WO2010082856A1 - Procédé de fabrication d'un liant polymère de construction et liant polymère de construction - Google Patents

Procédé de fabrication d'un liant polymère de construction et liant polymère de construction Download PDF

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Publication number
WO2010082856A1
WO2010082856A1 PCT/PL2009/000109 PL2009000109W WO2010082856A1 WO 2010082856 A1 WO2010082856 A1 WO 2010082856A1 PL 2009000109 W PL2009000109 W PL 2009000109W WO 2010082856 A1 WO2010082856 A1 WO 2010082856A1
Authority
WO
WIPO (PCT)
Prior art keywords
waste
weight
sulfur
slag
polymeric construction
Prior art date
Application number
PCT/PL2009/000109
Other languages
English (en)
Inventor
Andrzej Janiczek
Original Assignee
Myslowski, Wlodzimierz
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
Priority claimed from PL387038A external-priority patent/PL213685B1/pl
Priority claimed from PL388298A external-priority patent/PL213520B1/pl
Application filed by Myslowski, Wlodzimierz filed Critical Myslowski, Wlodzimierz
Priority to EA201170892A priority Critical patent/EA018572B1/ru
Publication of WO2010082856A1 publication Critical patent/WO2010082856A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/36—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing sulfur, sulfides or selenium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • This invention relates to the method of production of polymeric construction binder and polymeric construction binder based on granular blast-furnace slag and waste sulfur as well as waste slag from copper smelting and waste sulfur.
  • Polymeric construction binder based on blast-furnace slag and waste sulfur is material similar to traditional concrete based on Portland cement, which, unlike traditional concrete, possesses the following advantages: high compression and bending strength, higher than that of traditional concrete, short setting time during a few hours, low absorbability, good tightness, acid environment resistance, which most of building materials are not resistant to.
  • Sulfur binders manufactured the same in Poland are based on organic modifiers of the olefin hydrocarbon type. Such solutions are dangerous in use due to the risk of fire or explosion during the modification process and their toxic effect on personnel.
  • the aim of the invention is to develop a method of production of polymeric construction binder and polymeric construction binder based on blast-furnace slag or waste slag from copper smelting and to use waste sulfur and waste phosphogypsum as blast-furnace slag or waste slag from copper smelting pH reaction regulator in the production process, that results in reduction of the accumulated noxious waste amounts and allows to utilize them in an environmentally safe way.
  • the polymeric construction material according to the invention is produced when blast-furnace slag, broken up to 10 mm granulation and previously subjected to pH reaction regulation from pH of about 10 to pH of about 6.5 that is, to slightly acidic, using waste phosphogypsum, is added to liquid waste sulfur in the temperature of 130°C - 135°C.
  • metals contained in blast-furnace slag such as arsenic, selenium, phosphorus and their sulfides, inhibit the sulfur crystallization process and stabilize its polymeric form.
  • Sulfur S x chain structures replacing the cyclic structure dominate in the temperature of 130°C - 135°C.
  • Metals and their sulfides, including arsenic, selenium and phosphorus, which are sulfur modifiers, contained in blast-furnace slag undergo copolymerisation reaction with chain-structured sulfur and create a copolymer of highly-molecular compound qualities, such as occur in polymeric materials.
  • Polymeric construction material related to in the invention is composed from 40% - 60% by weight of waste sulfur, 20% - 45% by weight of blast-furnace slag of up to 10 mm granulation, which contains about 90% by weight of silicates, about 5% by weight of metals, including arsenic, selenium, phosphorus and their sulfides as well as metallic oxides, about 5% by weight of water, mixed with waste phosphogypsum, that is, blast-furnace pH reaction regulator, in the amount of 15% - 23% by weight.
  • Waste phosphogypsum mixed with blast-furnace slag in 1 :1 weight ratio changes the blast-furnace slag pH from the pH of about 10 to the pH of about 6.5, that is, to slightly acidic.
  • sulfur When loaded to a rotating heater (Fig.1), sulfur is heated to the temperature of 130 0 C - 135°C and takes the liquid form by disintegration of cyclic sulfur to linear form.
  • Previously weighted amounts of blast-furnace slag mixed with waste phosphogypsum, that is, with blast-furnace slag pH reaction regulator, are batched to liquid sulfur.
  • Polymeric construction binder created in this way can have a particular application through pouring it into a mould, pouring out on a particular surface instead of concrete based on construction cements.
  • Polymeric construction binder has not been reported to initiate reinforcement steel corrosion, however, reinforcement should be protected from penetration of the surrounding during steel reinforcement works in wet environment.
  • Polymeric construction material can be, after cooling, crushed in a jaw crusher and packed into bags, and then poured into a road machine called a road recycler, where, after the material is heated to an appropriate temperature, melted mass can be poured out onto a particular surface and used in roads and yards repairs.
  • Appropriate amount of polymeric construction binder added to road surfacing compositions decreases the amount of used road asphalt in these compositions by about 2% by weight and thus, decreases the costs of road construction.
  • polymeric construction material increases the temperature of road surface softening and prevents its rutting, that lengthens the period of road using.
  • Polymeric construction binder based on sulfur and blast-furnace slag possesses very good functional properties, that is, high compression strength of about 55 MPa, breaking strength of about 5 MPa, bending strength of about 7.5 MPa, water absorbability of about 1 %. Watertightness and frost resistance depend on proper vibrating of profiles made of the binder.
  • Polymeric construction binder is resistant to acidic environment; it has excellent adhesion to substrate and mineral materials used in road construction. In addition to this, it fills fissures and hollows in damaged concrete and road surfaces tightly.
  • Used blast-furnace slag composed of about 90% by weight of silicates, about 5% by weight of metals, including arsenic, selenium, phosphorus and their sulfides and metal oxides, about 5% by weight of water, is grey and it is used in broken-up form; to change its pH reaction from about 10 to pH reaction of about 6.5 it is mixed with waste phosphogypsum of pH reaction of about 4.
  • Phosphogypsum is a waste product of industrial phosphoric acid production.
  • Waste sulfur is a waste product of natural gas desulfurization or crude oil desulfurization, which assumes brown colour after it is melted. Production method of polymeric construction binder based on blast-furnace slag and waste sulfur according to the invention has been defined more closely in the examples of embodiment.
  • weighted amount of waste sulfur is delivered to the BO rotating heater (Fig. 1) through ZS charge.
  • the rotating heater With inside zone confined by two metal rings, sulfur is heated to the temperature of 130 0 C - 135°C with the help of two P burners and it changes its form from solid to liquid brown.
  • Temperature measurement in the sulfur heating zone is carried out by T thermometers.
  • the heater is placed at the inclination angle of 0°, and thus the molten sulfur rotates on the inside circumference of the heater and it is not shifted to the heater outlet.
  • Weighted amounts of dry blast-furnace slag mixed beforehand with waste phosphogypsum as the pH reaction regulator are batched through ZS charge to the heated sulfur.
  • the BO heater gains the slope of about 15°, as a result of which polymeric construction binder is removed from the heater and poured into a mould, onto a specified surface or it is cooled, broken up and packed into bags.
  • Polymeric construction binder obtained in this way is of colour grey similar to traditional concretes. It possesses high mechanical compression strength of about 55 MPa, resistance to acids, salts, oils.
  • the short time of polymeric construction binder setting allows for fast using of elements made of it; the bending strength is of about 7.5 MPa and breaking strength is of about 5 MPa.
  • the BO rotating heater possesses individual M drive and 00 gas exhaust draught. The BO rotating heater works in cycles, that is, after the produced polymeric construction binder has been removed from the heater, another cycle of loading waste sulfur, melting it and adding blast-furnace slag is repeated. In one cycle about 4 tons of polymeric construction binder are obtained.
  • Mode of preparation is identical with that from Example I; the difference is the percentage composition and the colour of the obtained polymeric construction binder lighter than of that obtained in Example I.
  • the invention involves also the development of polymeric construction material based on waste slag from copper smelting and waste sulfur.
  • Polymeric construction material according to this invention is formed when waste slag from copper smelting of 0 - 5 mm granulation is added to liquid waste sulfur at the temperature of 125°C - 135°C. Waste slag from copper smelting has the pH reaction of about 8.5 and thus it is subjected to the pH reaction regulation process by waste phosphogypsum to the pH reaction of about 6.0, which is slightly acidic.
  • Waste slag from copper smelting contains metals such as copper, phosphorus and their sulfides, which are extremely valuable in the sulfur modification process; the amounts of these metals are significantly higher than in other slag types.
  • Sulfur as an element of extremely electronegative character reacts vigorously with metals. Copper reacts with sulfur at room temperature, and at higher temperatures sulfur combines with almost every element.
  • waste slag from copper smelting has the pH reaction of about 8.5 unlike blast-furnace slag from steel melting, which has the pH reaction of 10.5; this is very important in the process of sulfur modification, since it is easier to obtain the pH reaction of below 7 with the help of waste phosphogypsum, which affects positively both the modification and the qualities of polymeric construction material formed as a result of modification of sulfur with waste slag from copper smelting.
  • metals contained in waste slag from copper smelting such as phosphorus, copper and their sulfides, inhibit sulfur crystallization process and stabilize its polymeric form.
  • Polymeric construction material based on waste slag from copper smelting and waste sulfur related to in the invention is composed of 30% - 50% by weight of waste sulfur, 10% - 45% by weight of 0 - 5 mm granulation waste slag from copper smelting, which contains about 45% of silicates, about 12% of aluminium trioxide, about 11 % of iron trioxide, about 6% of magnesium oxide, about 15% of calcium oxide, about 0.2% of phosphorus pentaoxide, about 0.4% of copper, mixed with pH reaction regulator for waste slag from copper smelting, that is, with waste phosphogypsum in the amount of 15% - 30% by weight.
  • waste phosphogypsum changes the pH reaction of waste slag from copper smelting from about 8.5 to about 6.0, that is, to slightly acidic.
  • Liquid sulfur previously liquefied in tank no. 3 by indirect heating with heating oil is loaded to the mixer no.1 (Fig. 2).
  • amounts of waste slag from copper smelting with the slag pH reaction regulator, that is, waste phosphogypsum, weighted beforehand are batched to mixer no 1. In the mixer at the temperature of 125°C - 135°C and at constant mixing with the speed of ca.
  • Construction material in the above version intended to be poured into a mould or to be poured onto a specified surface differs in its percentage composition from polymeric construction material for the production of road surfacing compositions based on road asphalts and polymeric construction material intended for repairs and making of new road surfacing.
  • the amount of the mineral filler of up to 2 mm granulation is reduced to 10% by weight in it.
  • Appropriate amount of polymeric construction material based on waste slag from copper smelting and waste sulfur added to road surfacing compositions decreases the amount of used road asphalt in these surfaces by about 3% by weight, and thus, decreases the costs of road construction.
  • polymeric construction material increases the temperature of road surfaces softening and prevents their rutting, that lengthens the period of these roads using.
  • Polymeric construction material based on waste slag from copper smelting and waste sulfur possesses very good functional properties, that is, compression strength of about 40MPa - 50MPa, breaking strength of about 5MPa, which is significantly higher than the breaking strength of traditional concretes, bending strength of about 7MPa, low absorbability of about 1%, good frost resistance and proper roughness, that is significant in the road surfacing forming process. It is a polymeric construction material which is resistant to acids and which possesses excellent adhesion to substrate and mineral materials used in road construction.
  • Compounds contained in polymeric construction material such as copper oxides, aluminium oxides, iron(ll) and iron(lll) compounds are hydrogen sulfide emission inhibitor when mixed with asphalt if there was a mixed asphalt and polymeric construction material temperature rise to the temperature higher than 150 0 C, that improves work safety during the production of those road compositions.
  • Used waste slag from copper smelting composed of about 45% by weight of silicates, about 12% by weight of aluminium trioxide, about 11% by weight of iron trioxide, about 6% by weight of magnesium oxide, about 15% by weight of calcium oxide, about 0.5% by weight of phosphorus pentaoxide, about 0.4% by weight of copper, is of colour grey and of up to 5 mm granulation.
  • waste phosphogypsum is a product of industrial phosphoric acid production.
  • Waste sulfur is a waste product of natural gas desulfurization or crude oil desulfurization, which assumes brown colour after it is melted. Production method of polymeric construction material based on waste slag from copper smelting and waste sulfur according to the invention has been defined more closely in the example of embodiment.
  • Polymeric construction material of the composition in % by weight to be cast in a mould or poured onto surfaces.
  • Waste slag from copper smelting 25 % Waste phosphogypsum as slag pH reaction regulator 15 %
  • Weighted amounts of waste sulfur are delivered to the mixer no. 1 (Fig. 2).
  • Mixer no. 1 is heated indirectly with heating oil which is heated in electric furnace.
  • Mixer no. 1 has a rotating agitator of 16 revolutions per minute.
  • Weighted amounts of waste slag from copper smelting mixed beforehand with waste phosphogypsum as the pH reaction regulator are batched to the mixer no. 1 at the temperature of 125 0 C - 135°C. At the temperature of 125°C - 135 0 C in the molten sulfur zone the contact of waste slag from copper smelting mixed with waste phosphogypsum and of liquid sulfur occurs. Mixing of the ingredients lasts for about 20 minutes.
  • Mineral filler of up to 2 mm 10 % Mode of preparation is identical with that from Example III; the difference lies in the fact that from the intermediate mixer no. 2 polymeric construction material is directed to granulation.
  • Granulate is used to prepare road surfacing compositions with increased softening temperature of 100 0 C - 115°C according to the "Sphere and Ring" method.
  • Mode of preparation of road surfacing composition based on polymeric construction material granulate is as follows: Warmed mineral materials used for road surfacing forming, that is, diabase, basalt of the temperature not exceeding 150 0 C are batched in a paving plant to the mixer no. 1 (Fig. 3).
  • the mixture of asphalt and granulate forms bonding agent of the composition in % by weight:
  • Obtained road surfacing layer is of colour black and excellently improves its properties, on which an opinion has previously been given.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un liant polymère de construction et un liant polymère de construction. Le procédé de fabrication du liant polymère de construction comprend la délivrance de 30 à 60 % en poids de déchets de soufre qui sont portés à la température de 125 °C à 135 °C dans le tambour rotatif d'un mélangeur, puis, après leur fusion, l'ajout à ceux-ci de 10 à 40 % en poids de déchets de laitier qui contiennent du sélénium, de l'arsenic, du phosphore et leurs sulfures et oxydes métalliques et qui sont fragmentés en un granulat d'une taille allant jusqu'à 10 mm et soumis auparavant à une régulation du pH à environ 6,5 à l'aide de déchets de phosphogypse en une quantité de 15 à 30 % en poids, puis l'ajout de charges minérales en une quantité pouvant atteindre 30 % en poids; le mélange est ensuite mélangé pendant environ 10 minutes à une vitesse d'environ 16 à 20 tours par minute; le liant de construction formé est ensuite versé dans des moules ou versé sur une surface spécifiée. Le liant polymère de construction est composé de déchets de soufre en une quantité de 30 à 60 % en poids, de déchets de laitier en une quantité de 10 à 45 % en poids, de déchets de phosphogypse en une quantité de 15 à 30 % en poids, et de charges minérales en une quantité de 10 à 40 % en poids.
PCT/PL2009/000109 2009-01-14 2009-12-21 Procédé de fabrication d'un liant polymère de construction et liant polymère de construction WO2010082856A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EA201170892A EA018572B1 (ru) 2009-01-14 2009-12-21 Способ производства строительного полимерного вяжущего и строительное полимерное вяжущее

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
PLP-387038 2009-01-14
PL387038A PL213685B1 (pl) 2009-01-14 2009-01-14 Sposób wytwarzania polimerycznego spoiwa budowlanego na bazie żużla wielkopiecowego i siarki odpadowej
PL388298A PL213520B1 (pl) 2009-06-17 2009-06-17 Sposób wytwarzania polimerycznego materiału budowlanego na bazie żużla odpadowego z wytopu miedzi i siarki odpadowej
PLP-388298 2009-06-17

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WO2010082856A1 true WO2010082856A1 (fr) 2010-07-22

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WO (1) WO2010082856A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8512469B2 (en) * 2010-05-28 2013-08-20 Wlodzimierz Myslowski Polymeric construction material on the basis of flotation waste from copper ore flotation and waste sulfur
CN114450315A (zh) * 2019-09-27 2022-05-06 株式会社Adeka 硫改性聚丙烯腈的制造方法
WO2022139779A1 (fr) 2020-12-21 2022-06-30 Юрий Евгеньевич АНДРОСЮК Procédé et installation de production de nano-liant polymère à base de soufre

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4058500A (en) 1975-05-29 1977-11-15 Vroom Alan H Sulphur cements, process for making same and sulphur concretes made therefrom
US4348313A (en) 1979-10-16 1982-09-07 The United States Of America As Represented By The Secretary Of The Department Of Commerce Concrete formulation comprising polymeric reaction product of sulfur/cyclopentadiene oligomer/dicyclopentadiene
BE899598A (fr) * 1984-05-07 1984-08-31 Arklow S A Procede de neutralisation et de solidification de dechets.
JP2000053461A (ja) * 1998-08-06 2000-02-22 Nippon Mitsubishi Oil Corp 構造物の製造方法
EP1065185A1 (fr) * 1999-07-02 2001-01-03 Mikhail Pildysh Agrégat synthétique et procédé pour sa préparation

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4058500A (en) 1975-05-29 1977-11-15 Vroom Alan H Sulphur cements, process for making same and sulphur concretes made therefrom
US4348313A (en) 1979-10-16 1982-09-07 The United States Of America As Represented By The Secretary Of The Department Of Commerce Concrete formulation comprising polymeric reaction product of sulfur/cyclopentadiene oligomer/dicyclopentadiene
BE899598A (fr) * 1984-05-07 1984-08-31 Arklow S A Procede de neutralisation et de solidification de dechets.
JP2000053461A (ja) * 1998-08-06 2000-02-22 Nippon Mitsubishi Oil Corp 構造物の製造方法
EP1065185A1 (fr) * 1999-07-02 2001-01-03 Mikhail Pildysh Agrégat synthétique et procédé pour sa préparation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
AKUTSU K. ET AL: "Study on the use of recovered sulfur", CHEMICAL ABSTRACTS, vol. 88, no. 24, 12 June 1978 (1978-06-12), pages 367, XP000185407, ISSN: 0009-2258 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8512469B2 (en) * 2010-05-28 2013-08-20 Wlodzimierz Myslowski Polymeric construction material on the basis of flotation waste from copper ore flotation and waste sulfur
CN114450315A (zh) * 2019-09-27 2022-05-06 株式会社Adeka 硫改性聚丙烯腈的制造方法
CN114450315B (zh) * 2019-09-27 2023-05-23 株式会社Adeka 硫改性聚丙烯腈的制造方法
WO2022139779A1 (fr) 2020-12-21 2022-06-30 Юрий Евгеньевич АНДРОСЮК Procédé et installation de production de nano-liant polymère à base de soufre

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Publication number Publication date
EA201170892A1 (ru) 2011-12-30
EA018572B1 (ru) 2013-08-30

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