EP2999749A1 - Process for preparing sulphur-aggregate composite - Google Patents
Process for preparing sulphur-aggregate compositeInfo
- Publication number
- EP2999749A1 EP2999749A1 EP14725457.7A EP14725457A EP2999749A1 EP 2999749 A1 EP2999749 A1 EP 2999749A1 EP 14725457 A EP14725457 A EP 14725457A EP 2999749 A1 EP2999749 A1 EP 2999749A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sulphur
- filler
- aggregate
- pellets
- bitumen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C7/00—Coherent pavings made in situ
- E01C7/08—Coherent pavings made in situ made of road-metal and binders
- E01C7/18—Coherent pavings made in situ made of road-metal and binders of road-metal and bituminous binders
- E01C7/182—Aggregate or filler materials, except those according to E01C7/26
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C7/00—Coherent pavings made in situ
- E01C7/08—Coherent pavings made in situ made of road-metal and binders
- E01C7/10—Coherent pavings made in situ made of road-metal and binders of road-metal and cement or like binders
- E01C7/14—Concrete paving
- E01C7/142—Mixtures or their components, e.g. aggregate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2555/00—Characteristics of bituminous mixtures
- C08L2555/20—Mixtures of bitumen and aggregate defined by their production temperatures, e.g. production of asphalt for road or pavement applications
- C08L2555/22—Asphalt produced above 140°C, e.g. hot melt asphalt
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2555/00—Characteristics of bituminous mixtures
- C08L2555/40—Mixtures based upon bitumen or asphalt containing functional additives
- C08L2555/50—Inorganic non-macromolecular ingredients
- C08L2555/52—Aggregate, e.g. crushed stone, sand, gravel or cement
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2555/00—Characteristics of bituminous mixtures
- C08L2555/40—Mixtures based upon bitumen or asphalt containing functional additives
- C08L2555/50—Inorganic non-macromolecular ingredients
- C08L2555/54—Sulfur or carbon black
Definitions
- the present invention provides a process for the preparation of a sulphur-aggregate composite.
- Elemental sulphur or modified sulphur can be used to bind aggregate and filler, thereby providing sulphur- aggregate composites such as sulphur concrete and sulphur asphalt .
- Sulphur concrete can be used in a variety of pre-cast concrete applications such as marine defences, paving slabs, road barriers and retaining walls.
- Sulphur asphalt wherein bitumen and sulphur are used to bind aggregate and filler, is typically used in the road construction and road paving industry.
- Sulphur dusts are potentially explosive so processes for the preparation of sulphur-aggregate composites must be carefully controlled to reduce the risk of sulphur dust explosions.
- the present inventors have sought to provide a process for the preparation of sulphur- aggregate composites having a reduced risk of sulphur dust explosion.
- the present invention provides a process for the preparation of a sulphur-aggregate composite comprising the steps of :
- sulphur-aggregate composite refers to a composite comprising sulphur, filler and aggregate.
- Fillers and aggregate are particulate inorganic
- Fillers have an average particle size in the range of from 0.1 ⁇ to 0.1 mm.
- Fine aggregate has an average particle size in the range of from 0.1 to 5mm.
- Coarse aggregate has an average particle size in the range of from 5 to 40mm.
- the present invention provides a process for the preparation of sulphur concrete.
- Sulphur concrete comprises sulphur, filler, coarse aggregate, and optionally fine aggregate.
- the present invention provides a process for the preparation of sulphur mortar.
- Sulphur mortar comprises sulphur, filler and fine aggregate, but does not comprise coarse aggregate .
- the present invention provides a process for the preparation of sulphur asphalt.
- Sulphur asphalt comprises sulphur, bitumen, filler and fine and/or coarse aggregate.
- the process of the invention comprises the steps of
- the mixing steps (c) and (e) may be combined in one step (i.e. the mixture of sulphur pellets and filler, the hot aggregate and the hot bitumen are mixed together in one step) or may be two separate steps (i.e. the mixture of sulphur pellets and filler may be mixed with the hot aggregate, and then may be subsequently mixed with the hot bitumen, or the hot bitumen may be mixed with the hot aggregate and then may be subsequently mixed with the mixture of sulphur pellets and filler, or the mixture of sulphur pellets and filler may be mixed with the hot bitumen and then may be subsequently mixed with the hot aggregate) .
- Sulphur is used the form of sulphur pellets.
- pellets is to any type of sulphur material that has been cast from the molten state into some kind of regularly sized particle, for example flakes, slates or sphere-shaped sulphur such as prills, granules, nuggets and pastilles or half pea sized sulphur.
- the sulphur pellets typically comprise from 50 to 100wt% of sulphur, based upon the weight of the sulphur pellets, preferably from 60wt% and most
- the sulphur pellets are 100wt% sulphur.
- the sulphur pellets may contain carbon black and, optionally, other ingredients, such as amyl acetate and wax.
- Carbon black may be present in amounts up to 5%wt, based on the pellet, preferably up to 2%wt.
- the content of carbon black in the sulphur pellet is at least 0.25%wt.
- the content of other ingredients, such as amyl acetate and wax typically does not exceed an amount of 1.0%wt each.
- wax When wax is present, it may be in the form of, for example, slack wax or wax derived from a Fischer-Tropsch process. Examples of suitable waxes for use herein are Sasobit (RTM) , a Fischer-Tropsch derived wax commercially available from Sasol, and SX100 wax, a Fischer-Tropsch wax from Shell Malaysia.
- RTM Sasobit
- SX100 wax a Fischer-Tropsch wax from Shell Malaysia.
- a suitable sulphur pellet for use herein is Thiopave (RTM) pellets commercially available from Shell.
- RTM Thiopave
- Another type of sulphur pellet that is advantageously used in the process of the invention is a pellet prepared by forming solidified sulphur seed particles by a method including intersecting a spray of water droplets through a spray of liquid sulphur droplets to thereby form the solidified sulphur seed particles, and, thereafter, coating the solidified sulphur seed particles with at least one layer of liquid sulphur, wherein each of the at least one layer of liquid sulphur is solidified thereby forming the sulphur particles.
- the sulphur pellets provided to the process will inherently contain a certain amount of sulphur dust.
- sulphur dust is defined as sulphur particles with longest dimensions smaller than 63 ⁇ . This dust is primarily produced during transportation of the sulphur pellets. The amount of dust will vary from batch to batch, and will even vary within a batch, e.g. there may be more dust at the bottom of a bag of pellets. It is this dust, inherently present within the sulphur pellets, that is primarily responsible for the risk of explosion. Further dust may be produced during the process for the preparation of the sulphur aggregate composite, but it is the dust present within the sulphur pellets that is most problematic.
- the filler used in step (a) is typically any available inorganic filler material.
- the filler is a material that provides non-explosible dusts.
- the filler is suitably chosen from limestone, fly ash, quartz, Portland cement, alumina, titania, carbon black, gypsum, talc, gabbro or mica.
- the filler is preferably chosen from limestone, fly ash, quartz and Portland cement.
- the weight ratio of sulphur pellets to filler in step (a) is suitably between 1:5 and 5:1, preferably between 1:2 and 2:1, most preferably about 1:1.
- the inventors have found that using a weight ratio of sulphur pellets to filler within this range can provide dusts with reduced explosibility and can also provide sulphur- aggregate composites with desirable properties. If insufficient filler is used, then this may not be used.
- step (a) it may be desirable to increase the amount of filler in step (a) .
- the preferred amount of filler will also be determined by the desired properties of the final sulphur-aggregate composite. It is possible to incorporate further filler in the sulphur- aggregate composite, e.g. by heating additional filler with the aggregate in step (b) and mixing this additional filler with the mixture of sulphur pellets and filler and hot aggregate in step (c) .
- the amounts of sulphur, filler and aggregate in the sulphur-aggregate composites of the invention can be chosen by the skilled person in view of the proposed application of the sulphur-aggregate composite. The skilled person will seek to ensure that sufficient sulphur is incorporated to bind the filler and aggregate, that sufficient filler and aggregate are incorporated to provide mechanical strength and that the balance of components provides a mixture with suitable workability for the proposed application.
- the presence of sulphur can improve the strength and rutting resistance of the paving mixture and it is important to include sufficient sulphur to realise these advantages.
- too much sulphur can decrease the workability of the sulphur asphalt paving mixture .
- Sulphur mortar preferably comprises from 5 to 40wt% sulphur, from 45 to
- Sulphur concrete preferably comprises from 5 to 40wt% sulphur, from 25 to 50wt% coarse aggregate, from 20 to 40wt% fine aggregate and from 1 to 10wt% filler; more preferably from 5 to 30wt% sulphur, from 30 to 40wt% coarse aggregate, from 25 to 35wt% fine aggregate and from 3 to 8wt% filler.
- Sulphur asphalt preferably comprises from 0.5 to 8wt% sulphur, from 2 to 10wt% bitumen, from 10 to 70wt% aggregate and from 30 to 90wt% filler; more preferably from 0.8 to 3wt% sulphur, from 3 to 6wt% bitumen, from 20 to 60wt% aggregate and from 40 to 80wt% filler.
- the weight percentages are based upon the weight of the sulphur-aggregate composite.
- the sulphur-aggregate composite When the sulphur-aggregate composite is sulphur concrete or sulphur mortar, the sulphur-aggregate composite preferably comprises modifier. Sulphur
- modifiers are compounds that improve the durability of sulphur concrete and sulphur mortar.
- the amount of modifier is preferably from 0.001 to lwt%, more
- the modifier is typically one of the most expensive components in the concrete, so it is desirable to limit the amount of modifier.
- Suitable modifiers include olefinic modifiers such as 5 ethylidene-2- norbornene (ENB) , 5 vinyl-2-norbornene (VNB) ,
- the modifier may be an organosilane or an organotitanate. Particularly preferred organosilanes are
- the modifier is present in the sulphur pellets.
- the modified is added separately to the process, e.g. during step (c) .
- the sulphur-aggregate composite When the sulphur-aggregate composite is sulphur asphalt, the sulphur-aggregate composite comprises bitumen.
- the bitumen can be selected from a wide range of bituminous compounds .
- the bitumen that can be employed may be straight run bitumen, thermally cracked residue or precipitation bitumen, e.g. from propane.
- the bitumen may also have been subjected to blowing.
- the blowing may be carried out by treating the bitumen with an oxygen-containing gas, such as air, oxygen-enriched air, pure oxygen or any other gas that comprises molecular oxygen and an inert gas, such as carbon dioxide or nitrogen.
- the blowing operation may be conducted at temperatures of 175 to 400°C, preferably from 200 to 350°C.
- the blowing treatment may be conducted by means of a catalytic process.
- the bitumen is preferably a paving grade bitumen suitable for road application having a penetration of, for example, from 9 to lOOOdmm, more preferably of from 15 to 450dmm (tested at 25°C according to EN 1426: 1999) and a softening point of from 25 to 100°C, more preferably of from 25 to 60°C (tested according to EN 1427: 1999).
- step (a) of the process of the invention sulphur pellets are mixed with filler to provide a mixture of sulphur pellets and filler.
- the sulphur pellets may be mixed with the filler simply by pouring the filler into a weigh bin (or hopper) followed by the sulphur pellets. Then both components are provided simultaneously to step (c) .
- the sulphur pellets may be mixed with the filler by providing both the sulphur pellets and the filler to a conveyor belt, which then transports these components to step (c) .
- Step (c) may be carried out at ambient temperature, although it is possible that the filler may be at a higher temperature if it has just been dried.
- step (b) of the process of the invention aggregate is heated to provide hot aggregate.
- the aggregate is preferably heated to a temperature of from 125 to 190°C, more preferably from 125 to 150°C. If the temperature is below 125°C, it is possible that the aggregate will not melt the sulphur pellets when they are combined in step (c) . If the temperature too high, then this increases the potential for producing undesirable fumes of hydrogen sulphide and sulphur dioxide.
- Step (b) suitably takes place in an aggregate dryer drum.
- step (c) of the process of the invention the mixture of sulphur pellets and filler is mixed with the hot aggregate.
- This step is suitably carried out at a temperature at which the sulphur is molten, i.e.
- Step (c) suitably takes place in a pug mill.
- step (c) can take place in a drum or in an after-coater .
- the process of the invention provides further steps of
- bitumen is preferably heated at a temperature of from 60°C to 200°C, preferably from 80 to
- Step (d) suitably takes place in a bitumen tank.
- the mixing steps (c) and (e) may be combined in one step (i.e. the mixture of sulphur pellets and filler, the hot aggregate and the hot bitumen are mixed together in one step) or may be two separate steps (i.e. the mixture of sulphur pellets and filler may be mixed with the hot aggregate, and then may be subsequently mixed with the hot bitumen, or the hot bitumen may be mixed with the hot aggregate and then may be subsequently mixed with the mixture of sulphur pellets and filler, or the mixture of sulphur pellets and filler may be mixed with the hot bitumen and then may be subsequently mixed with the hot aggregate) .
- the hot bitumen is mixed with the hot aggregate, and then there is subsequent mixing with the mixture of sulphur pellets and filler as this may provide reduced fuming.
- the process of the invention suitably provides further steps of
- step (f) pouring the product of step (c) into a mould; and (g) cooling.
- the sulphur-aggregate composite After cooling, the sulphur-aggregate composite can be demoulded .
- sulphur-aggregate composite may be incorporated into the sulphur-aggregate composite.
- polymers for sulphur asphalt it may be desirable to include polymers in to the composition. These polymers may be pre-blended with the bitumen or may be added in one of the mixing steps, i.e. in step (c) or step (e) .
- One preferred type of polymer is a copolymer comprising one or more vinyl aromatic compounds and one or more conjugated dienes, such as styrene-butadiene-styrene . This is desirably pre-blended with the bitumen.
- Another preferred type of polymer is a copolymer formed from monomers including ethylene and glycidyl methacrylate or glycidyl acrylate.
- For sulphur concrete or sulphur mortar it may be desirable to incorporate pigments and it is preferable to incorporate modifiers as described above.
- the invention further provides a process for preparing an asphalt pavement, wherein sulphur asphalt is prepared by a process according to the invention, and further comprising steps of :
- step (h) spreading the product of step (e) into a layer; and (i) compacting the layer.
- Tests were carried out to determine the limiting sulphur concentration, i.e. the maximum quantity (%wt.) of sulphur dust mixed with the filler dust that is non- explosible across a wide range of dust loadings. The tests were carried out using a 20-litre sphere and conformed to the principles of BS EN 14034-1: and BS EN
- the standard test involved charging a known quantity of dust into the charge port of the sphere, which is then pressurised to 20 barg.
- the sphere was evacuated to -600 mbarg and the dust was injected into it from the charge port via a fast acting valve.
- the combination of vacuum in the sphere and pressure in the charge port resulted in net pressure of 0 barg when the dust was dispersed in the sphere.
- Tests involving hybrid admixtures were all carried out in a nominal 10% Lower Explosive
- the sphere was evacuated to -900 mbarg.
- Vaporisation of the ethanol was facilitated by the reduced pressure within the vessel and corresponded to a rise in the pressure within the vessel.
- the rise in pressure was measured using a digital precision pressure gauge accurate to 0.1 mbar (a pressure rise of 1 mbar is equivalent to 0.1% vol) thus allowing accurate measurement of the quantity of ethanol introduced.
- the LEL of ethanol was taken to be 3.3% vol. and the nominal volume of ethanol vapour required for the tests was 10% of the LEL, 0.33% vol. This corresponded to a pressure rise of 3.3 mbar when injecting the ethanol into the sphere.
- the ethanol was injected into the sphere using a precision HPLC syringe. A nominal volume of 0.08ml ethanol was required to generate the required vapour pressure. However, the suction from the sphere pulled the ethanol from the syringe, making control of the actual injected volume difficult.
- the volume injected into the sphere varied giving pressure rises between 2.8 mbar and 4.0 mbar, which equate to 0.28% vol. (8.5% of LEL) and 0.40% vol. (12.1% of LEL) .
- the filler materials were limestone, flyash, quartz and Portland cement.
- Table 1 shows the composition of the mixtures, the Test Protocol used, the Ignition Energy and whether the mixture was explosible or non-explosible .
- the ignition energy has a significant effect on the explosibility of the limestone and sulphur mixtures .
- the limiting sulphur concentration of mixtures of sulphur with Portland cement is 6% sulphur by wt .
- sulphur pellets are provided in combination with filler and the resulting dusts will contain both sulphur dust and filler. These dusts will have a lower risk of explosion when compared to dusts containing sulphur alone. These dusts may not always be non-explosible (depending on the relative amounts of sulphur dust and filler, and
- the present invention has provided the inventors with an additional means of reducing the risk of sulphur dust explosion.
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- Engineering & Computer Science (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Road Paving Structures (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP14725457.7A EP2999749A1 (en) | 2013-05-21 | 2014-05-21 | Process for preparing sulphur-aggregate composite |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP13168532 | 2013-05-21 | ||
PCT/EP2014/060436 WO2014187857A1 (en) | 2013-05-21 | 2014-05-21 | Process for preparing sulphur-aggregate composite |
EP14725457.7A EP2999749A1 (en) | 2013-05-21 | 2014-05-21 | Process for preparing sulphur-aggregate composite |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2999749A1 true EP2999749A1 (en) | 2016-03-30 |
Family
ID=48484999
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14725457.7A Withdrawn EP2999749A1 (en) | 2013-05-21 | 2014-05-21 | Process for preparing sulphur-aggregate composite |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP2999749A1 (en) |
EA (1) | EA028817B1 (en) |
WO (1) | WO2014187857A1 (en) |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6824600B2 (en) * | 2000-05-23 | 2004-11-30 | Shell Canada Limited | Paving binders and manufacturing methods |
EP2714791A1 (en) * | 2011-05-25 | 2014-04-09 | Shell Internationale Research Maatschappij B.V. | Asphalt composition |
-
2014
- 2014-05-21 EP EP14725457.7A patent/EP2999749A1/en not_active Withdrawn
- 2014-05-21 EA EA201592209A patent/EA028817B1/en not_active IP Right Cessation
- 2014-05-21 WO PCT/EP2014/060436 patent/WO2014187857A1/en active Application Filing
Non-Patent Citations (2)
Title |
---|
None * |
See also references of WO2014187857A1 * |
Also Published As
Publication number | Publication date |
---|---|
EA028817B1 (en) | 2018-01-31 |
EA201592209A1 (en) | 2016-04-29 |
WO2014187857A1 (en) | 2014-11-27 |
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