WO2009130546A1 - Compositions for the sanitizing anti-pollution, water and oil repellent, protective and polishing treatment of stone materials, their preparation and use - Google Patents

Compositions for the sanitizing anti-pollution, water and oil repellent, protective and polishing treatment of stone materials, their preparation and use Download PDF

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Publication number
WO2009130546A1
WO2009130546A1 PCT/IB2008/053933 IB2008053933W WO2009130546A1 WO 2009130546 A1 WO2009130546 A1 WO 2009130546A1 IB 2008053933 W IB2008053933 W IB 2008053933W WO 2009130546 A1 WO2009130546 A1 WO 2009130546A1
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WIPO (PCT)
Prior art keywords
resins
compositions
resin
water
compositions according
Prior art date
Application number
PCT/IB2008/053933
Other languages
French (fr)
Inventor
Giovanni Ottavio Delle Monache
Alessandro Galletto
Original Assignee
Industrial Chem Italia S.R.L.
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
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Application filed by Industrial Chem Italia S.R.L. filed Critical Industrial Chem Italia S.R.L.
Publication of WO2009130546A1 publication Critical patent/WO2009130546A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5042Zirconium oxides or zirconates; Hafnium oxides or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/10Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/18Polyesters; Polycarbonates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/2038Resistance against physical degradation
    • C04B2111/2061Materials containing photocatalysts, e.g. TiO2, for avoiding staining by air pollutants or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/2092Resistance against biological degradation

Definitions

  • the present invention relates to the field of products for the treatment of stone surfaces. State of the art
  • Figure 1 is a graph showing the absorption efficiency to olive oil of a surface treated with a composition according to the invention.
  • Figure 2 is a graph showing the absorption efficiency to Coca Cola ® of a surface treated with a composition according to the invention.
  • Figure 3 is a graph showing the absorption efficiency to coffee of a surface treated with a composition according to the invention.
  • the present invention relates to the production of polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general, also in photosensitive form or their mixtures, with antimicrobial, anti-mould and photocatalytic properties combined with water-oil repellent, protective and polishing properties.
  • the present invention allows the aforesaid problems to be overcome through the use of polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general, also in photosensitive form or mixtures thereof, containing Ti ⁇ 2 , or CuO and/or Ag.
  • Stone materials according to the invention are intended as: marbles, granites, natural stones and their aggregate derivatives, while concrete derivatives are intended as all those products in solid state in which the binder is mixed with water and if necessary with aggregates with various grain sizes.
  • Polyester resins are intended as those commercially available generally obtained through esterification of a mixture of a saturated dibasic acid and of an aliphatic acid with aliphatic glycols; the epoxy resins utilized according to the invention are also those commercially available of the photosetting or thermosetting type obtained through condensation of bisphenol and epichlorhydrine.
  • Fluoropolymers are intended as those commercially available resins (both water and solvent based) containing compounds based on fluorite in its various forms (PTFE, PVDF, PFA, FEP etc.), and in particular acrylic and non-acrylic fluorinated copolymers. Some of these resins are commercially and generically called
  • TiO 2 according to the invention is intended both as the oxide in powder form and dispersions or suspensions thereof, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2-Propanediol, Ethylene Glycol etc.; the oxide can either be in Anatase or Rutile form.
  • Ag can also be utilized both as a metal powder and in dispersions or suspensions, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2- Propanediol, Ethylene Glycol etc.; if preferred inert carriers such as Zeolite can be used; in particular in formulations containing Fluoropolymers or silicone resins, the Ag is present in ionic or metallic form.
  • CuO according to the invention is intended both as the oxide in powder form and in dispersions or suspensions, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2-Propanediol, Ethylene Glycol etc..
  • the compounds according to the invention normally contain a quantity in weight of TiO 2 or CuO between 0.03% and 10%, preferably 0.2% with respect to the resin.
  • the quantity in weight of Ag is between 0.0002% and 2%, preferably 0.05% with respect to the resin in the case of pure Ag.
  • inert carriers such as Zeolite for the Ag
  • their quantity in weight is between 0.1% and 15%, preferably 2.5% with respect to the resin.
  • dispersions of Ag in ionic form the quantity is between 0.0002 % and 5%
  • compositions according to the invention To prepare the compositions according to the invention, the dispersions or powders defined above, obtained on the market or prepared according to known methods, are added to the resins as defined above, also obtained on the market or prepared according to essentially known techniques as described above.
  • the resins thus obtained are applied either prior to, or in an intermediate step of, the smoothing or polishing process, to eliminate defects and control the porosity of the stone materials; they allow the appearance and properties of finished or semifinished stone and cement products to be improved, also making the surfaces sanitizing, easy to maintain and purifying for the surrounding environment.
  • the resins according to the invention can also be used directly in the production processes of aggregates, which employ them as binder.
  • the examples below show how the resins according to the invention were obtained.
  • Photocatalytic epoxy resin The following quantities of raw materials were added to a plastic beaker positioned on a magnetic stirrer under constant stirring using a magnetic bar:
  • the product was applied to marble chip using a brush and left to dry for approximately 48 hours.
  • the product was applied to marble chip using a brush and left to dry for approximately 48 hours.
  • PCA Plate Count Agar
  • SAB c Sabouraud Agar + Chloramphenicol
  • the resin according to example 4 was also tested for oil repellency and resistance to Coca Cola ® and coffee according to the standard ASTM D1308 with results shown in the accompanying graphs.

Abstract

There are described compositions based on polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general in all forms and also in photosensitive form utilizable to improve the appearance and hygiene properties of stone surfaces, processes for their preparation and use.

Description

COMPOSITIONS FOR THE SANITIZING, ANTI-POLLUTION, WATER AND OIL REPELLENT, PROTECTIVE AND POLISHING TREATMENT OF STONE MATERIALS, THEIR PREPARATION AND USE.
Field of the invention The present invention relates to the field of products for the treatment of stone surfaces. State of the art
Processing of stone and concrete derivatives, in general in the form of slabs and marble chips, in the majority of cases requires the surfaces to be treated with resin or the application of coatings and/or impregnating agents in order to protect the materials from dust, liquids, moulds and stains in general, and to repair imperfections such as fractures, porosity, splitting, cavities, etc. Moreover, there is increasing demand for the surfaces of these materials to have antibacterial properties, also in view of the decrease in hygiene standards due to the increase in the volumes of goods handled and to the variety of their sources. Besides these needs, which are intrinsic to the use of the aforesaid materials, a quality required of the surfaces of these materials is that they contribute towards decreasing atmospheric pollution. Currently, after resin coating or final treatment of the materials additional treatments are required to obtain the aforesaid qualities, in which the surfaces are treated with products capable of performing the aforesaid action (such as solutions containing TiO2, the photocatalytic and antibacterial properties of which are well- known). In view of the above, there is obviously an interest in developing products that allow the desired effects to be obtained without the additional treatments currently necessary and at the same time without having to substantially modify the technological process currently employed in operations to perform resin coating or final treatment of materials with any surface finish. Brief description of the Figures Figure 1 is a graph showing the absorption efficiency to olive oil of a surface treated with a composition according to the invention. Figure 2 is a graph showing the absorption efficiency to Coca Cola® of a surface treated with a composition according to the invention.
Figure 3 is a graph showing the absorption efficiency to coffee of a surface treated with a composition according to the invention.
Summary of the invention The present invention relates to the production of polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general, also in photosensitive form or their mixtures, with antimicrobial, anti-mould and photocatalytic properties combined with water-oil repellent, protective and polishing properties.
Detailed description of the invention The present invention allows the aforesaid problems to be overcome through the use of polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general, also in photosensitive form or mixtures thereof, containing Tiθ2, or CuO and/or Ag.
Stone materials according to the invention are intended as: marbles, granites, natural stones and their aggregate derivatives, while concrete derivatives are intended as all those products in solid state in which the binder is mixed with water and if necessary with aggregates with various grain sizes.
Polyester resins are intended as those commercially available generally obtained through esterification of a mixture of a saturated dibasic acid and of an aliphatic acid with aliphatic glycols; the epoxy resins utilized according to the invention are also those commercially available of the photosetting or thermosetting type obtained through condensation of bisphenol and epichlorhydrine.
Fluoropolymers are intended as those commercially available resins (both water and solvent based) containing compounds based on fluorite in its various forms (PTFE, PVDF, PFA, FEP etc.), and in particular acrylic and non-acrylic fluorinated copolymers. Some of these resins are commercially and generically called
Teflon®.
Silicone resins are intended as those commercially available resins (both water and solvent based) composed in general by cage-like oligosiloxanes (commercially called silanes or siloxanes in general) in the general formula of the type RnSiXmOy1 where R is a non-reactive group (typically Methyl or Phenyl group) and X is a functional group (H, OH, Cl or alkoxyl group) and where n = 0, 1 , 2, 3, 4; m = 0, 1 , 2, 3, 4; Y = 0, 1 , 2, 3, 4
TiO2 according to the invention is intended both as the oxide in powder form and dispersions or suspensions thereof, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2-Propanediol, Ethylene Glycol etc.; the oxide can either be in Anatase or Rutile form.
Ag can also be utilized both as a metal powder and in dispersions or suspensions, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2- Propanediol, Ethylene Glycol etc.; if preferred inert carriers such as Zeolite can be used; in particular in formulations containing Fluoropolymers or silicone resins, the Ag is present in ionic or metallic form.
CuO according to the invention is intended both as the oxide in powder form and in dispersions or suspensions, such as colloidal dispersions, in water or other solvents, such as 2-propanol, 1 ,2-Propanediol, Ethylene Glycol etc.. The compounds according to the invention normally contain a quantity in weight of TiO2 or CuO between 0.03% and 10%, preferably 0.2% with respect to the resin. The quantity in weight of Ag is between 0.0002% and 2%, preferably 0.05% with respect to the resin in the case of pure Ag.
Employing inert carriers such as Zeolite for the Ag, their quantity in weight is between 0.1% and 15%, preferably 2.5% with respect to the resin. In the case of dispersions of Ag in ionic form the quantity is between 0.0002 % and 5%
To prepare the compositions according to the invention, the dispersions or powders defined above, obtained on the market or prepared according to known methods, are added to the resins as defined above, also obtained on the market or prepared according to essentially known techniques as described above.
The resins thus obtained are applied either prior to, or in an intermediate step of, the smoothing or polishing process, to eliminate defects and control the porosity of the stone materials; they allow the appearance and properties of finished or semifinished stone and cement products to be improved, also making the surfaces sanitizing, easy to maintain and purifying for the surrounding environment.
The resins according to the invention can also be used directly in the production processes of aggregates, which employ them as binder. The examples below show how the resins according to the invention were obtained.
Example 1
Photocatalytic epoxy resin The following quantities of raw materials were added to a plastic beaker positioned on a magnetic stirrer under constant stirring using a magnetic bar:
99 g Bond epoxy resin Industrial Chem Italia
1 g Dispersion in 1.2 propandiol of nanometric Rutile TiO2 15 nm
20% in weight The following was added after approximately one hour under constant stirring
46 g Hardener Bond Industrial Chem Italia
Subsequently, the product was applied to marble chip using a brush and left to dry for approximately 48 hours.
Example 2 Antibacterial epoxy resin
The following quantities of raw materials were added to a plastic beaker positioned on a magnetic stirrer under constant stirring using a magnetic bar:
96 g Bond epoxy resin Industrial Chem Italia
4 g Ag in zeolite powder The following was added after approximately one hour under constant stirring
46 g Hardener Bond Industrial Chem Italia
Subsequently, the product was applied to marble chip using a brush and left to dry for approximately 48 hours.
Example 3 High penetration antibacterial epoxy resin
The following quantities of raw materials were added to a plastic beaker positioned on a magnetic stirrer under constant stirring using a magnetic bar:
76 g Bond epoxy resin Industrial Chem Italia
25 g Fluid Bond fluidifier Industrial Chem Italia 4 g Ag in Zeolite powder
The following was added after approximately one hour under constant stirring
46 g Hardener Bond Industrial Chem Italia Example 4
Water-based antibacterial water and oil repellent product
The following quantities of raw materials were added to a plastic beaker positioned on a magnetic stirrer under constant stirring using a magnetic bar: 80 g of distilled water
20 g fluoropolymer SiI 87
0.2 g nanometric Ag aqueous suspension 5%
0.1 g Ag ion solution 2.5%
The resins thus obtained were applied to a stone aggregate in the intermediate polishing step (examples 1-2 and 3) and to polished granite (example 4).
The antibacterial tests (48 h in oven with Plate Count Agar (PCA) culture media for psychrophilic bacteria count and Sabouraud Agar + Chloramphenicol (SAB c) total fungal count with inhibition of contaminating bacterial flora), were performed on samples taken to final polishing normally exposed to natural radiation on a day that was not particularly sunny with the following results:
Resin according to example 1
PCA: 1 CFU/plate = 0.02 CFU/cm2
SAB: 0 CFU/plate = 0 CFU/cm2
Resin according to example 2 PCA : 19 CFU /plate = 0.45 CFU/cm2
SAB: 7 CFU/plate = 0.2 CFU/cm2
Resin according to example 3
PCA : 35 CFU/plate = 0.6/cm2
SAB: 14 CFU/plate = 0.4/cm2 Resin according to example 4 (applied to sample of "Kashmir White" polished granite)
PCA : 42 CFU/plate = 0.7/cm2
SAB: 22 CFU/plate = 0.4/cm2
The resin according to example 4 was also tested for oil repellency and resistance to Coca Cola® and coffee according to the standard ASTM D1308 with results shown in the accompanying graphs.
Comparing the CFU values measured with the IMA table of limit values indicated in the INAIL (national institute for insurance against industrial accidents) guidelines for microbiological monitoring of workplaces, it can be seen that: a) performances of the resin according to example 1 in the presence of adequate irradiation are compatible with use in ultra clean rooms (protective isolation, operating theatres for ear prostheses, some electronic and pharmaceutical industry processes); b) performances of the resin according to example 2 are compatible with use in clean rooms (operating theatres for general surgery, intensive care, dialysis, some electronic and pharmaceutical industry processes, microbiology laboratories); c) performances of the resin according to example 3 are compatible with use in doctor's surgeries, laboratories, food industries, kitchens, restaurants, factories; d) performances of the resin according to example 4 are compatible with use in doctor's surgeries, laboratories, food industries, kitchens, restaurants, factories. The resin also shows exceptional resistance to absorption of oil and Coca
Cola® and high resistance to absorption of coffee.

Claims

1. Compositions for the treatment of stone surfaces or materials comprising polyester, epoxy, polyurethane, fluoropolymer resins and silicone resins in general, also in photosensitive form or their mixtures, containing TiO2, or CuO and/or Ag.
2. Compositions according to claim 1 , wherein said polyester resins are conventional resins obtained through esterification of a mixture of a saturated dibasic acid and of an aliphatic acid with aliphatic glycols.
3. Compositions according to claim 1 , wherein said polyester resins utilized are conventional resins of the photosetting or thermosetting type obtained through condensation of bisphenol and epichlorhydrine.
4. Compositions according to claims 1 - 3, wherein said TiO2 or CuO is composed of oxide in powder form or dispersions or suspensions thereof in water or other solvents.
5. Compositions according to claims 1 - 4, wherein the Ag is composed of a metallic powder or dispersions or suspensions thereof in water or other solvents, if necessary in the presence of inert carriers or is present in ionic form.
6. Composition according to claim 1 - 5, wherein the quantity in weight of TiO2 or CuO is between 0.03% and 10%, preferably 0.2% with respect to the resin.
7. Composition according to claims 1 - 6, wherein the quantity in weight of Ag is between 0.0002% and 2%, preferably 0.05% with respect to the resin in the case of pure Ag, while when carriers are used their quantity in weight is between 0.1 - 15%, preferably 2.5% with respect to the resin.
8. Composition according to claims 1 - 6, wherein the Ag is present in ionic form and in quantities between 0.0002 % and 5%.
9. Process for the preparation of resins according to claims 1 - 8, wherein said dispersions or said powders are added to said resins according to known methodologies.
10. Process for the treatment of stone materials wherein the compositions according to claim 1 - 8 are applied prior to, or in an or in an intermediate step of, the smoothing or polishing process, of the stone material.
11. Process according to claim 10, wherein said stone materials are marbles, granites, natural stones, their aggregate derivatives, and concrete derivatives.
12. Concrete derivatives comprising the compositions according to claims 1 - 8 as binders.
13. Process for the production of concrete derivatives according to claim 12 wherein the resins according to claims 1 - 8 are employed directly as binders to form the relative aggregates.
PCT/IB2008/053933 2008-04-24 2008-09-26 Compositions for the sanitizing anti-pollution, water and oil repellent, protective and polishing treatment of stone materials, their preparation and use WO2009130546A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITFI2008A000085 2008-04-24
ITFI20080085 ITFI20080085A1 (en) 2008-04-24 2008-04-24 COMPOSITIONS FOR SANITIZING AND ANTI-POLLUTION TREATMENT OF STONE MATERIALS, THEIR PREPARATION AND USE.

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2607318A4 (en) * 2010-08-17 2015-08-05 Sakai Chemical Industry Co Method for producing dispersion of rutile-type titanium oxide particles
ES2571180A1 (en) * 2014-11-20 2016-05-24 Canto Leopoldo Diez Improved procedure for the treatment of ornamental stones and ornamental stone obtained from it (Machine-translation by Google Translate, not legally binding)
EP2662348A3 (en) * 2012-05-06 2016-05-25 EGC SEED CAPITAL Sp. z.o.o. A method for manufacturing of resin-coated stone slabs
CN113582721A (en) * 2021-08-03 2021-11-02 童晓斐 Control panel and manufacturing process thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2607318A4 (en) * 2010-08-17 2015-08-05 Sakai Chemical Industry Co Method for producing dispersion of rutile-type titanium oxide particles
EP2662348A3 (en) * 2012-05-06 2016-05-25 EGC SEED CAPITAL Sp. z.o.o. A method for manufacturing of resin-coated stone slabs
ES2571180A1 (en) * 2014-11-20 2016-05-24 Canto Leopoldo Diez Improved procedure for the treatment of ornamental stones and ornamental stone obtained from it (Machine-translation by Google Translate, not legally binding)
CN113582721A (en) * 2021-08-03 2021-11-02 童晓斐 Control panel and manufacturing process thereof

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