2.
  • degree of substitution means the number of carboxymethyl groups for each anhydroglycosidic unit of the cellulose; the DS is measured following the ASTM Standard Test Method D1439-
  • the Brookfield viscosity of the depolymerized CMC measured at 20 rpm and 20 °C in water solution at 25 wt% concentration is usually below 6500 mPa * s, preferably below 4000 mPa * s.
  • the depolymerized CMC of the invention is salified with alkali metal ions, such as sodium or potassium, or ammonium or quaternary ammonium ions.
  • alkali metal ions such as sodium or potassium, or ammonium or quaternary ammonium ions.
  • the depolymerized carboxymethyl cellulose of the invention is salified with potassium or sodium ions, more preferably with sodium ions.
  • the depolymerization methods can be applied both on purified or technical grade carboxymethyl cellulose having a DS ranging from 0.4 to 1.6, preferably from 0.6 to 1.2.
  • the depolymerized CMC can be obtained from a technical grade carboxymethyl cellulose having a content of active substance of from 55 to 75 % by dry weight.
  • Technical grade CMC are not washed after the etherification reaction and usually contain from 25 to 45 % by dry weight of the carboxymethylation by-products.
  • These by-products are normally salts of chloride and glycolate, such as sodium chloride and sodium glycolate
  • the depolymerized CMC of the invention is obtained from a purified CMC containing more than 96 by dry weight of active substance.
  • the depolymerized CMC of the invention can be incorporated into the gypsum composition as solid or can be added as a concentrated liquid form.
  • the depolymerized CMC is added as a concentrated aqueous solution containing from 20 to 45 wt% (active substance) of depolymerised CMC, preferably from 27 to 37 wt% (active substance).
  • Any alkyl hydrogenpolysiloxane commonly used in the field can be utilized for the realization of the present invention.
  • the alkyl hydrogenpolysiloxanes described in the above mentioned patents are examples of suitable polysiloxanes.
  • alkyl hydrogenpolysiloxane can be chosen among the linear or cyclic hydrogenopolysiloxanes of Formula (I) or (II) shown below:
  • n and m are integers comprised between 0 and 200 and 1 and 200 respectively, m and q are integers comprised between 1 and 5 and 1 and 10 respectively, with l ⁇ n + m ⁇ 200 and 3 ⁇ p+q ⁇ 10;
  • Ri and F are identical or different and represent independently: • a Ci-Cs linear or branched alkyl group, such as a methyl, ethyl, propyl, isopropyl, n-butyl, sec-butyl, tert-butyl, isobutyl, pentyl, hexyl and octyl group;
  • a Ci-Cs linear or branched alkyl group such as a methyl, ethyl, propyl, isopropyl, n-butyl, sec-butyl, tert-butyl, isobutyl, pentyl, hexyl and octyl group;
  • a C 1 -C 4 alkoxy group such as a methoxy, ethoxy, propoxy, isopropoxy and n-butoxy group;
  • a C 3 -C 10 cycloalkyl group such as a cyclopentyl or cyclohexyl group
  • a C 6 -C 14 aryl group unsubstituted or substituted by at least one Ci- C 4 alkyl radical or a C 2 -C 12 alkenyl radical, such as a phenyl, naphthyl, tolyl, xylyl and ethylphenyl group;
  • a aralkyl group in which the aryl portion is C 6 -C 10 and the alkyl portion is C 1 -C 4 , such as a benzyl, phenylethyl, phenylpropyl or naphthylmethyl group, wherein said aryl groups can be substituted or non-substituted;
  • a C 2 -C 12 alkenyl group such as example a vinyl, allyl or crotonyl group.
  • alkyl hydrogenpolysiloxanes suitable for the realization of the present invention are methyl hydrogenopolysiloxanes such as SILRES® BS 94 and SILRES® BS 46 from Wacker Chemie AG.
  • the alkyl hydrogenpolysiloxane of the invention is used as such in the form of an oil or in the form of an oil-in-water emulsion.
  • the composition can comprise further additives commonly used in the field, such as dispersants, for example polyphosphates or low molecular weight polyacrylic acids, foaming agents, such as ethoxylated alcohols or ethoxylated alcohol sulfates, ethoxylated fatty acids and the like; setting accelerators, such as potassium sulfate and aluminum sulphate; setting retarders, such as proteins or tartaric acid salts; lightening products, rheology modifiers, fillers or fibers, such as silica or cellulose fibers; other functional additives such as starch, silicone oil, waxes and the like.
  • dispersants for example polyphosphates or low molecular weight polyacrylic acids
  • foaming agents such as ethoxylated alcohols or ethoxylated alcohol sulfates, e
  • the gypsum composition can be in the form of powder or of moldable mass.
  • the gypsum composition in the form of moldable mass contains, based on 100 pbw of gypsum, from 30 to 110 pbw, preferably from 40 to 80 pbw, of water.
  • the gypsum composition can be prepared following any conventional method and equipment known in the art.
  • a concentrated solution of depolymeryzed CMC is diluted with water and mixed with the alkyl hydrogenpolysiloxane. Then the dry gypsum powder or a aqueous gypsum slurry is added to this mixture for obtaining, after stirring, the inventive gypsum composition.
  • the gypsum compositions of this invention can be used to prepare waterproof gypsum products, such as cast, molded or extruded articles, for example plasterboards, gypsum tiles and gypsum bricks, or to prepare wallboard coatings and products for filling joints or similar spaces, for example, in preparing filler materials, joint sealants, plaster cements and gypsum plasters.
  • waterproof gypsum products such as cast, molded or extruded articles, for example plasterboards, gypsum tiles and gypsum bricks
  • wallboard coatings and products for filling joints or similar spaces, for example, in preparing filler materials, joint sealants, plaster cements and gypsum plasters.
  • the Brookfield (BRK) viscosity of the CMC solutions was measured with a DV-E Brookfield® viscometer at 20 °C and at 20 rpm.
  • the degree of substitution (DS) of the carboxymethyl cellulose was measured following the ASTM Standard Test Method D1439-03 (Degree of Etherification).
  • the active matter content of the carboxymethyl cellulose is determined following the ASTM Standard Test Method D 1439-03 (Purity).
  • the active matter content of the solution of depolymerized carboxymethyl cellulose was calculated from the matter content subtracting the amount of salts (acids, bases, buffers, and the like) added in the depolymerization process.
  • GPC Gel permeation chromatography
  • the following columns were used at a temperature of 60 °C: SupelcoProgel - TSK G3000 PWXL, G5000 PWXL, G6000 PWXL, and Progel-TSK PWXL guard columns.
  • the HPLC was set at a flow rate of 0.8 ml/min for 50 minutes.
  • Scagliola Extra (CaS0 4* l/2H 2 0 provided from Nuova Siga S.r.L, Italy) was used in all the Examples.
  • gypsum composition of the invention For the preparation of gypsum composition of the invention, an aqueous solutions of depolymerized CMC (D-CMC), obtained by enzymatic depolymerization of a purified sodium CMC having a DS of about 0.75, was used.
  • the solution had a active matter content of 35 wt% and a BRK viscosity of about 4,000 mPa * s.
  • the weight average molecular weight of the CMC obtained from the depolymerisation was about 23,000
  • HPG low viscosity hydroxyl propyl guar
  • MS hydroxypropyl molar substitution
  • the gypsum compositions were prepared by adding the depolymerized CMC solution or the HPG into a plastic beaker containing 330 g of water. The mixture were stirred for about 20 seconds (180 sec for HPG) using a MAVER ALC W 750 rod stirrer equipped with a cowles blade (1400 rpm). Subsequently, an methyl hydrogenpolysyloxane (SILRES® BS 94 from Wacker Chemie AG) was added to the beakers and mixed for another 30 seconds. 750 g of Scagliola Extra were then slowly poured into the mixture to minimize dusting. The gypsum compositions so obtained were mixed for 120 seconds and, after this period, were transferred into disc PVC molds having inside dimensions of 8 cm (diam.) by 4 cm (h.).
  • SILRES® BS 94 from Wacker Chemie AG
  • the gypsum compositions were allowed to solidify in the moulds for 1 hour in a climatic chamber set at 23 °C and 50% humidity.
  • the gypsum discs so obtained were then removed from the molds and transferred in an oven at 40 °C for 24 hours. After the drying step, the discs were removed from the oven and allowed to cool in a desiccator for 1 hour at room temperature.
  • the gypsum discs were then weighed and immersed in water for two hours. After the extraction from water, the discs were allowed to drain and wiped up. Finally, the gypsum discs were weighed to determine the amount of water uptake.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Medicinal Preparation (AREA)

Abstract

La présente invention concerne des compositions de gypse comprenant un alkylhydrogénopolysiloxane et une carboxyméthylcellulose dépolymérisée et un procédé de production de produits de gypse étanches à l'eau, qui comprend l'utilisation desdites compositions de gypse.
EP20746576.6A 2019-07-22 2020-07-17 Compositions de gypse Pending EP4003931A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT102019000012597A IT201900012597A1 (it) 2019-07-22 2019-07-22 Composizioni di gesso
PCT/EP2020/070357 WO2021013751A1 (fr) 2019-07-22 2020-07-17 Compositions de gypse

Publications (1)

Publication Number Publication Date
EP4003931A1 true EP4003931A1 (fr) 2022-06-01

Family

ID=68653506

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20746576.6A Pending EP4003931A1 (fr) 2019-07-22 2020-07-17 Compositions de gypse

Country Status (3)

Country Link
EP (1) EP4003931A1 (fr)
IT (1) IT201900012597A1 (fr)
WO (1) WO2021013751A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115160801A (zh) * 2022-07-20 2022-10-11 江苏博拓新型建筑材料股份有限公司 一种增强型有机硅微胶囊石膏防水乳液及其制备方法与应用

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1223287B (de) 1964-09-04 1966-08-18 Wacker Chemie Gmbh Verfahren zum Herstellen von wasserabweisenden Formkoerpern und UEberzuegen aus anorganischen Massen
DE3429311C1 (de) 1984-08-09 1985-12-05 Bayer Ag, 5090 Leverkusen Verfahren zur Herstellung wasserabweisender poroeser Formkoerper aus Gips
FI895708A0 (fi) 1989-02-10 1989-11-29 Alko Ab Oy Vattenloeslig soenderdelningsprodukt.
ATE167488T1 (de) 1990-07-02 1998-07-15 Aqualon Co Niedrigviskose-polysaccharidzusammensetzung mit hohem festkörpergehalt
US5366810A (en) 1992-10-09 1994-11-22 General Electric Company Water-repellent wallboard
GB9315434D0 (en) 1993-07-26 1993-09-08 Courtaulds Plc Hydrolysis of polysaccharides
DE4434280C2 (de) 1994-09-26 1998-09-10 Clariant Gmbh Verfahren zur Herstellung von niedermolekularen Celluloseethern und ihre Verwendung als Überzugsmaterial für feste Dosiereinheiten
FR2776654B1 (fr) 1998-03-31 2000-06-16 Rhodia Chimie Sa Procede d'hydrofugation du platre mettant en oeuvre au moins un alkylhydrogenopolysiloxane et au moins un hydrocolloide
DE10220659A1 (de) 2002-05-09 2003-11-27 Wacker Chemie Gmbh Behandlung von Gips mit H-Siloxan und Stärkeether
DE10323205A1 (de) * 2003-05-22 2004-12-16 Wacker Polymer Systems Gmbh & Co. Kg Hydrophobierendes Additiv
ITVA20030025A1 (it) 2003-07-17 2005-01-18 Lamberti Spa Depolimerizzazione enzimatica di carbossimetilcellulosa e relativi prodotti.
US7294195B2 (en) 2005-08-08 2007-11-13 Wacker Chemical Corporation Water repellant gypsum compositions
FR2897863B1 (fr) 2006-02-28 2008-07-11 Bpb Plc Procede d'hydrofugation d'un produit a base de gypse forme a partir d'une composition a base de platre

Also Published As

Publication number Publication date
IT201900012597A1 (it) 2021-01-22
WO2021013751A1 (fr) 2021-01-28

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