WO2021197633A1 - Système de toit - Google Patents

Système de toit Download PDF

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Publication number
WO2021197633A1
WO2021197633A1 PCT/EP2020/059655 EP2020059655W WO2021197633A1 WO 2021197633 A1 WO2021197633 A1 WO 2021197633A1 EP 2020059655 W EP2020059655 W EP 2020059655W WO 2021197633 A1 WO2021197633 A1 WO 2021197633A1
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WO
WIPO (PCT)
Prior art keywords
component
water
roof structure
flat roof
structure according
Prior art date
Application number
PCT/EP2020/059655
Other languages
English (en)
Inventor
Dorte Bartnik JOHANSSON
Miroslav Nikolic
Charlotte LIND
Original Assignee
Rockwool International A/S
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 Rockwool International A/S filed Critical Rockwool International A/S
Priority to PCT/EP2020/059655 priority Critical patent/WO2021197633A1/fr
Publication of WO2021197633A1 publication Critical patent/WO2021197633A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
    • C03C25/26—Macromolecular compounds or prepolymers
    • C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/005—Lignin
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
    • E04D11/00—Roof covering, as far as not restricted to features covered by only one of groups E04D1/00 - E04D9/00; Roof covering in ways not provided for by groups E04D1/00 - E04D9/00, e.g. built-up roofs, elevated load-supporting roof coverings
    • E04D11/002—Roof covering, as far as not restricted to features covered by only one of groups E04D1/00 - E04D9/00; Roof covering in ways not provided for by groups E04D1/00 - E04D9/00, e.g. built-up roofs, elevated load-supporting roof coverings consisting of two or more layers, at least one of the layers permitting turfing of the roof
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
    • E04D11/00—Roof covering, as far as not restricted to features covered by only one of groups E04D1/00 - E04D9/00; Roof covering in ways not provided for by groups E04D1/00 - E04D9/00, e.g. built-up roofs, elevated load-supporting roof coverings
    • E04D11/02—Build-up roofs, i.e. consisting of two or more layers bonded together in situ, at least one of the layers being of watertight composition
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
    • E04D13/00—Special arrangements or devices in connection with roof coverings; Protection against birds; Roof drainage ; Sky-lights
    • E04D13/04—Roof drainage; Drainage fittings in flat roofs, balconies or the like
    • E04D13/0404—Drainage on the roof surface
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A30/00—Adapting or protecting infrastructure or their operation
    • Y02A30/24—Structural elements or technologies for improving thermal insulation
    • Y02A30/254—Roof garden systems; Roof coverings with high solar reflectance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
    • Y02B80/32—Roof garden systems

Definitions

  • the invention relates to roof systems of the type commonly known as “blue roofs”, which comprise a water attenuation layer formed of a matrix of man-made vitreous fibres (MMVF) bonded with a cured binder composition.
  • blue roofs In urban areas with a large number of buildings and pavings, flooding risk is high. When rain is heavy then a high volume of water reaches buildings and from there the ground in a short time. Often sewers cannot cope with extreme amounts of water in such a short time, resulting in flooding.
  • the use of a blue roof provides means for storing or buffering water on flat roofs, thus attenuating the arrival of water into the sewers, waterways and river systems.
  • Blue roof structures which are flat roofs designed to allow attenuation of rainfall during heavy rain and storm events.
  • a blue roof will release water at a managed and controlled rate into the sewers, waterways and river systems around the building having the blue roof.
  • Blue roofs are described by the National Federation of roofing Contractors Limited (NFRC) in their NFCR Technical Guidance Note for the construction and design of blue roofs.
  • a blue roof comprises a water attenuation layer which is formed of a material which absorbs and holds incoming rain water and subsequently releases it for discharge at a controlled rate.
  • the water attenuation layer is formed of water retention elements of the honeycomb type made out of e.g. polypropylene.
  • An example is Nophadrain ND WSE-70.
  • W02020/018599A2 describes a green roof structure which can also have blue roof functionality.
  • a green roof is a flat roof having capability to support plant growth.
  • the structure comprises a load layer which can be a plant growth layer and a retention layer configured to retain storm water.
  • Mineral wool is mentioned as a possible component for a layer for the roof.
  • W02020/058384 describes a blue roof including the option for the water storage component to be formed of mineral wool.
  • ACO SpongeTop
  • the attenuation layer is formed of plates of hydrophilic compression-resistant stone wool plates.
  • the hydrophilic stone wool plates hold and buffer water and release it either by evaporation or by controlled discharge from the roof.
  • Bonded MMVF such as stone wool
  • products are generally produced by converting a melt made of suitable raw materials to fibres in conventional manner.
  • the fibres are blown into a forming chamber and, while airborne and while still hot, are sprayed with a binder solution and deposited as a mat or web onto a travelling conveyor.
  • the fibre mat is then transferred to a curing oven where heated air is blown through the mat to cure the binder and rigidly bond the mineral fibres together.
  • the binder resins of choice have been phenol-formaldehyde resins which can be economically produced and can be extended with urea prior to use as a binder.
  • formaldehyde-free binders such as, for instance, the binder compositions based on polycarboxy polymers and polyols or polyamines, such as disclosed in EP-A-583086, EP-A-990727, EP-A-1741726, US-A-5, 318,990 and US-A- 2007/0173588.
  • non-phenol-formaldehyde binders are the addition/-elimination reaction products of aliphatic and/or aromatic anhydrides with alkanolamines, e.g., as disclosed in WO 99/36368, WO 01/05725, WO 01/96460, WO 02/06178,
  • WO 2008/023032 discloses urea-modified binders of that type which provide mineral wool products having reduced moisture take-up. Since some of the starting materials used in the production of these binders are rather expensive chemicals, there is an ongoing need to provide formaldehyde- free binders which are economically produced.
  • a further effect in connection with previously known aqueous binder compositions from mineral fibres is that at least the majority of the starting materials used for the productions of these binders stem from fossil fuels.
  • a further effect in connection with previously known aqueous binder compositions for mineral fibres is that they involve components which are corrosive and/or harmful. This requires protective measures for the machinery involved in the production of mineral wool products to prevent corrosion and also requires safety measures for the persons handling this machinery. This leads to increased costs and health issues and there is therefore a need to provide binder compositions for mineral fibres with a reduced content of corrosive and/or harmful materials.
  • known MMVF products for water absorption but used in applications other than blue roofs can contain wetting agents to improve hydrophilicity.
  • certain wetting agents may be washed out of the MMVF product over time. This is particularly problematic as the wetting agent may leach out and contaminate the surrounding ground.
  • the wetting agent is washed out, the water holding properties of the device can significantly change.
  • MMVF water attenuation elements comprising a binder that is formaldehyde-free but has equivalent or superior mechanical handling properties (e.g. compression strength) as phenol-formaldehyde binders. It would be desirable for such elements to have improved water holding properties (e.g. improved drainage, water buffering, and infiltration). Furthermore, it would be desirable for such a binder to be economical to produce and be based predominantly on renewable sources. Finally, it would be desirable for such a binder to be such that the element does not require the further addition of wetting agent and thus prevent leaching of wetting agents into the surrounding ground.
  • a flat roof structure comprising at least one water attenuation layer comprising at least one water attenuation element formed of man-made vitreous fibres (MMVF) bonded with a cured aqueous binder composition, wherein the aqueous binder composition prior to curing comprises: a component (i) in form of one or more oxidized lignins; a component (ii) in form of one or more cross-linkers; a component (iii) in form of one or more plasticizers. , a waterproof layer below the water attenuation layer, and at least one drainage point in fluid communication with the water attenuation layer and arranged to direct water away from the flat roof structure.
  • MMVF man-made vitreous fibres
  • the material that forms the water attenuation layer is MMVF, bonded with the defined aqueous binder composition.
  • the MMVF structure has the capacity to absorb and hold water for a considerable period of time. It also, however, has the ability to release the water with a certain delay, defined by the so-called discharge rate.
  • Figure 1 shows a section from a possible lignin structure.
  • Figure 2 shows lignin precursors and common inter-unit linkages.
  • Figure 3 shows four groups of technical lignins available in the market.
  • Figure 4 shows a summary of the properties of technical lignins.
  • Figures 5A to 5E show the results of compression strength tests.
  • Figure 6 shows the results of average water buffering.
  • Figure 7 shows the results of average water drainage.
  • Figure 8 shows the results of average water infiltration/discharge.
  • Figure 9 shows a typical warm roof structure incorporating the water attenuation layer of the invention.
  • the flat roof structure has the technical characteristics described in the NFRC Guideline mentioned above and should preferably attenuate water for no more than a 24-hour period from the end of the maximum designed rainfall event.
  • the discharge rate should preferably be calculated to allow the roof to be half empty of attenuated water in a 12-hour period.
  • the overall discharge rate can preferably be in the range of from 3 to 15 litre per second per hectare, preferably 5 to 8 litre per second per hectare of site surrounding the building having the flat roof.
  • the elements of the flat roof structure must have the correct structural capacity to resist the permanent (dead) load of the required finishes and any temporary (live) loading produced by maintenance/emergency vehicles or other elements.
  • the components should be designed to accommodate the full capacity of the predicted storm water for a 24-hour period.
  • the flat roof structure according to the invention comprises a water attenuation element.
  • a water attenuation element Preferably it is formed of an array of water attenuation elements arranged in fluid communication with each other so as to form a continuous layer. Details of preferred aspects of the water attenuation elements are given below.
  • a waterproof layer below the water attenuation layer is arranged a waterproof layer.
  • This can be formed of any of the known materials for providing the waterproof layer in a flat roof.
  • the flat roof structure may comprise other layers above the water attenuation layer, and/or between the water attenuation layer and the waterproof layer, and/or below the waterproof layer, depending on which structure is used.
  • the structure includes a discharge layer below the water attenuation layer. This is generally in fluid communication with the water attenuation layer and has the function of removing water from the attenuation layer and guiding it to the drainage points.
  • the flat roof structure is a warm roof structure, in which the principal thermal insulation is placed immediately below the roof covering, meaning the waterproof membrane layer, resulting in the structural deck and support being at a temperature close to that of the interior of the building.
  • a warm roof comprises, from top to bottom: a surface/landscaping layer; optionally a substrate layer; the water attenuation layer; optionally a discharge layer; a waterproof membrane layer; a thermal insulation layer; optionally a vapour control layer; then the base structural substrate on which the flat roof is constructed.
  • Figure 9 illustrates an expanded view of the layers in an example of a warm roof structure.
  • This comprises a surface/landscaping layer 1 formed of topsoil for plant growth; a substrate layer 2 formed of MMVF for retaining water for the plant growth; the water attenuation layer 3; a waterproof membrane layer 4; a thermal insulation layer 5 formed of MMVF; a vapour control layer 6; then the base structural substrate 7 on which the flat roof is constructed.
  • flat roof structure can be provided, for instance an inverted roof structure.
  • This is a variant of the warm roof in which the principal thermal insulation is placed above the roof covering, resulting in the roof covering, structural deck and structural support being at a temperature close to that of the interior of the building.
  • This is based on the conventional structure for an inverted roof and comprises, from top to bottom: a surface/landscaping layer; optionally a substrate layer; the water attenuation layer; a water flow reducing layer/ discharge layer; inverted thermal insulation layer; a waterproof membrane layer; then the base structural substrate on which the flat roof is constructed.
  • the flat roof structure has at least one drainage point which is in fluid communication with the water attenuation layer.
  • the connection may be direct or indirect, for instance via the discharge layer. Water which is received and held in the water attenuation layer thus can travel to the or each drainage point.
  • the drainage point is usually connected with a gutter system so as to carry the water away from the flat roof structure. Usually it is carried downwardly towards the ground and into the sewers and waterways.
  • the drain at the drainage point may be any of the known drain constructions for blue roofs such as described in the NFRC Guideline mentioned above, or W02020/018599, or W02020/058384.
  • the flat roof structure includes a discharge layer below the water attenuation layer.
  • This provides a preferably multidirectional free flowing path guiding the water to the drainage points.
  • This can also be referred to as a water flow reducing layer.
  • it can be made of any of the known materials for such a layer, for instance recycled high impact polystyrene (HIPS) sheets combined and covered with a potential range of different geotextiles and films of e.g. Polypropylene (PP) and Polyethylene (PE). Examples are Nophadrain ND 100 / 120 or ND 800 and others.
  • the discharge layer may also comprise a layer formed of a matrix of man-made vitreous fibres (MMVF) bonded with a cured binder composition. The thickness can for instance be in the range 10 to 50 mm, preferably 15 to 30 mm.
  • a discharge layer may comprise two or more sub-layers - for instance a layer of MMVF and a layer of a more conventional material as mentioned above.
  • the water attenuation element comprises an integrated discharge area in its bottom part, formed of cross-cut grooves in the bottom surface of the element, such as e.g. grooves of 2 x 2 cm. In this way water flow to the drainage points on the roof is promoted.
  • the water attenuation layer and the discharge layer are formed by a single type of element.
  • the lower part forming the discharge layer can have a higher density than the upper part forming the water attenuation layer, thus providing additional compressive strength. This is especially valuable in the case where grooves are present as it can compensate for any loss in compressive strength caused by the grooves.
  • the flat roof structure of the invention is a blue roof, in that it has the capacity to absorb and retain and subsequently release/discharge water from the water attenuation layer. In addition it may have the characteristics of a green roof. Thus it may also be provided with one or more layers above the water attenuation layer including a growth substrate layer in which plants may be grown and optionally a water retention layer for retention of water for the plant growth.
  • Green roof structures are also known and any of the growth substrates which have been described for such structures can be used as a growth substrate layer in the invention.
  • a preferred example is an MMVF growth substrate.
  • Such a growth substrate layer is formed of a matrix of MMVF bonded with a binder.
  • the binder may be any of the types known for use in MMVF growth substrates. Preferably it is of the same type as the binder required as essential in the water attenuation layer.
  • the density of a growth substrate layer formed of MMVF is preferably in the range 40 to 80 kg/m 3 , preferably in the range 50 to 70 kg/m 3 .
  • MMVF used for a growth substrate layer is preferably hydrophilic and can contain wetting agent. However, preferably it does not contain wetting agent.
  • a water attenuation element is hydrophilic, that is, it attracts water. Hydrophilic has its normal meaning in the art.
  • the hydrophilicity of the water attenuation element may be defined in terms of the contact angle with water.
  • the MMVF of the device has a contact angle with water of less than 90°.
  • the contact angle is measured by a sessile drop measurement method. Any sessile drop method can be used, for example with a contact angle goniometer.
  • a droplet is placed on the solid surface and an image of the drop is recorded in time.
  • the static contact angle is then defined by fitting Young-Laplace equation around the droplet.
  • the contact angle is given by the angle between the calculated drop shape function and the sample surface, the projection of which in the drop image is referred to as the baseline.
  • the equilibrium contact angles are used for further evaluation and calculation of the surface free energy using the Owens, Wendt, Rabel and Kaeble method.
  • the method for calculating the contact angle between material and water is well-known to the skilled person.
  • Hydrophilicity of the attenuation element may be defined by the hydraulic conductivity.
  • the attenuation element has a hydraulic conductivity of 5 m/day to 300 m/day, preferably 50 m/day to 200 m/day. Hydraulic conductivity is measured in accordance with ISO 17312:2005. The advantage of this hydraulic conductivity is that the attenuation element can absorb excess water and transfer it away with sufficient speed to prevent flooding.
  • the hydrophilicity of a sample of MMVF substrate can also be measured by determining the sinking time of a sample.
  • a sample of MMVF substrate having dimensions of 100x100x100 mm is required for determining the sinking time.
  • a container with a minimum size of 200x200x200 mm is filled with water.
  • the sinking time is the time from when the sample first contacts the water surface to the time when the test specimen is completely submerged.
  • the sample is placed in contact with the water in such a way that a cross-section of 100x100 mm first touches the water.
  • the sample will then need to sink a distance of just over 100mm in order to be completely submerged. The faster the sample sinks, the more hydrophilic the sample is.
  • the MMVF substrate is considered hydrophilic if the sinking time is less than 120 seconds. Preferably the sinking time is less than 60 seconds.
  • the water attenuation element may have a sinking time of a few seconds, such as less than 15 seconds, preferably less than 10 seconds.
  • the method of the present invention comprises a water attenuation element comprising man-made vitreous fibres (MMVF).
  • MMVF man-made vitreous fibres
  • the man-made vitreous fibres (MMVF) can have any suitable oxide composition.
  • the fibres can be glass fibres, ceramic fibres, basalt fibres, slag fibres or rock or stone fibres.
  • the fibres are preferably of the types generally known as rock, stone or slag fibres, most preferably stone fibres.
  • Stone fibres commonly comprise the following oxides, in percent by weight:
  • the MMVF have the following levels of elements, calculated as oxides in wt%: SiO 2 : at least 30, 32, 35 or 37; not more than 51 , 48, 45 or 43
  • Al 2 O 3 at least 12, 16 or 17; not more than 30, 27 or 25
  • CaO at least 8 or 10; not more than 30, 25 or 20
  • MgO at least 2 or 5; not more than 25, 20 or 15 FeO (including Fe203): at least 4 or 5; not more than 15, 12 or 10 FeO+MgO: at least 10, 12 or 15; not more than 30, 25 or 20 Na 2 O+K 2 O: zero or at least 1; not more than 10 CaO+MgO: at least 10 or 15; not more than 30 or 25 Ti02: zero or at least 1 ; not more than 6, 4 or 2
  • the MMVF made by the method of the invention preferably have the composition in wt%:
  • Another preferred composition for the MMVF is as follows in wt%:
  • K 2 O 0-15% preferably 2-12% R 2 O (Na 2 O + K 2 O) 10-14.7% preferably 10-13.5%
  • Glass fibres commonly comprise the following oxides, in percent by weight: SiO 2 : 50 to 70
  • Glass fibres can also contain the following oxides, in percent by weight: Na 2 O+K 2 O: 8 to 18, in particular Na 2 O+K 2 O greater than CaO+MgO B 2 O 3 : 3 to 12
  • Some glass fibre compositions can contain Al 2 O 3 : less than 2% .
  • the geometric mean fibre diameter is often in the range of 1.5 to 10 microns, in particular 2 to 8 microns, preferably 2 to 5 microns.
  • the water attenuation element comprises at least 90 wt% man-made vitreous fibres by weight of the total solid content of the water attenuation element.
  • An advantage of having such an amount of fibres present in the water attenuation element is that there are sufficient pores formed between the fibres to allow the device to hold large amounts of water.
  • the remaining solid content may be made up primarily of binder.
  • the water attenuation element is preferably in the form of a coherent MMVF substrate i.e. a coherent mass. That is, the water attenuation element is preferably a coherent matrix of man-made vitreous fibres, which has been produced as such, but can also be formed by granulating a slab of mineral wool and consolidating the granulated material.
  • a coherent substrate is a single, unified substrate.
  • the water attenuation element according to the invention may optionally comprise a wetting agent.
  • a wetting agent has its normal meaning in the art, and may be a cationic, anionic or non-ionic surfactant.
  • the water attenuation element may comprise a non-ionic wetting agent such as Rewopal®.
  • the water attenuation element may comprise an ionic surfactant, more preferably an alkyl ether sulphate surfactant wetting agent.
  • the wetting agent may be an alkali metal alkyl ether sulphate or an ammonium alkyl ether sulphate.
  • the wetting agent is a sodium alkyl ether sulphate.
  • a commercially available alkyl ether sulphate surfactant wetting agent is Texapon®.
  • the wetting agent may also be a linear alkyl benzene sulphonate anionic surfactant.
  • non-ionic wetting agents may be washed out of the MMVF water attenuation element over time. It is therefore preferable to use an ionic wetting agent, especially an anionic wetting agent, such as linear alkyl benzene sulphonate or Texapon ®. These do not wash out of the MMVF device to the same extent.
  • the water attenuation element may comprise 0.01 to 1 wt% wetting agent, preferably 0.05 to 0.5 wt% wetting agent, more preferably 0.1 to 0.3 wt% wetting agent.
  • the water attenuation element does not comprise any wetting agent.
  • the water attenuation element preferably comprises no wetting agent i.e. comprises 0 wt% wetting agent.
  • wetting agents reduces the number of additives in the element, which is environmentally advantageous, and also saves costs.
  • wetting agents are made from non-renewable sources so it is beneficial to avoid their use.
  • wetting agents may be washed out of the water attenuation element. This is problematic because the wetting agent may contaminate the waterways. When a wetting agent is washed out this also changes the nature of the water attenuation element, typically changing drainage into the water attenuation layer, buffering, and discharge/infiltration, making it difficult to predict the behaviour. Avoiding the use of a wetting agent avoids these problems.
  • the water attenuation element comprising MMVF preferably has a density in the range of 70 to 200 kg/m 3 , preferably 100 to 180 kg/m 3 and in particular in the range 120 to 150 kg/m 3 .
  • the advantage of this density is that the water attenuation element has relatively high compression strength.
  • a force distribution plate is positioned on top of the water attenuation element in order to distribute the force applied to the water attenuation element. Preferably such a force distribution plate is not required due to the density of the water attenuation element.
  • the water attenuation element comprising MMVF preferably has volume in the range of 10 litres to 300 litres, preferably 100 litres to 250 litres, more preferably 150 litres to 200 litres.
  • the precise volume is chosen according to the volume of water which is expected to be managed.
  • multiple elements are preferably used in an array.
  • the water attenuation element comprising MMVF preferably has thickness greater than 50 mm, more preferably at least 55 mm. it can be at least 100 mm and preferably up to 500 mm. In particular it may be up to 200 mm, for instance up to 150 mm.
  • the elements are usually cuboid with two parallel major faces joined by perpendicular minor faces. They may be arranged in an array with the major faces abutting, or with the minor faces abutting. They may be arranged abutting in a horizontal array. Additionally they may be arranged in two or more layers.
  • the vast majority of the water attenuation element is used to buffer the amount of water that is conveyed to the water attenuation element.
  • the water holding capacity of the water attenuation element is at least 80% of the volume, preferably 80-99 %, most preferably 85-95 %.
  • the water holding capacity of the water attenuation element is high due to the open pore structure and the hydrophilicity.
  • the amount of water that is retained by the water attenuation element when it gives off water is less than 20 %vol, preferably less than 10 %vol, most preferably less than 5%vol.
  • the water retained may be 2 to 20 %vol, such as 5 to 10 %vol.
  • the buffering capacity of the water attenuation element that is the difference between the maximum amount of water that can be held, and the amount of water that is retained when the water attenuation element gives off water, is at least 60 %vol, preferably at least 70 %vol, preferably at least 80 %vol.
  • the buffering capacity may be 60 to 90 %vol, such as 60 to 85 %vol.
  • the water holding capacity, the amount of water retained and the buffering capacity of the water attenuation element can be measured in accordance with EN 13041 - 1999.
  • Man-made vitreous fibres can be made from a mineral melt.
  • a mineral melt is provided in a conventional manner by providing mineral materials and melting them in a furnace.
  • This furnace can be any of the types of furnace known for production of mineral melts for MMVF, for instance a shaft furnace such as a cupola furnace, a tank furnace, or a cyclone furnace.
  • the fiberization can be by a spinning cup process in which melt is centrifugally extruded through orifices in the walls of a rotating cup (spinning cup, also known as internal centrifugation).
  • the fiberization can be by centrifugal fiberization by projecting the melt onto and spinning off the outer surface of one fiberizing rotor, or off a cascade of a plurality of fiberizing rotors, which rotate about a substantially horizontal axis (cascade spinner).
  • the melt is thus formed into a cloud of fibres entrained in air and the fibres are collected as a web on a conveyor and carried away from the fiberizing apparatus.
  • the web of fibres is then consolidated, which can involve cross lapping and/or longitudinal compression and/or vertical compression and/or winding around a mandrel to produce a cylindrical product for pipe insulation. Other consolidation processes may also be performed.
  • the binder composition is applied to the fibres preferably when they are a cloud entrained in air. Alternatively it can be applied after collection on the conveyor but this is less preferred. After consolidation the consolidated web of fibres is passed into a curing device to cure the binder.
  • the curing is carried out at temperatures from 100 to 300°C, such as 170 to 270°C, such as 180 to 250°C, such as 190 to 230°C.
  • the curing takes place in a conventional curing oven for mineral wool production, preferably operating at a temperature of from 150 to 300°C, such as 170 to 270°C, such as 180 to 250°C, such as 190 to 230°C.
  • the curing takes place for a time of 30 seconds to 20 minutes, such as 1 to 15 minutes, such as 2 to 10 minutes.
  • curing takes place at a temperature of 150 to 250 °C for a time of 30 seconds to 20 minutes.
  • the curing process may commence immediately after application of the binder to the fibres.
  • the curing is defined as a process whereby the binder composition undergoes a physical and/or chemical reaction which in case of a chemical reaction usually increases the molecular weight of the compounds in the binder composition and thereby increases the viscosity of the binder composition, usually until the binder composition reaches a solid state.
  • the cured binder composition binds the fibres to form a structurally coherent matrix of fibres.
  • the curing of the binder in contact with the mineral fibres takes place in a heat press.
  • the curing of a binder in contact with the mineral fibres in a heat press has the particular advantage that it enables the production of high-density products.
  • the curing process comprises drying by pressure.
  • the pressure may be applied by blowing air or gas through/over the mixture of mineral fibres and binder.
  • the binder composition used according to the present invention is in the form of an aqueous composition. Preferred features are discussed below.
  • the aqueous binder comprises
  • the binders used according to the present invention are formaldehyde free.
  • the term "formaldehyde free” is defined to characterize a mineral wool product where the emission is below 5 ⁇ g/m 2 /h of formaldehyde from the mineral wool product, preferably below 3 ⁇ g/m 2 /h.
  • the test is carried out in accordance with ISO 16000 for testing aldehyde emissions.
  • Component (i) is in form of one or more oxidized lignins.
  • Lignin, cellulose and hemicellulose are the three main organic compounds in a plant cell wall. Lignin can be thought of as the glue, that holds the cellulose fibres together. Lignin contains both hydrophilic and hydrophobic groups. It is the second most abundant natural polymer in the world, second only to cellulose, and is estimated to represent as much as 20-30% of the total carbon contained in the biomass, which is more than 1 billion tons globally.
  • Fig. 1 shows a section from a possible lignin structure.
  • lignin There are at least four groups of technical lignins available in the market. These four groups are shown in Fig. 3.
  • a possible fifth group, Biorefinery lignin is a bit different as it is not described by the extraction process, but instead by the process origin, e.g. biorefining and it can thus be similar or different to any of the other groups mentioned.
  • Each group is different from each other and each is suitable for different applications.
  • Lignin is a complex, heterogenous material composed of up to three different phenyl propane monomers, depending on the source.
  • Softwood lignins are made mostly with units of coniferyl alcohol, see fig. 2 and as a result, they are more homogeneous than hardwood lignins, which has a higher content of syringyl alcohol, see fig. 2.
  • the appearance and consistency of lignin are quite variable and highly contingent on process.
  • Lignosulfonate from the sulfite pulping process remains the largest commercial available source of lignin, with capacity of 1.4 million tonnes. But taking these aside, the kraft process is currently the most used pulping process and is gradually replacing the sulfite process. An estimated 78 million tonnes per year of lignin are globally generated by kraft pulp production but most of it is burned for steam and energy. Current capacity for kraft recovery is estimated at 160,000 tonnes, but sources indicate that current recovery is only about 75,000 tonnes. Kraft lignin is developed from black liquour, the spent liquor from the sulfate or kraft process. At the moment, 3 well-known processes are used to produce the kraft lignin: LignoBoost, LignoForce and SLRP.
  • the kraft process introduces thiol groups, stilbene while some carbohydrates remain. Sodium sulphate is also present as an impurity due to precipitation of lignin from liquor with sulphuric acid but can potentially be avoided by altering the way lignin is isolated.
  • the kraft process leads to high amount of phenolic hydroxyl groups and this lignin is soluble in water when these groups are ionized (above pH ⁇ 10).
  • kraft lignin is generally higher in purity than lignosulfonates.
  • the molecular weight are 1000-3000 g/mol.s
  • Soda lignin originates from sodium hydroxide pulping processes, which are mainly used for wheat straw, bagasse and flax. Soda lignin properties are similar to kraft lignins one in terms of solubility and T g . This process does not utilize sulphur and there is no covalently bound sulphur. The ash level is very low. Soda lignin has a low solubility in neutral and acid media but is completely soluble at pH 12 and higher.
  • the lignosulfonate process introduces large amount of sulphonate groups making the lignin soluble in water but also in acidic water solutions.
  • Lignosulfonates has up to 8% sulfur as sulphonate, whereas kraft lignin has 1- 2% sulfur, mostly bonded to the lignin.
  • the molecular weight of lignosulfonate is
  • This lignin contains more leftover carbohydrates compared to other types and has a higher average molecular weight.
  • the typical hydrophobic core of lignin together with large number of ionized sulphonate groups make this lignin attractive as a surfactant and it often finds application in dispersing cement etc.
  • a further group of lignins becoming available is lignins resulting from biorefining processes in which the carbohydrates are separated from the lignin by chemical or biochemical processes to produce a carbohydrate rich fraction. This remaining lignin is referred to as biorefinery lignin. Biorefineries focus on producing energy, and producing substitutes for products obtained from fossil fuels and petrochemicals as well as lignin. The lignin from this process is in general considered a low value product or even a waste product mainly used for thermal combustion or used as low grade fodder or otherwise disposed of. Organosolv lignin availability is still considered on the pilot scale.
  • the process involves extraction of lignin by using water together with various organic solvents (most often ethanol) and some organic acids.
  • An advantage of this process is the higher purity of the obtained lignin but at a much higher cost compared to other technical lignins and with the solubility in organic solvents and not in water.
  • Previous attempts to use lignin as a basic compound for binder compositions for mineral fibres failed because it proved difficult to find suitable cross-linkers which would achieve desirable mechanical properties of the cured mineral wool product and at the same time avoid harmful and/or corrosive components.
  • lignin is used to replace oil derived chemicals, such as phenol in phenolic resins in binder applications or in bitumen. It is also used as cement and concrete additives and in some aspects as dispersants.
  • the cross-linking of a polymer in general should provide improved properties like mechanical, chemical and thermal resistance etc.
  • Lignin is especially abundant in phenolic and aliphatic hydroxyl groups that can be reacted leading to cross- linked structure of lignin.
  • Different lignins will also have other functional groups available that can potentially be used. The existence of these other groups is largely dependent on the way lignin was separated from cellulose and hemicellulose (thiols in kraft lignin, sulfonates in lignosulfonate etc.) depending on the source. It has been found that by using oxidized lignins, binder compositions for mineral fibres can be prepared which allow excellent properties of the mineral fibre product produced.
  • the component (i) is in form of one or more oxidized kraft lignins. In one embodiment, the component (i) is in form of one or more oxidized soda lignins.
  • the component (i) is in form of one or more ammonia- oxidized lignins.
  • ammonia- oxidized lignins is to be understood as a lignin that has been oxidized by an oxidation agent in the presence of ammonia.
  • AOL ammonia-oxidized lignin
  • ammonia is partially or fully replaced by an alkali metal hydroxide, in particular sodium hydroxide and/or potassium hydroxide.
  • a typical oxidation agent used for preparing the oxidized lignins is hydrogen peroxide.
  • the ammonia-oxidized lignin comprises one or more of the compounds selected from the group of ammonia, amines, hydroxides or any salts thereof.
  • the component (i) is having a carboxylic acid group content of 0.05 to 10 mmol/g, such as 0.1 to 5 mmol/g, such as 0.20 to 1.5 mmol/g, such as 0.40 to 1.2 mmol/g, such as 0.45 to 1.0 mmol/g, based on the dry weight of component (i). In one embodiment, the component (i) is having an average carboxylic acid group content of more than 1.5 groups per macromolecule of component (i), such as more than 2 groups, such as more than 2.5 groups.
  • the carboxylic acid group content of the oxidized lignins plays an important role in the surprising advantages of the aqueous binder compositions for mineral fibres according to the present invention.
  • the carboxylic acid group of the oxidized lignins improve the cross-linking properties and therefore allow better mechanical properties of the cured mineral fibre products.
  • Component (ii) is in form of one or more cross-linkers.
  • the component (ii) comprises in one embodiment one or more cross-linkers selected from b-hydroxyalkylamide-cross-linkers and/or oxazoline-cross-linkers.
  • b-hydroxyalkylamide-cross-linkers is a curing agent for the acid-functional macromolecules. It provides a hard, durable, corrosion resistant and solvent resistant cross-linked polymer network. It is believed the b-hydroxyalkylamide cross-linkers cure through esterification reaction to form multiple ester linkages.
  • the hydroxy functionality of the b-hydroxyalkylamide-cross-linkers should be an average of at least 2, preferably greater than 2 and more preferably 2-4 in order to obtain optimum curing response.
  • Oxazoline group containing cross-linkers are polymers containing one of more oxazoline groups in each molecule and generally, oxazoline containing crosslinkers can easily be obtained by polymerizing an oxazoline derivative.
  • the patent US6818699 B2 provides a disclosure for such a process.
  • the component (ii) is an epoxidised oil based on fatty acid triglyceride.
  • epoxidised oils based on fatty acid triglycerides are not considered hazardous and therefore the use of these compounds in the binder compositions according to the present invention do not render these compositions unsafe to handle.
  • the component (ii) is a molecule having 3 or more epoxy groups.
  • the component (ii) is one or more flexible oligomer or polymer, such as a low Tg acrylic based polymer, such as a low Tg vinyl based polymer, such as low Tg polyether, which contains reactive functional groups such as carbodiimide groups, such as anhydride groups, such as oxazoline groups, such as amino groups, such as epoxy groups.
  • component (ii) is selected from the group consisting of cross-linkers taking part in a curing reaction, such as hydroxyalkylamide, alkanolamine, a reaction product of an alkanolamine and a polycarboxylic acid.
  • cross-linkers taking part in a curing reaction, such as hydroxyalkylamide, alkanolamine, a reaction product of an alkanolamine and a polycarboxylic acid.
  • the reaction product of an alkanolamine and a polycarboxylic acid can be found in US6706853B1.
  • aqueous binder compositions according to the present invention are due to the interaction of the oxidized lignins used as component (i) and the cross-linkers mentioned above. It is believed that the presence of carboxylic acid groups in the oxidized lignins enable the very effective cross-linking of the oxidized lignins.
  • the component (ii) is one or more cross-linkers selected from the group consisting of multifunctional organic amines such as an alkanolamine, diamines, such as hexamethyldiamine, triamines.
  • the component (ii) is one or more cross-linkers selected from the group consisting of polyethylene imine, polyvinyl amine, fatty amines.
  • the component (ii) is one or more fatty amides. In one embodiment, the component (ii) is one or more cross-linkers selected from the group consisting of dimethoxyethanal, glycolaldehyde, glyoxalic acid.
  • the component (ii) is one or more cross-linkers selected from polyester polyols, such as polycaprolactone.
  • the component (ii) is one or more cross-linkers selected from the group consisting of starch, modified starch, CMC. In one embodiment, the component (ii) is one or more cross-linkers in form of aliphatic multifunctional carbodiimides.
  • the component (ii) is one or more cross-linkers selected from melamine based cross-linkers, such as a hexakis(methylmethoxy)melamine (HMMM) based cross-linkers.
  • melamine based cross-linkers such as a hexakis(methylmethoxy)melamine (HMMM) based cross-linkers.
  • Picassian XL 701 , 702, 725 (Stahl Polymers), such as ZOLDINE® XL-29SE (Angus Chemical Company), such as CX300 (DSM), such as Carbodilite V-02-L2 (Nisshinbo Chemical Inc.).
  • Component (ii) can also be any mixture of the above mentioned compounds.
  • the binder composition according to the present invention comprises component (ii) in an amount of 1 to 40 wt.-%, such as 4 to 20 wt.-%, such as 6 to 12 wt.-%, based on the dry weight of component (i).
  • Component (iii) is in form of one or more plasticizers.
  • component (iii) is in form of one or more plasticizers selected from the group consisting of polyols, such as carbohydrates, hydrogenated sugars, such as sorbitol, erythriol, glycerol, monoethylene glycol, polyethylene glycols, polyethylene glycol ethers, polyethers, phthalates and/or acids, such as adipic acid, vanillic acid, lactic acid and/or ferullic acid, acrylic polymers, polyvinyl alcohol, polyurethane dispersions, ethylene carbonate, propylene carbonate, lactones, lactams, lactides, acrylic based polymers with free carboxy groups and/or polyurethane dispersions with free carboxy groups, polyamides, amides such as carbamide/urea, or any mixtures thereof.
  • polyols such as carbohydrates
  • hydrogenated sugars such as sorbitol, erythriol, glycerol
  • component (iii) is in form of one or more plasticizers selected from the group consisting of carbonates, such as ethylene carbonate, propylene carbonate, lactones, lactams, lactides, compounds with a structure similar to lignin like vanillin, acetosyringone, solvents used as coalescing agents like alcohol ethers, polyvinyl alcohol.
  • plasticizers selected from the group consisting of carbonates, such as ethylene carbonate, propylene carbonate, lactones, lactams, lactides, compounds with a structure similar to lignin like vanillin, acetosyringone, solvents used as coalescing agents like alcohol ethers, polyvinyl alcohol.
  • component (iii) is in form of one or more non-reactive plasticizer selected from the group consisting of polyethylene glycols, polyethylene glycol ethers, polyethers, hydrogenated sugars, phthalates and/or other esters, solvents used as coalescing agents like alcohol ethers, acrylic polymers, polyvinyl alcohol.
  • non-reactive plasticizer selected from the group consisting of polyethylene glycols, polyethylene glycol ethers, polyethers, hydrogenated sugars, phthalates and/or other esters, solvents used as coalescing agents like alcohol ethers, acrylic polymers, polyvinyl alcohol.
  • component (iii) is one or more reactive plasticizers selected from the group consisting of carbonates, such as ethylene carbonate, propylene carbonate, lactones, lactams, lactides, di- or tricarboxylic acids, such as adipic acid, or lactic acid, and/or vanillic acid and/or ferullic acid, polyurethane dispersions, acrylic based polymers with free carboxy groups, compounds with a structure similar to lignin like vanillin, acetosyringone.
  • carbonates such as ethylene carbonate, propylene carbonate, lactones, lactams, lactides, di- or tricarboxylic acids, such as adipic acid, or lactic acid, and/or vanillic acid and/or ferullic acid
  • polyurethane dispersions acrylic based polymers with free carboxy groups, compounds with a structure similar to lignin like vanillin, acetosyringone.
  • component (iii) is in form of one or more plasticizers selected from the group consisting of fatty alcohols, monohydroxy alcohols such as pentanol, stearyl alcohol.
  • component (iii) comprises one or more plasticizers selected from the group consisting of polyethylene glycols, polyethylene glycol ethers.
  • plasticizers having a boiling point of more than 100 °C, in particular 140 to 250 °C strongly improves the mechanical properties of the mineral fibre products according to the present invention although, in view of their boiling point, it is likely that these plasticizers will at least in part evaporate during the curing of the aqueous binders in contact with the mineral fibres.
  • component (iii) comprises one or more plasticizers having a boiling point of more than 100 °C, such as 110 to 280 °C, more preferred 120 to 260 °C, more preferred 140 to 250 °C. It is believed that the effectiveness of these plasticizers in the aqueous binder composition according to the present invention is associated with the effect of increasing the mobility of the oxidized lignins during the curing process. It is believed that the increased mobility of the lignins or oxidized lignins during the curing process facilitates the effective cross-linking.
  • component (iii) comprises one or more polyethylene glycols having an average molecular weight of 150 to 50000 g/mol, in particular 150 to 4000 g/mol, more particular 150 to 1000 g/mol, preferably 150 to 500 g/mol, more preferably 200 to 400 g/mol. In one embodiment, component (iii) comprises one or more polyethylene glycols having an average molecular weight of 4000 to 25000 g/mol, in particular 4000 to 15000 g/mol, more particular 8000 to 12000 g/mol.
  • component (iii) is capable of forming covalent bonds with component (i) and/or component (ii) during the curing process.
  • a component would not evaporate and remain as part of the composition but will be effectively altered to not introduce unwanted side effects e.g. water absorption in the cured product.
  • Non-limiting examples of such a component are caprolactone and acrylic based polymers with free carboxyl groups.
  • component (iii) is selected from the group consisting of fatty alcohols, monohydroxy alcohols, such as pentanol, stearyl alcohol.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of alkoxylates such as ethoxylates such as butanol ethoxylates, such as butoxytriglycol.
  • component (iii) is selected from one or more propylene glycols.
  • component (iii) is selected from one or more glycol esters.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of adipates, acetates, benzoates, cyclobenzoates, citrates, stearates, sorbates, sebacates, azelates, butyrates, valerates.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of phenol derivatives such as alkyl or aryl substituted phenols.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of silanols, siloxanes.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of sulfates such as alkyl sulfates, sulfonates such as alkyl aryl sulfonates such as alkyl sulfonates, phosphates such as tripolyphosphates; such as tributylphosphates.
  • component (iii) is selected from one or more hydroxy acids. In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of monomeric amides such as acetamides, benzamide, fatty acid amides such as tall oil amides.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of quaternary ammonium compounds such as trimethylglycine, distearyldimethylammoniumchloride.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of vegetable oils such as castor oil, palm oil, linseed oil, tall oil, soybean oil.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of hydrogenated oils, acetylated oils. In one embodiment, component (iii) is selected from one or more fatty acid methyl esters.
  • component (iii) is selected from one or more plasticizers selected from the group consisting of alkyl polyglucosides, gluconamides, aminoglucoseamides, sucrose esters, sorbitan esters.
  • plasticizers refers to a substance that is added to a material in order to make the material softer, more flexible (by decreasing the glass-transition temperature Tg) and easier to process.
  • Component (iii) can also be any mixture of the above mentioned compounds.
  • component (iii) is present in an amount of 0.5 to 50, preferably 2.5 to 25, more preferably 3 to 15 wt.-%, based on the dry weight of component (i).
  • Aqueous binder composition for mineral fibers comprising components (i) and (iia)
  • the present inventors have found that the excellent binder properties can also be achieved by a two-component system which comprises component (i) in form of one or more oxidized lignins and a component (iia) in form of one or more modifiers, and optionally any of the other components mentioned above and below.
  • component (iia) is a modifier in form of one or more compounds selected from the group consisting of epoxidised oils based on fatty acid triglycerides.
  • component (iia) is a modifier in form of one or more compounds selected from molecules having 3 or more epoxy groups.
  • component (iia) is a modifier in form of one or more flexible oligomer or polymer, such as a low Tg acrylic based polymer, such as a low Tg vinyl based polymer, such as low Tg polyether, which contains reactive functional groups such as carbodiimide groups, such as anhydride groups, such as oxazoline groups, such as amino groups, such as epoxy groups.
  • a low Tg acrylic based polymer such as a low Tg vinyl based polymer, such as low Tg polyether
  • reactive functional groups such as carbodiimide groups, such as anhydride groups, such as oxazoline groups, such as amino groups, such as epoxy groups.
  • component (iia) is one or more modifiers selected from the group consisting of polyethylene imine, polyvinyl amine, fatty amines. In one embodiment, the component (iia) is one or more modifiers selected from aliphatic multifunctional carbodiimides.
  • Component (iia) can also be any mixture of the above mentioned compounds.
  • the excellent binder properties achieved by the binder composition for mineral fibers comprising components (i) and (iia), and optional further components, are at least partly due to the effect that the modifiers used as components (iia) at least partly serve the function of a plasticizer and a crosslinker.
  • the aqueous binder composition comprises component (iia) in an amount of 1 to 40 wt.-%, such as 4 to 20 wt.-%, such as 6 to 12 wt.-%, based on the dry weight of the component (i).
  • the aqueous binder composition used in the present invention comprises further components.
  • the aqueous binder composition used in the present invention comprises a catalyst selected from inorganic acids, such as sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and/or phosphoric acid, and/or any salts thereof such as sodium hypophosphite, and/or ammonium salts, such as ammonium salts of sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and/or phosphoric acid.
  • a catalyst selected from inorganic acids, such as sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and/or phosphoric acid, and/or any salts thereof such as sodium hypophosphite, and/or ammonium salts, such as ammonium salts of sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and/or phosphoric acid.
  • the aqueous binder composition used in the present invention comprises a catalyst selected from Lewis acids, which can accept an electron pair from a donor compound forming a Lewis adduct, such as ZnCI 2 , Mg (CIO4) 2 , Sn [N(SO 2 -n-C8F17) 2 ] 4 .
  • the aqueous binder composition according to the present invention comprises a catalyst selected from metal chlorides, such as KCI, MgCI 2 , ZnCI 2 , FeCI 3 and SnCI 2 .
  • the aqueous binder composition used in the present invention comprises a catalyst selected from organometallic compounds, such as titanate-based catalysts and stannum based catalysts.
  • the aqueous binder composition used in the present invention comprises a catalyst selected from chelating agents, such as transition metals, such as iron ions, chromium ions, manganese ions, copper ions.
  • chelating agents such as transition metals, such as iron ions, chromium ions, manganese ions, copper ions.
  • the aqueous binder composition used in the present invention further comprises a further component (iv) in form of one or more silanes.
  • the aqueous binder composition used in the present invention comprises a further component (iv) in form of one or more coupling agents, such as organofunctional silanes.
  • component (iv) is selected from group consisting of organofunctional silanes, such as primary or secondary amino functionalized silanes, epoxy functionalized silanes, such as polymeric or oligomeric epoxy functionalized silanes, methacrylate functionalized silanes, alkyl and aryl functionalized silanes, urea funtionalised silanes or vinyl functionalized silanes.
  • organofunctional silanes such as primary or secondary amino functionalized silanes
  • epoxy functionalized silanes such as polymeric or oligomeric epoxy functionalized silanes, methacrylate functionalized silanes, alkyl and aryl functionalized silanes, urea funtionalised silanes or vinyl functionalized silanes.
  • the aqueous binder composition used in the present invention further comprises a component (v) in form of one or more components selected from the group of ammonia, amines or any salts thereof.
  • ammonia, amines or any salts thereof as a further component can in particular be useful when oxidized lignins are used in component (i), which oxidised lignin have not been oxidized in the presence of ammonia.
  • the aqueous binder composition used in the present invention further comprises a further component in form of urea, in particular in an amount of 5 to 40 wt.-%, such as 10 to 30 wt.-%, 15 to 25 wt.-%, based on the dry weight of component (i).
  • the aqueous binder composition used in the present invention further comprises a further component in form of one or more carbohydrates selected from the group consisting of sucrose and reducing sugars in an amount of 5 to 50 wt.-%, such as 5 to less than 50 wt.-%, such as 10 to 40 wt.-%, such as 15 to 30 wt.-% based on the dry weight of component (i).
  • a binder composition having a sugar content of 50 wt.-% or more, based on the total dry weight of the binder components is considered to be a sugar based binder.
  • a binder composition having a sugar content of less than 50 wt.-%, based on the total dry weight of the binder components is considered a non-sugar based binder.
  • the aqueous adhesive composition used in the present invention further comprises a further component in form of one or more surface active agents that are in the form of non-ionic and/or ionic emulsifiers such as polyoxyethylenes (4) lauryl ether, such as soy lecithin, such as sodium dodecyl sulfate.
  • non-ionic and/or ionic emulsifiers such as polyoxyethylenes (4) lauryl ether, such as soy lecithin, such as sodium dodecyl sulfate.
  • the aqueous binder composition used in the present invention comprises
  • component (i) 0.1 to 5 mmol/g, such as 0.20 to 1.5 mmol/g, such as 0.40 to 1.2 mmol/g, such as 0.45 to 1.0 mmol/g, based on the dry weight of component (i);
  • the aqueous binder composition used in the present invention comprises
  • component (i) in form of one or more ammonia-oxidized lignins having a carboxylic acid group content of 0.05 to 10 mmol/g, such as 0.1 to 5 mmol/g, such as 0.20 to 1.5 mmol/g, such as 0.40 to 1.2 mmol/g, such as 0.45 to 1.0 mmol/g, based on the dry weight of component (i);
  • the aqueous binder composition used in the present invention comprises
  • component (i) in form of one or more ammonia-oxidized lignins having an average carboxylic acid group content of more than 1.5 groups per macromolecule of component (i), such as more than 2 groups, such as more than 2.5 groups;
  • component (ii) in form of one or more cross-linkers selected from b- hydroxyalkylamide-cross-linkers and/or oxazoline-cross-linkers and/or is one or more cross-linkers selected from the group consisting of multifunctional organic amines such as an alkanolamine, diamines, such as hexamethyldiamine, triamines;
  • the aqueous binder composition used in the present invention comprises
  • component (i) in form of one or more ammonia-oxidized lignins having an average carboxylic acid group content of more than 1.5 groups per macromolecule of component (i), such as more than 2 groups, such as more than 2.5 groups;
  • the aqueous binder composition used in the present invention consists essentially of a component (i) in form of one or more oxidized lignins; a component (ii) in form of one or more cross-linkers; a component (iii) in form of one or more plasticizers; a component (iv) in form of one or more coupling agents, such as organofunctional silanes; optionally a component in form of one or more compounds selected from the group of ammonia, amines or any salts thereof; optionally a component in form of urea; optionally a component in form of a more reactive or non-reactive silicones; optionally a hydrocarbon oil; optionally one or more surface active agents; water.
  • a component (i) in form of one or more oxidized lignins a component (ii) in form of one or more cross-linkers; a component (iii) in form of one or more plasticizers; a component (iv) in form of one or more coup
  • the aqueous binder composition used in the present invention consists essentially of - a component (i) in form of one or more oxidized lignins;
  • a component (iv) in form of one or more coupling agents such as organofunctional silanes; optionally a component in form of one or more compounds selected from the group of ammonia, amines or any salts thereof; optionally a component in form of urea; - optionally a component in form of a more reactive or non-reactive silicones;
  • Oxidised lignins which can be used as component in the aqueous binder composition for mineral fibres according to the present invention and method for preparing such oxidised lignins
  • oxidised lignins which can be used as component of the binder composition and their preparation.
  • Oxidised lignins which can be used as component for the binders used in the present invention can be prepared by a method comprising bringing into contact
  • component (a) comprising one or more lignins - a component (b) comprising ammonia, one or more amine components, and/or any salt thereof.
  • component (c) comprising one or more oxidation agents.
  • Component (a) comprises one or more lignins.
  • component (a) comprises one or more kraft lignins, one or more soda lignins, one or more lignosulfonate lignins, one or more organosolv lignins, one or more lignins from biorefining processess of lignocellulosic feedstocks, or any mixture thereof.
  • component (a) comprises one or more kraft lignins.
  • component (b) comprises ammonia, one or more amino components, and/or any salts thereof.
  • replacement of the alkali hydroxides used in previously known oxidation processes of lignin by ammonia, one or more amino components, and/or any salts thereof plays an important role in the improved properties of the oxidised lignins prepared according to the present invention. It has surprisingly been found that the lignins oxidised by an oxidation agent in the presence of ammonia or amines contain significant amounts of nitrogen as a part of the structure of the oxidised lignins.
  • the improved fire resistance properties of the oxidised lignins when used in products where they are comprised in a binder composition, said oxidised lignins prepared according to the present invention are at least partly due to the nitrogen content of the structure of the oxidised lignins.
  • component (b) comprises ammonia and/or any salt thereof.
  • component (b), besides ammonia, one or more amino components, and/or any salts thereof, also comprises a comparably small amount of an alkali and/or earth alkali metal hydroxide, such as sodium hydroxide and/or potassium hydroxide.
  • component (b) comprises alkali and/or earth alkali metal hydroxides, such as sodium hydroxide and/or potassium hydroxide, as a component in addition to the ammonia, one or more amino components, and/or any salts thereof
  • the amount of the alkali and/or earth alkali metal hydroxides is usually small, such as 5 to 70 weight parts, such as 10 to 20 weight parts alkali and/or earth alkali metal hydroxide, based on ammonia.
  • component (c) comprises one or more oxidation agents.
  • component (c) comprises one or more oxidation agents in form of hydrogen peroxide, organic or inorganic peroxides, molecular oxygen, ozone, air, halogen containing oxidation agents, or any mixture thereof.
  • component (c) comprises hydrogen peroxide.
  • Hydrogen peroxide is perhaps the most commonly employed oxidant due to combination of low price, good efficiency and relatively low environmental impact. When hydrogen peroxide is used without the presence of catalysts, alkaline conditions and temperature are important due to the following reactions leading to radical formation:
  • the derivatized lignins prepared with the method according to the present invention contain increased amounts of carboxylic acid groups as a result of the oxidation process. Without wanting to be bound by any particular theory, it is believed that the carboxylic acid group content of the oxidised lignins prepared in the process according to the present invention plays an important role in the desirable reactivity properties of the derivatized lignins prepared by the method according to the present invention.
  • oxidised lignin is more hydrophilic. Higher hydrophilicity can enhance solubility in water and facilitate the adhesion to polar substrates such as mineral fibers.
  • the method according to the present invention comprises further components, in particular a component (d) in form of an oxidation catalyst, such as one or more transition metal catalyst, such as iron sulfate, such as manganese, palladium, selenium, tungsten containing catalysts.
  • a component (d) in form of an oxidation catalyst such as one or more transition metal catalyst, such as iron sulfate, such as manganese, palladium, selenium, tungsten containing catalysts.
  • Such oxidation catalysts can increase the rate of the reaction, thereby improving the properties of the oxidised lignins prepared by the method according to the present invention.
  • a component (a) comprises one or more lignins a component (b) comprises ammonia - a component (c) comprises one or more oxidation agents in form of hydrogen peroxide, wherein the mass ratios of lignin, ammonia and hydrogen peroxide are such that the amount of ammonia is 0.01 to 0.5 weight parts, such as 0.1 to 0.3, such as 0.15 to 0.25 weight parts ammonia, based on the dry weight of lignin, and wherein the amount of hydrogen peroxide is 0.025 to 1.0 weight parts, such as 0.05 to 0.2 weight parts, such as 0.075 to 0.125 weight parts hydrogen peroxide, based on the dry weight of lignin.
  • the method comprises the steps of:
  • component (a) in form of an aqueous solution and/or dispersion of one more lignins, the lignin content of the aqueous solution being 1 to 50 weight-%, such as 5 to 25 weight-
  • % such as 15 to 22 weight-%, such as 18 to 20 weight-%, based on the total weight of the aqueous solution;
  • component (b) comprising an aqueous solution of ammonia, one or more amine components, and/or any salt thereof;
  • component (c) comprising an oxidation agent
  • the pH adjusting step is carried so that the resulting aqueous solution and/or dispersion is having a pH > 9, such as > 10, such as > 10.5. In one embodiment, the pH adjusting step is carried out so that the resulting aqueous solution and/or dispersion is having a pH in the range of 10.5 to 12. In one embodiment, the pH adjusting step is carried out so that the temperature is allowed to raise to > 25 °C and then controlled in the range of 25 - 50 °C, such as 30 - 45 °C, such as 35 - 40 °C.
  • the temperature is allowed to raise > 35 °C and is then controlled in the range of 35 - 150 °C, such as 40 - 90 °C, such as 45 - 80 °C.
  • the oxidation step is carried out for a time of 1 second to 48 hours, such as 10 seconds to 36 hours, such as 1 minute to 24 hours such as 2 - 5 hours.
  • Oxidised lignins which can be used as component for the binders used in the present invention can be prepared by a method comprising bringing into contact
  • component (a) comprising one or more lignins
  • component (b) comprising ammonia and/or one or more amine components, and/or any salt thereof and/or an alkali and/or earth alkali metal hydroxide, such as sodium hydroxide and/or potassium hydroxide
  • component (c) comprising one or more oxidation agents
  • component (d) in form of one or more plasticizers.
  • Component (a) comprises one or more lignins.
  • component (a) comprises one or more kraft lignins, one or more soda lignins, one or more lignosulfonate lignins, one or more organosolv lignins, one or more lignins from biorefining processess of lignocellulosic feedstocks, or any mixture thereof.
  • component (a) comprises one or more kraft lignins.
  • component (b) comprises ammonia, one or more amino components, and/or any salts thereof and/or an alkali and/or earth alkali metal hydroxide, such as sodium hydroxide and/or potassium hydroxide.
  • Ammonia-oxidized lignins is to be understood as a lignin that has been oxidized by an oxidation agent in the presence of ammonia.
  • the term “ammonia- oxidized lignin” is abbreviated as AOL.
  • component (b) comprises ammonia and/or any salt thereof.
  • component (b) comprises ammonia and/or any salt thereof.
  • component (b) besides ammonia, one or more amino components, and/or any salts thereof, also comprises a comparably small amount of an alkali and/or earth alkali metal hydroxide, such as sodium hydroxide and/or potassium hydroxide.
  • component (b) comprises alkali and/or earth alkali metal hydroxides, such as sodium hydroxide and/or potassium hydroxide, as a component in addition to the ammonia, one or more amino components, and/or any salts thereof
  • the amount of the alkali and/or earth alkali metal hydroxides is usually small, such as 5 to 70 weight parts, such as 10 to 20 weight parts alkali and/or earth alkali metal hydroxide, based on ammonia.
  • component (c) comprises one or more oxidation agents.
  • component (c) comprises one or more oxidation agents in form of hydrogen peroxide, organic or inorganic peroxides, molecular oxygen, ozone, air, halogen containing oxidation agents, or any mixture thereof.
  • active radicals from the oxidant will typically abstract the proton from the phenolic group as that bond has the lowest dissociation energy in lignin. Due to lignin’s potential to stabilize radicals through mesomerism, multiple pathways open up to continue (but also terminate) the reaction and various intermediate and final products are obtained.
  • the average molecular weight can both increase and decrease due to this complexity (and chosen conditions) and in their experiments, we have typically seen moderate increase of average molecular weight of around 30%.
  • component (c) comprises hydrogen peroxide.
  • Hydrogen peroxide is perhaps the most commonly employed oxidant due to combination of low price, good efficiency and relatively low environmental impact. When hydrogen peroxide is used without the presence of catalysts, alkaline conditions and temperature are important due to the following reactions leading to radical formation:
  • the derivatized lignins prepared with the method according to the present invention contain increased amounts of carboxylic acid groups as a result of the oxidation process. Without wanting to be bound by any particular theory, it is believed that the carboxylic acid group content of the oxidized lignins prepared in the process plays an important role in the desirable reactivity properties of the derivatized lignins prepared by the method.
  • Another advantage of the oxidation process is that the oxidized lignin is more hydrophilic. Higher hydrophilicity can enhance solubility in water and facilitate the adhesion to polar substrates such as mineral fibres.
  • Component (d) comprises one or more plasticizers.
  • component (d) comprises one or more plasticizers in form of polyols, such as carbohydrates, hydrogenated sugars, such as sorbitol, erythriol, glycerol, monoethylene glycol, polyethylene glycols, polyethylene glycol ethers, polyethers, phthalates and/or acids, such as adipic acid, vanillic acid, lactic acid and/or ferullic acid, acrylic polymers, polyvinyl alcohol, polyurethane dispersions, ethylene carbonate, propylene carbonate, lactones, lactams, lactides, acrylic based polymers with free carboxy groups and/or polyurethane dispersions with free carboxy groups, polyamides, amides such as carbamide/urea., or any mixtures thereof. It has been found that the inclusion of component (d) in form of one or more plasticizers provides a decrease of the viscosity of the reaction mixture which allows a very efficient method to produce oxidised lignins.
  • plasticizers in form of
  • component (d) comprises one or more plasticizers in form of polyols, such as carbohydrates, hydrogenated sugars, such as sorbitol, erythriol, glycerol, monoethylene glycol, polyethylene glycols, polyvinyl alcohol, acrylic based polymers with free carboxy groups and/or polyurethane dispersions with free carboxy groups, polyamides, amides such as carbamide/urea, or any mixtures thereof.
  • polyols such as carbohydrates, hydrogenated sugars, such as sorbitol, erythriol, glycerol, monoethylene glycol, polyethylene glycols, polyvinyl alcohol, acrylic based polymers with free carboxy groups and/or polyurethane dispersions with free carboxy groups, polyamides, amides such as carbamide/urea, or any mixtures thereof.
  • component (d) comprises one or more plasticizers selected from the group of polyethylene glycols, polyvinyl alcohol, urea or any mixtures thereof.
  • the method comprises further components, in particular a component (v) in form of an oxidation catalyst, such as one or more transition metal catalyst, such as iron sulfate, such as manganese, palladium, selenium, tungsten containing catalysts.
  • an oxidation catalyst such as one or more transition metal catalyst, such as iron sulfate, such as manganese, palladium, selenium, tungsten containing catalysts.
  • transition metal catalyst such as iron sulfate, such as manganese, palladium, selenium, tungsten containing catalysts.
  • the person skilled in the art will use the components (a), (b), (c), and (d) in relative amounts that the desired degree of oxidation of the lignins is achieved.
  • the method is carried out such that the method comprises
  • component (a) comprises one or more lignins
  • component (b) comprises ammonia
  • - a component (c) comprises one more oxidation agents in form of hydrogen peroxide
  • - a component (d) comprises one or more plasticizers selected from the group of polyethylene glycol, wherein the mass ratios of lignin, ammonia, hydrogen peroxide and polyethylene glycol are such that the amount of ammonia is 0.01 to 0.5 weight parts, such as 0.1 to 0.3, such as 0.15 to 0.25 weight parts ammonia (25 weight% solution in water), based on the dry weight of lignin, and wherein the amount of hydrogen peroxide (30 weight% solution in water) is 0.025 to 1.0 weight parts, such as 0.07 to 0.50 weight parts, such as 0.15 to 0.30 weight parts hydrogen peroxide, based on the dry weight of lignin, and wherein the amount of polyethylene glycol is 0.03 to 0.60 weight parts, such as 0.07 to 0.50 weight parts, such as 0.10 to 0.40 weight parts polyethylene glycol, based on the dry weight of lignin.
  • the method comprises the steps of:
  • component (a) in form of an aqueous solution and/or dispersion of one more lignins, the lignin content of the aqueous solution being 5 to 90 weight-%, such as 10 to 85 weight- %, such as 15 to 70 weight-%, based on the total weight of the aqueous solution;
  • the pH adjusting step is carried so that the resulting aqueous solution and/or dispersion is having a pH > 9, such as > 10, such as > 10.5.
  • the pH adjusting step is carried out so that the resulting aqueous solution and/or dispersion is having a pH in the range of 9.5 to 12.
  • the pH adjusting step is carried out so that the temperature is allowed to raise to > 25 °C and then controlled in the range of 25 - 50 °C, such as 30 - 45 °C, such as 35 - 40 °C.
  • the temperature is allowed to raise to > 35 °C and is then controlled in the range of 35 - 150 °C, such as 40 - 90 °C, such as 45 - 80 °C.
  • the oxidation step is carried out for a time of 1 seconds to 24 hours, such as 1 minutes to 12 hours, such as 10 minutes to 8 hours, such as
  • the method is carried out such that the dry matter content of the reaction mixture is 20 to 80 wt.%, such as 40 to 70 wt.%.
  • the method is carried out such that the viscosity of the oxidised lignin has a value of 100 cP to 100.000 cP, such as a value of 500 cP to 50.000 cP, such as a value of 1.000 cP to 25.000 cP.
  • viscosity is dynamic viscosity and is defined as the resistance of the liquid/paste to a change in shape, or movement of neighbouring portions relative to one another.
  • the viscosity is measured in centipoise (cP), which is the equivalent of 1 mPa s (milipascal second).
  • Viscosity is measured at 20°C using a viscometer.
  • the dynamic viscosity can be measured at 20°C by a Cone Plate Wells Brookfield Viscometer.
  • the method is carried out such that the method comprises a rotator-stator device.
  • the method is carried out such that the method is performed as a continuous or semi-continuous process.
  • Apparatus for performing the method is carried out such that the method is performed as a continuous or semi-continuous process.
  • the present disclosure also includes an apparatus for performing the method described above.
  • the apparatus for performing the method comprises:
  • the apparatus is constructed in such a way that the inlets for the premix of the components (a), (b) and (d) are to the rotor-stator device and the apparatus furthermore comprises a chamber, said chamber having an inlet for component (c) and said chamber having an outlet for an oxidised lignin.
  • a rotator-stator device is a device for processing materials comprising a stator configured as an inner cone provided with gear rings.
  • the stator cooperates with a rotor having arms projecting from a hub. Each of these arms bears teeth meshing with the teeth of the gear rings of the stator. With each turn of the rotor, the material to be processed is transported farther outward by one stage, while being subjected to an intensive shear effect, mixing and redistribution.
  • the rotor arm and the subjacent container chamber of the upright device allow for a permanent rearrangement of the material from the inside to the outside and provide for a multiple processing of dry and/or highly viscous matter so that the device is of excellent utility for the intensive mixing, kneading, fibrillating, disintegrating and similar processes important in industrial production.
  • the upright arrangement of the housing facilitates the material's falling back from the periphery toward the center of the device.
  • the rotator-stator device used in the method comprises a stator with gear rings and a rotor with teeth meshing with the teeth of the stator.
  • the rotator-stator device has the following features: Between arms of the rotor protrudes a guiding funnel that concentrates the material flow coming in from above to the central area of the container.
  • the outer surface of the guiding funnel defines an annular gap throttling the material flow.
  • a feed screw is provided that feeds towards the working region of the device.
  • the guiding funnel retains the product in the active region of the device and the feed screw generates an increased material pressure in the center.
  • the method is carried out such that the method uses one rotator-stator device.
  • the mixing of the components and the reaction of the components is carried out in the same rotator-stator device.
  • the method is carried out such that the method uses two or more rotator-stator devices, wherein at least one rotator-stator device is used for the mixing of the components and at least one rotator-stator device is used for reacting the components.
  • This process can be divided into two steps:
  • Inline rotor-/stator machine which has much higher shear forces - circumferential speeds of up to 55 m/s) - and creates beneficial conditions for a very quick chemical reaction.
  • the machine is to be used continuously.
  • the highly concentrated (45 to 50 wt-%) mass of Lignin/water is prepared.
  • the lignin powder is added slowly to the warm water (30 to 60 deg.C) in which the correct amount of watery ammonia and/or alkali base have been added. This can be done in batch mode, or the materials are added intermittently/continuously creating a continuous flow of mass to the next step.
  • the created mass should be kept at a temperature of about 60 deg. to keep the viscosity as low as possible and hence the material pumpable.
  • the hot mass of lignin/water at a pH of 9 to 12 is then transferred using a suitable pump, e.g. progressive cavity pump or another volumetric pump, to the oxidation step.
  • the oxidation is done in a closed rotor-/stator system in a continuous inline reaction.
  • a watery solution of ammonia and/or alkali base is dosed with a dosing pump into the rotor-/stator chamber at the point of highest turbulence/shear. This ensures a rapid oxidation reaction.
  • the oxidized material (AOL) leaves the inline-reactor and is collected in suitable tanks.
  • the oxidized lignins prepared have very desirable reactivity properties and at the same time display improved fire resistance properties when used in products where they are comprised in a binder composition, and improved long term stability over previously known oxidized lignins.
  • the oxidised lignin also displays improved hydrophilicity.
  • An important parameter for the reactivity of the oxidized lignins prepared is the carboxylic acid group content of the oxidized lignins.
  • the oxidized lignin prepared has a carboxylic acid group content of 0.05 to 10 mmol/g, such as 0.1 to 5 mmol/g, such as 0.20 to 2.0 mmol/g, such as 0.40 to 1.5 mmol/g, such as 0.45 to 1.0 mmol/g, based on the dry weight of component (a).
  • carboxylic acid group content is by using average carboxylic acid group content per lignin macromolecule according to the following formula:
  • the oxidized lignin prepared has an average carboxylic acid group content of more than 1.5 groups per macromolecule of component (a), such as more than 2 groups, such as more than 2.5 groups.
  • Oxidised lignins which can be used as a component for the binder used in the present invention can be prepared by a method comprising bringing into contact
  • component (a) comprising one or more lignins
  • component (b) comprising ammonia and/or one or more amine components, and/or any salt thereof and/or an alkali and/or earth alkali metal hydroxide, such as sodium hydroxide and/or potassium hydroxide,
  • component (c) comprising one or more oxidation agents, optionally a component (d) in form of one or more plasticizers, and allowing a mixing/oxidation step, wherein an oxidised mixture is produced, followed by an oxidation step, wherein the oxidised mixture is allowed to continue to react for a dwell time of dwell time of 1 second to 10 hours, such as 10 seconds to 6 hours, such as 30 seconds to 2 hours.
  • Components (a), (b), (c) and (d) are as defined above under Method II to prepare oxidised lignins.
  • the process comprises a premixing step in which components are brought into contact with each other.
  • the premixing step is carried out as a separate step and the mixing/oxidation step is carried out subsequently to the premixing step.
  • component (c) is then added to the premixture produced in the premixing step.
  • the premixing step corresponds to the mixing/oxidation step.
  • the components for example component (a), component (b) and component (c) are mixed and an oxidation process is started at the same time. It is possible that the subsequent dwell time is performed in the same device as that used to perform the mixing/oxidation step.
  • component (c) is air.
  • the dwell time is so chosen that the oxidation reaction is brought to the desired degree of completion, preferably to full completion.
  • system for performing the method comprises:
  • At least one reaction device in particular at least one reaction tube, which is arranged downstream in the process flow direction to at least one or more of the outlets.
  • the system comprises one or more inlets for component (c) and/or component (d). In one embodiment, the system comprises a premixing device.
  • the premixing device can comprise one or more inlets for water and/or component (a) and/or component (b) and/or component (c) and/or component (d). In one embodiment, the premixing device comprises inlets for water and component (a) and component (b).
  • component (c) is also mixed with the three mentioned ingredients (water, component (a) and component (b)). It is then possible that the premixing device has a further inlet for component (c). If component (c) is air, it is possible that the premixing device is formed by an open mixing vessel, so that in this case component (c) is already brought into contact with the other components (water, component (a) and component (b)) through the opening of the vessel. Also in this embodiment of the invention, it is possible that the premixing device optionally comprises an inlet for component (d).
  • the system is constructed in such a way that the inlets for components (a), (b) and (d) are inlets of a premixing device, in particular of an open rotor-stator device, whereby the system furthermore comprises an additional rotor-stator device, said additional rotor-stator device having an inlet for component (c) and said additional rotor-stator device having an outlet for an oxidized lignin.
  • the premixing step and the mixing/oxidizing step are carried out simultaneously.
  • the premixing device and the mixing/oxidizing device are a single device, i. e. a rotor-stator device.
  • one rotator-stator device used in the method according to the present invention comprises a stator with gear rings and a rotor with teeth meshing with the teeth of the stator.
  • the rotator-stator device has the following features: Between arms of the rotor protrudes a guiding funnel that concentrates the material flow coming in from above to the central area of the container. The outer surface of the guiding funnel defines an annular gap throttling the material flow.
  • a feed screw is provided that feeds towards the working region of the device. The guiding funnel retains the product in the active region of the device and the feed screw generates an increased material pressure in the center.
  • the system for performing the method comprises: - one or more inlets for water, components (a) and (b),
  • mixer/heat-exchanger which is arranged downstream in the process flow direction to the at least one or more of the outlets, whereby the mixer/heat-exchanger comprises a temperature control device.
  • the system comprises additional one or more inlets for component (c) and/or component (d).
  • the system comprises a premixing device.
  • the premixing device can comprise one or more inlets for water and/or component (a) and/or component (b) and/or component (c) and/or component (d).
  • the premixing device comprises inlets for water and component (a) and component (b). It is possible that, in a premixing step, component (c) is also mixed with the three mentioned ingredients (water, component (a) and component (b)). It is then possible that the premixing device has a further inlet for component (c). If component (c) is air, it is possible that the premixing device is formed by an open mixing vessel, so that in this case component (c) is already brought into contact with the other components (water, component (a) and component (b)) through the opening of the vessel. Also in this embodiment of the invention, it is possible that the premixing device optionally comprises an inlet for component (d).
  • the system is constructed in such a way that the inlets for components (a), (b) and (d) are inlets of an open rotor-stator device, whereby the system furthermore comprises a mixer/heat-exchanger, having an inlet for component (c) and an outlet for an oxidized lignin.
  • premixing step and the mixing/oxidizing step are carried out simultaneously.
  • the premixing device and the mixing/oxidizing device are a single device.
  • one rotator-stator device used in the method according to the present invention comprises a stator with gear rings and a rotor with teeth meshing with the teeth of the stator.
  • the rotator-stator device has the following features: Between arms of the rotor protrudes a guiding funnel that concentrates the material flow coming in from above to the central area of the container. The outer surface of the guiding funnel defines an annular gap throttling the material flow.
  • a feed screw is provided that feeds towards the working region of the device. The guiding funnel retains the product in the active region of the device and the feed screw generates an increased material pressure in the center.
  • premixing devices can also be used as premixing devices.
  • the premixing step is carried out in the mixing and oxidizing apparatus.
  • the mixing and oxidizing apparatus is a static mixer.
  • a static mixer is a device for the continuous mixing of fluid materials, without moving components.
  • One design of static mixer is the plate-type mixer and another common device type consists of mixer elements contained in a cylindrical (tube) or squared housing.
  • the mixer/heat-exchanger is constructed as multitube heat exchanger with mixing elements.
  • the mixing element are preferably fixed installations through which the mixture has to flow, whereby mixing is carried out as a result of the flowing through.
  • the mixer/heat-exchanger can be constructed as a plug flow reactor. Examples
  • Compressive strength (in Y-direction) was determined on eight 75 kg/m 3 MMVF cubes with dimensions 10 x 10 x 10 cm.
  • Table 1 shows the results for cubes with a 2.1 wt% binder according to the invention and without any wetting agent.
  • Table 2 shows the results for cubes with 2.1 wt% binder according to the invention and with a sodium lauryl ether sulphate (SLES) wetting agent.
  • SLES sodium lauryl ether sulphate
  • the binder according to the invention had the following composition: -AOL (ammonia oxidised lignin): 1000 kg (284 kg lignin UPM BioPiva, 57 kg H202 (35%), 53 kg NH40H (24.7%), 506 kg water)
  • MMVF substrate comprising 2.1 wt% formaldehyde-free binder according to the present invention; density of 76 kg/m 3 ; 3.5 litres/ton of wetting agent (Texapon®).
  • the binder in this product had the following composition: -AOL (ammonia oxidised lignin): 1000 kg (284 kg lignin UPM BioPiva 100, 57 kg H 2 O 2 (35%), 53 kg NH 4 OH (24.7%), 506 kg water)
  • PEG 200 44 kg -Crosslinker (Primid XL552 - b-hydroxyalkyl- amide (HAA) crosslinker supplied by EMS-Chemie AG) : 22 kg
  • Primid XL552 has the following structure: Product 2: MMVF substrate comprising 2.1 wt% formaldehyde-free binder according to the present invention; density of 76 kg/m 3 ; no wetting agent.
  • the binder in this product is the same as described above for Product 1.
  • Comparative Product 1 MMVF substrate comprising 2.6 wt% PUF binder; density of 77 kg/m 3 ; 5.7 litres/ton of wetting agent (Linear Alkyl Sulphonate).
  • the binder in this product was made as follows:
  • Comparative Product 2 MMVF substrate comprising 2.6 wt% PUF binder; density of 77 kg/m 3 ; 3.5 litres/ton of wetting agent (Texapon®). The binder in this product is the same as described above for Comparative Product 1.
  • Comparative Product 3 MMVF substrate comprising 2.8 wt% formaldehyde-free binder; density of 78 kg/m 3 ; 6.7 litres/ton of wetting agent (LAS). The binder in this product was made by reacting the following together:
  • AAA resin 239 kg Dextrose: 575 kg Water: 1.1 kg Silane.
  • the AAA resin was made as follows:
  • MMVF substrate comprising 2.8 wt% formaldehyde-free binder; density of 78 kg/m 3 ; 3.5 litres/ton of wetting agent (Texapon®).
  • the binder in this product is the same as described above for Comparative Product 3.
  • the binder amount used in Products 1 and 2 of the invention is significantly lower than the amounts used in Comparative Products 1 to 4.
  • comparable compression results are seen when compared with the PUF binder and another formaldehyde-free binder. Therefore, using lower amounts of the binder of the invention, equivalent compression strength is achieved. It would be expected that increasing the binder amount of the invention to 2.8 wt% would result in improved compression strength. However, having comparable compression results at lower amounts provides the added advantage of reducing the total amount of binder in the product.
  • the average buffering, average drainage and average infiltration of MMVF samples were measured.
  • a plexiglass column is prepared using sand and the MMVF sample to be tested.
  • the column is firstly filled with sand to approximately 25 cm in height.
  • the water attenuation element is positioned on top of the sand.
  • the column is filled with water from an adjacent tank.
  • the column is drained. For every 2 litres of water drained from the column, time and weight is noted. This is executed for approximately 2 hours. Then the valve for drainage is closed. - The remaining water infiltrates into the filler sand which leave the column via a hose into buckets. The weight and time after a decrease of 2 litres water is measured for as long as possible.
  • the binder of the invention and the PUF binder were made as described above under Example 2. From the results, it can be seen that the samples of the invention with or without wetting agent show similar properties. The wetting agent, therefore, does not have a significant effect.
  • samples 1 and 2 buffer more quickly than all other compared mineral wool types. Drainage of Samples 1 and 2 (according to the invention) proceeds quicker than Samples 3 and 4 and is similar to Sample 5. Infiltration/discharging of Samples 1 and 2 (according to the invention) proceeds faster than all other compared mineral wool types.
  • a binder as used in the water attenuation element of the invention was prepared as follows:
  • a foam dampening agent (Skumdaemper 11-10 from NCA-Verodan ) is added. The temperature of the batch is maintained at 40°C.
  • kraft lignin is soluble in water at relatively high pH, it is known that at certain weight percentage the viscosity of the solution will strongly increase. It is typically believed that the reason for the viscosity increase lies in a combination of strong hydrogen bonding and interactions of p-electrons of numerous aromatic rings present in lignin. For kraft lignin an abrupt increase in viscosity around 21-22 wt.-% in water was observed and 19 wt.-% of kraft lignin were used in the example presented.
  • Ammonia aqueous solution was used as base in the pH adjusting step.
  • the amount was fixed at 4 wt.-% based on the total reaction weight.
  • the pH after the pH adjusting step and at the beginning of oxidation was 10.7.
  • Table IA2 shows the results of CHNS elemental analysis before and after oxidation of kraft lignin. Before the analysis, the samples were heat treated at 160 °C to remove adsorbed ammonia. The analysis showed that a certain amount of nitrogen became a part of the structure of the oxidised lignin during the oxidation process.
  • the oxidation is an exothermic reaction and increase in temperature is noted upon addition of peroxide.
  • temperature was kept at 60 °C during three hours of reaction.
  • V 2s and V 1s are endpoint volumes of a sample while V 2b and V 1b are the volume for the blank.
  • C acid is 0.1 M HCI in this case and m s is the weight of the sample.
  • Table IA4 The values obtained from aqueous titration before and after oxidation are shown in table IA4.
  • the average COOH functionality can also be quantified by a saponification value which represents the number of mg of KOH required to saponify 1 g lignin. Such a method can be found in AOCS Official Method Cd 3-25. Average molecular weight was also determined before and after oxidation with a PSS PolarSil column (9:1 (v/v) dimethyl sulphoxide/water eluent with 0.05 M LiBr) and UV detector at 280nm. Combination of COOH concentration and average molecular weight also allowed calculating average carboxylic acid group content per lignin macromolecule and these results are shown in table IA5.
  • Example IB upscaling the lignin oxidation in ammonia by hydrogen peroxide to pilot scale
  • the first scale up step was done from 1 L (lab scale) to 9 L using a professional mixer in stainless steel with very efficient mechanical mixing
  • the next scale up step was done in a closed 200 L reactor with efficient water jacket and an efficient propeller stirrer.
  • the scale was this time 180 L and hydrogen peroxide was added in two steps with appr. 30 minute separation.
  • This up-scaling went relatively well, though quite some foaming was an issue partly due to the high degree reactor filling.
  • To control the foaming a small amount of food grade defoamer was sprayed on to the foam. Most importantly the temperature controllable and end temperatures below 70 °C were obtained using external water-cooling.
  • the pilot scale reactions were performed in an 800 L reactor with a water cooling jacket and a twin blade propeller stirring.
  • the content of each of the components in a given oxidised lignin solution is based on the anhydrous mass of the components or as stated below.
  • Kraft lignin was supplier by UPM as BioPiva100TM as dry powder.
  • NH 4 OH 25% was supplied by Sigma-Aldrich and used in supplied form.
  • H 2 O 2 , 30% was supplied by Sigma-Aldrich and used in supplied form or by dilution with water.
  • PEG 200 was supplied by Sigma-Aldrich and were assumed anhydrous for simplicity and used as such.
  • PVA Mw 89.000-98.000, Mw 85.000- 124.000, Mw 130.000, Mw 146.000-186.000
  • Cas no 9002-89-5 were supplied by Sigma-Aldrich and were assumed anhydrous for simplicity and used as such.
  • Urea (Cas no 57-13-6) was supplied by Sigma-Aldrich and used in supplied form or diluted with water.
  • Glycerol (Cas no 56-81-5) was supplied by Sigma-Aldrich and was assumed anhydrous for simplicity and used as such.
  • the content of the oxidised lignin after heating to 200 °C for 1h is termed “Dry solid matter” and stated as a percentage of remaining weight after the heating.
  • Disc-shaped stone wool samples (diameter: 5 cm; height 1 cm) were cut out of stone wool and heat-treated at 580 °C for at least 30 minutes to remove all organics.
  • the solids of the binder mixture were measured by distributing a sample of the binder mixture (approx. 2 g) onto a heat treated stone wool disc in a tin foil container. The weight of the tin foil container containing the stone wool disc was weighed before and directly after addition of the binder mixture.
  • V 2s and Vi s are endpoint volumes of a sample while V 2b and Vi b are the volume for a blank sample.
  • C acid is 0.1 M HCI in this case and m s,g is the weight of the sample.
  • entry numbers of the oxidised lignin example correspond to the entry numbers used in Table II.
  • Example IIA 71 ,0 g lignin UPM Biopiva 100 was dissolved in 149,0 g water at 20°C and added 13,3 g 25% NH 4 OH and stirred for 1h by magnetic stirrer, where after 16,8g H 2 O2 30% was added slowly during agitation. The temperature was increased to 60°C in the water bath. After 1h of oxidation, the water bath was cooled and hence the reaction was stopped. The resulting material was analysed for COOH, dry solid matter, pH, viscosity and density.
  • a Cavitron CD1000 rotor-stator device was used to carry out the mixing/oxidation step.
  • the rotor-stator device was run at 250 Hz (55 m/s circumferential speed) with a counter pressure at 2 bar.
  • the dwell time in the reaction tube was 3,2 minutes and in the reaction vessel 2 hours.
  • This premixture was then transferred to a static mixer and a mixer/heat- exchanger, where the oxidation was made by use of H202 (35 vol%). Dosage of the premixture was 600 l/h and the H202 was dosed at 17,2 l/h. The dwell time in the mixer/heat-exchanger was 20 minutes. The temperature of the mixture increased during the oxidation step up to 95 °C.
  • the final product was analysed for the COOH group content, dry solid matter, pH, viscosity and remaining H202.
  • a binder was made based on this AOL: 49,3 g AOL (19,0 % solids), 0,8 g primid XL552 (100 % solids) and 2,4 g PEG200 (100 % solids) were mixed with 0,8 g water to yield 19% solids; and then used for test of mechanical properties in bar tests.
  • the mechanical strength of the binders was tested in a bar test. For each binder, 16 bars were manufactured from a mixture of the binder and stone wool shots from the stone wool spinning production.
  • the aged bars as well as five unaged bars were broken in a 3 point bending test (test speed: 10.0 mm/min; rupture level: 50%; nominal strength: 30 N/mm 2 ; support distance: 40 mm; max deflection 20 mm; nominal e- module 10000 N/mm 2 ) on a Bent Tram machine to investigate their mechanical strengths.

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Abstract

L'invention concerne une structure de toit plat comprenant au moins une couche d'atténuation d'eau, laquelle comprend au moins un élément d'atténuation d'eau formé de fibres vitreuses artificielles liées avec une composition de liant durci. La structure de toit plat comprend en outre une couche de réduction d'eau au-dessous de la couche d'atténuation d'eau et au moins un point d'évacuation en communication fluidique avec la couche d'atténuation d'eau et agencé de manière à diriger l'eau de la structure de toit plat vers le sol. Le liant est une composition aqueuse qui comprend un composant (i) sous la forme d'une ou de plusieurs lignines oxydées ; un composant (ii) sous la forme d'un ou de plusieurs agents de réticulation ; un composant (iii) sous la forme d'un ou de plusieurs plastifiants.
PCT/EP2020/059655 2020-04-03 2020-04-03 Système de toit WO2021197633A1 (fr)

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Publication number Priority date Publication date Assignee Title
EP0583086A1 (fr) 1992-08-06 1994-02-16 Rohm And Haas Company Composition aqueuse et thermodurcissable et son utilisation comme liant pour non-tissés en fibres de verre
US5318990A (en) 1993-06-21 1994-06-07 Owens-Corning Fiberglas Technology Inc. Fibrous glass binders
WO1999036368A1 (fr) 1998-01-16 1999-07-22 Rockwool International A/S Compose servant de liant de fibres minerales et son procede de preparation
EP0990727A1 (fr) 1998-10-02 2000-04-05 Johns Manville International Inc. Liant pour fibre de verre à base de polycarboxy/polyol
WO2001005725A1 (fr) 1999-07-16 2001-01-25 Rockwool International A/S Resine destinee a un liant pour laine minerale et comprenant le produit de reaction d'une amine avec un premier et un second anhydride
WO2001096460A2 (fr) 2000-06-16 2001-12-20 Rockwool International A/S Liants pour produits de laine minerale
WO2002006178A1 (fr) 2000-07-04 2002-01-24 Rockwool International A/S Liant pour produits du type laine minerale
US20030042344A1 (en) 2001-08-29 2003-03-06 Klaus Fisch Device for processing materials
WO2004007615A1 (fr) 2002-07-15 2004-01-22 Rockwool International A/S Composition de liant aqueuse sans formaldehyde pour fibres minerales
US6818699B2 (en) 2000-09-28 2004-11-16 Unitika Ltd. Aqueous dispersion of polyester resin, production method of the same, and aqueous coating composition
WO2006061249A1 (fr) 2004-12-10 2006-06-15 Rockwool International A/S Liant aqueux destine a des fibres minerales
EP1741726A1 (fr) 2005-07-08 2007-01-10 Rohm and Haas France SAS Composition aqueuse durcissable et son utilisation comme liant hydrofuge pour fibres de verre non-tissées
US20070173588A1 (en) 2003-04-16 2007-07-26 Saint-Gobain Isover Mineral fibre sizing composition containing a carboxylic polyacid and a polyamine, preparation method thereof and resulting products
WO2008023032A1 (fr) 2006-08-23 2008-02-28 Rockwool International A/S Liant aqueux modifié par l'urée pour fibres minérales
WO2016120576A1 (fr) * 2015-01-30 2016-08-04 Saint-Gobain Isover Composition d'encollage pour laine minerale a base de lignosulfonate et d'un compose carbonyle, et produits isolants obtenus
WO2020018599A2 (fr) 2018-07-16 2020-01-23 Green Roof Specialty Products Llc Couche de drainage par frottement dans un toit végétalisé, un pavage ou un ensemble solaire
WO2020058384A1 (fr) 2018-09-21 2020-03-26 Low & Bonar Inc. Appareil et procédé de gestion d'eau de ruissellement de toit

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0583086A1 (fr) 1992-08-06 1994-02-16 Rohm And Haas Company Composition aqueuse et thermodurcissable et son utilisation comme liant pour non-tissés en fibres de verre
US5318990A (en) 1993-06-21 1994-06-07 Owens-Corning Fiberglas Technology Inc. Fibrous glass binders
WO1999036368A1 (fr) 1998-01-16 1999-07-22 Rockwool International A/S Compose servant de liant de fibres minerales et son procede de preparation
US6706853B1 (en) 1998-01-16 2004-03-16 Rockwool International A/S Compound for use as a mineral fibre binder and process for providing such
EP0990727A1 (fr) 1998-10-02 2000-04-05 Johns Manville International Inc. Liant pour fibre de verre à base de polycarboxy/polyol
WO2001005725A1 (fr) 1999-07-16 2001-01-25 Rockwool International A/S Resine destinee a un liant pour laine minerale et comprenant le produit de reaction d'une amine avec un premier et un second anhydride
WO2001096460A2 (fr) 2000-06-16 2001-12-20 Rockwool International A/S Liants pour produits de laine minerale
WO2002006178A1 (fr) 2000-07-04 2002-01-24 Rockwool International A/S Liant pour produits du type laine minerale
US6818699B2 (en) 2000-09-28 2004-11-16 Unitika Ltd. Aqueous dispersion of polyester resin, production method of the same, and aqueous coating composition
US20030042344A1 (en) 2001-08-29 2003-03-06 Klaus Fisch Device for processing materials
WO2004007615A1 (fr) 2002-07-15 2004-01-22 Rockwool International A/S Composition de liant aqueuse sans formaldehyde pour fibres minerales
US20070173588A1 (en) 2003-04-16 2007-07-26 Saint-Gobain Isover Mineral fibre sizing composition containing a carboxylic polyacid and a polyamine, preparation method thereof and resulting products
WO2006061249A1 (fr) 2004-12-10 2006-06-15 Rockwool International A/S Liant aqueux destine a des fibres minerales
EP1741726A1 (fr) 2005-07-08 2007-01-10 Rohm and Haas France SAS Composition aqueuse durcissable et son utilisation comme liant hydrofuge pour fibres de verre non-tissées
WO2008023032A1 (fr) 2006-08-23 2008-02-28 Rockwool International A/S Liant aqueux modifié par l'urée pour fibres minérales
WO2016120576A1 (fr) * 2015-01-30 2016-08-04 Saint-Gobain Isover Composition d'encollage pour laine minerale a base de lignosulfonate et d'un compose carbonyle, et produits isolants obtenus
WO2020018599A2 (fr) 2018-07-16 2020-01-23 Green Roof Specialty Products Llc Couche de drainage par frottement dans un toit végétalisé, un pavage ou un ensemble solaire
WO2020058384A1 (fr) 2018-09-21 2020-03-26 Low & Bonar Inc. Appareil et procédé de gestion d'eau de ruissellement de toit

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Title
CHEMICAL ABSTRACTS, Columbus, Ohio, US; abstract no. 9002-89-5

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