WO2022226863A1 - Procédé de préparation, à l'aide de résidus de sable bitumineux, de pigment composite et de charge pour revêtement - Google Patents

Procédé de préparation, à l'aide de résidus de sable bitumineux, de pigment composite et de charge pour revêtement Download PDF

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Publication number
WO2022226863A1
WO2022226863A1 PCT/CN2021/090847 CN2021090847W WO2022226863A1 WO 2022226863 A1 WO2022226863 A1 WO 2022226863A1 CN 2021090847 W CN2021090847 W CN 2021090847W WO 2022226863 A1 WO2022226863 A1 WO 2022226863A1
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WIPO (PCT)
Prior art keywords
oil sand
sand tailings
calcining
raw material
ultra
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PCT/CN2021/090847
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English (en)
Chinese (zh)
Inventor
任冬寅
尚志新
张梅
马洪才
曲铭海
王培玉
孔云
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德州学院
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Priority to CN202180013962.9A priority Critical patent/CN115443314B/zh
Priority to PCT/CN2021/090847 priority patent/WO2022226863A1/fr
Publication of WO2022226863A1 publication Critical patent/WO2022226863A1/fr

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    • 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
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints

Definitions

  • the invention belongs to the field of green resource utilization of industrial solid waste, and in particular relates to a method for preparing composite pigments and fillers for coatings by utilizing oil sand tailings.
  • carbon black is the most widely used colorant (pigment) in the coatings field and is often used to produce black or gray coatings.
  • pigment the most widely used colorant (pigment) in the coatings field and is often used to produce black or gray coatings.
  • the composition, density, particle size, hydrophilicity and other physical and chemical properties of carbon black are quite different from commonly used inorganic fillers (such as calcium carbonate, barium sulfate, calcined kaolin, talc, wollastonite, etc.) Delamination leads to floating and blooming of the paint, which in turn affects the storage stability of the paint.
  • Carbon black has a large specific surface area and high oil absorption value, and it is easy to absorb a large amount of solvents and additives, causing problems such as thickening, thickening and whitening of oil-based coatings after storage.
  • titanium dioxide-based white composite pigments and fillers are prepared by physical coating or chemical coating, due to the difference in properties of carbon black and inorganic fillers, it is difficult to obtain the corresponding composite pigments and fillers, and there is no black composite pigment yet. related reports on fillers.
  • Oil sand tailings are the black solids remaining after oil extraction from oil sands.
  • the main components are slightly different depending on the place of origin, but they are all dominated by natural minerals, such as calcium carbonate, quartz sand and clay minerals.
  • the surface of natural minerals in oil sand tailings is coated with a small amount of organic matter such as bitumen and heavy oil, which makes it difficult for them to be directly utilized and stored in large quantities.
  • every ton of oil extracted will produce 3-15 tons of oil sand tailings.
  • the accumulation of a large amount of tailings not only occupies a large amount of land and pollutes the environment, but also a waste of resources.
  • the present invention provides a method for preparing composite pigments and fillers for coatings by utilizing oil sand tailings.
  • the inventors of the present invention realized that the oil sand tailings themselves are natural minerals, and after undergoing high temperature, alkali treatment or organic solution extraction and other processes in the process of oil extraction, they are loose and porous, easy to pulverize, Physical and chemical properties are stable and so on.
  • the oil sand tailings are black and contain a small amount of heavy oil such as asphalt. If the particle surface of the oil sand tailings can be uniformly coated with a layer of asphalt organic matter, then the oil sand tailings will have the ability to produce composite pigments for coatings. filler potential.
  • the method of the invention can prepare composite pigments and fillers (that is, the composite pigments and fillers have the functions of pigments and fillers at the same time) according to the mineral properties of the oil sand tailings through a suitable production process, which not only solves the problems in the coating industry, but also realizes the
  • the green high-value utilization of oil sand tailings has good technical applicability and can comprehensively utilize various oil sand tailings.
  • a method for preparing composite pigments and fillers for coatings using oil sand tailings comprising some of the five steps of heat treatment, coarse crushing, magnetic separation, ultra-fine processing and surface modification step:
  • the heat treatment includes two steps of drying and calcination.
  • the drying is to use drying equipment to dry the oil sand tailings with a water content of more than 1% at a predetermined temperature, and to dry the water content to less than 1%.
  • calcining equipment is used to calcine the oil sand tailings twice under a predetermined atmosphere and temperature, so that the surface asphalt of the oil sand tailings can be uniformly wrapped and carbonized respectively.
  • the heat treatment can reasonably select the 0-2 stage process in drying and calcination according to the actual situation of the raw materials.
  • Coarse crushing use coarse crushing equipment to crush the heat-treated oil sand tailings to less than 0.2mm for magnetic separation.
  • Magnetic separation Part of the iron-rich material in the coarsely pulverized material is selected by a magnetic separator.
  • the magnetically selected iron-rich materials can be used as cement raw materials for the production of cement. When the iron content in the material after heat treatment is low, the magnetic separation step can be omitted.
  • Ultra-fine processing use ultra-fine processing equipment to mix the coarsely pulverized or magnetically separated materials and toners to evenly pulverize to a certain fineness, and the ultra-finely processed materials can be used as composite pigments and fillers for Water-based paint, paint or powder coating.
  • the production processes involved in the method of the present invention are all purely physical processes, and do not involve processes such as strong acid and alkali, high pressure, etc.
  • the production process is safe, green, and environmentally friendly, and no three wastes are discharged.
  • Sand adaptability is high.
  • the composite pigment and filler produced by the method of the invention has uniform dispersion, good affinity with resin and excellent coloring effect, and can be widely used in the fields of paint, water paint and powder coating.
  • the technical scheme of the invention not only solves the problems in the coating industry, but also truly realizes the green and high value-added utilization of oil sand tailings.
  • FIG. 1 is a flow chart of a method for preparing composite pigments and fillers for coatings by utilizing oil sand tailings according to an embodiment of the present invention.
  • an embodiment of the present invention provides a method for preparing a composite pigment and filler for coatings by utilizing oil sand tailings raw materials, the method comprising:
  • heat treatment of the oil sand tailings raw material wherein the heat treatment includes drying the oil sand tailings raw material and calcining the oil sand tailings raw material, so that the particles of the oil sand tailings are coated on the surface of the oil sand tailings raw material by bitumen and carbonized;
  • the coarsely pulverized oil sand tailings are ultra-finely processed, so that the ultra-finely processed oil sand tailings are used as the composite pigment and filler.
  • the step of drying the oil sand tailings raw material is performed by a drying device so that the water content of the oil sand tailings raw material is lower than 1%
  • the drying device includes a centrifugal dehydrator, a filter press, and a flash dryer , a spray dryer, a fluidized bed dryer, a rotary kiln dryer and a drum dryer, or any combination thereof
  • the temperature of the drying step is in the range of 100-200°C, preferably 150°C.
  • the calcining of the oil sand tailings raw material is performed by a calcining device under a calcining atmosphere, and the calcining device includes any one of a tunnel kiln, an internal heating rotary kiln, an external heating rotary kiln and a pusher kiln or any of them.
  • the calcining atmosphere includes an inert gas protective atmosphere, a reducing atmosphere or a weakly oxidizing atmosphere.
  • the calcining includes a first calcining and a second calcining of the oil sand tailings feedstock, the first calcining at a temperature ranging from 200-350°C (eg, 250°C or 300°C) and calcining
  • the time range for calcination is 10-480 minutes (eg 200 minutes or 300 minutes); the temperature range for the second calcination is 350-1300°C (eg 800°C or 1000°C) and the time range for calcination is 10-480 minutes (eg 300 minutes or 400 minutes).
  • the step of coarsely pulverizing the heat-treated oil sand tailings is performed by a coarse crushing device including a hammer crusher, a cone crusher, an impact crusher, a roller press, a vertical mill and any of the Raymond mills or any combination of them.
  • the step of ultra-finely processing the mixture of coarsely pulverized oil sand tailings and toner is performed by ultra-fine processing equipment including ring roll mills, mechanical mills, ball mills, jet mills, Any one or any combination of steam mill, hot air jet mill, agitated mill and sand mill;
  • the toners include red red, strontium chrome yellow, zinc chrome yellow, barium chrome yellow, calcium chrome yellow, Phosphate, phosphomolybdate, aluminum dihydrogen tripolyphosphate, zinc molybdate, zinc borate, mica iron oxide, titanium dioxide, zinc oxide, graphite, ultramarine blue, phthalocyanine blue, barium sulfate, iron red, barium sulfate Any one or any combination thereof;
  • the dosage of the toner is 0-90% of the powder mass of the coarsely pulverized oil sand tailings; the toner can play the role of fine-tuning and improving paint resistance.
  • the method further includes performing magnetic separation on the coarsely pulverized oil sand tailings, wherein the magnetically selected iron-rich material is used as a cement raw material, and after the magnetic separation The oil sand tailings are used for subsequent ultrafine processing.
  • the step of magnetically separating the coarsely pulverized oil sand tailings is performed by a dry magnetic separator, and the range of the magnetic field strength of the dry magnetic separator is 0.02-2.0T.
  • the method further includes surface modification of the ultra-finely processed oil sand tailings to obtain modified composite pigments and fillers.
  • the step of surface modification is performed by a modification device or in a cavity of an ultrafine machining device.
  • the surface modification can be selected according to the type of modifier and the type of ultra-fine processing equipment to be completed in the grinding chamber of the ultra-fine processing equipment, or completed by the modification equipment after the pulverization is completed.
  • the modification equipment includes any one or any combination of a three-roll modifier, a high-speed mixer and a tower modifier
  • the modifier used in the surface modification is a silane coupling agent, Aluminate coupling agents, titanate coupling agents, rare earth coupling agents, fatty acids and their salts, polyalcohols, higher alcohols, ammonium polyacrylate, sodium polyacrylate, sodium hexametaphosphate and sodium tripolyphosphate Any one or any combination of them;
  • the amount of the modifier is 0.01-25% (for example, 10% or 15%) of the powder mass of the ultra-finely processed oil sand tailings;
  • the surface modifier is The typical temperature range is 50-300°C (eg 200°C).
  • the coating is powder coating, water-based coating or paint.
  • the raw material particle size of Indonesian oil sand tailings is greater than 0.2mm and the water content is greater than 1%. Its main chemical composition is shown in Table 1.
  • the adopted processing techniques are drying, calcination, coarse pulverization, magnetic separation, ultra-fine processing and surface modification.
  • the specific preparation process parameters are as follows: First, the raw material of Indonesian oil sand tailings is dried with hot air through a drum dryer. The temperature of the air inlet of the drum dryer is 190 °C and the outlet temperature is 80 °C. The dried oil sand tailings The water content is 0.3%. Then, the dried oil sand tailings are calcined in two stages under the protection of nitrogen by using a tunnel kiln.
  • the time is 120min; then use Raymond mill to grind the oil sand tailings to a particle size of less than 0.2mm, and then use a dry magnetic separator to magnetically separate the dried oil sand tailings under a magnetic field strength of 1.5T.
  • the chemical composition of the final material is shown in Table 1. After the material after magnetic separation is mixed with 1% strontium chrome yellow uniformly, ultrafine processing is carried out with a fluidized bed jet mill at a pressure of 0.8Mpa and a classifier speed of 1700rpm to obtain a composite pigment and filler A; finally, the ultrafine processing is carried out.
  • the particle size of Canadian oil sand tailings is greater than 0.2 mm and the water content is greater than 1%.
  • the main chemical composition is shown in Table 3.
  • the processing techniques adopted in this embodiment are drying, calcination, coarse crushing, magnetic separation, ultra-fine processing and surface modification.
  • the specific preparation process parameters are as follows: First, use a fluidized bed dryer to dry the Canadian oil sand tailings raw material with hot air. The air inlet temperature of the dryer is 183°C and the outlet temperature is 75°C. The water content of the tailings is 0.3%. Then, using an internal combustion rotary kiln, the dried oil sand tailings are calcined in two stages in a reducing atmosphere.
  • the temperature at the kiln head is 200 °C, and the temperature at the kiln tail is 1000 °C.
  • the calcination time of the first stage is 5min, and the second stage calcination The time is 20min; then the oil sand tailings are ground with a vertical mill to a particle size of less than 0.2mm, and then the dried oil sand tailings are subjected to magnetic separation with a dry magnetic separator under a magnetic field strength of 1.5T.
  • the chemical composition of the material is shown in Table 3.
  • the filler B is subjected to ultra-fine processing with a steam kinetic energy mill under the conditions of a steam pressure of 1.2Mpa and a temperature of 180°C in the grinding chamber. At 1500 rpm, respectively, composite pigments and fillers B were prepared (the particle size distribution is shown in Table 4). Finally, for a part of the ultra-finely processed material, 0.5% silane coupling agent (KH560) and 0.5% silane coupling agent (KH540) are sprayed directly into steam through the atomizing nozzle In the mill, in-situ modification was carried out to obtain the modified composite pigment and filler B, and its particle size distribution is shown in Table 4.
  • KH560 0.5% silane coupling agent
  • KH540 0.5% silane coupling agent
  • the surface of the composite pigment and filler prepared by the method of the present invention is tightly coated with a layer of carbon-based organic matter, which can play the dual role of pigment and filler, and can significantly improve the compatibility with organic resins. Affinity and Dispersion.
  • the method of the present invention can not only reduce the production cost of the coating, but also can significantly improve the storage, corrosion resistance, weather resistance and other properties of the coating.
  • the method of the invention has significant environmental protection significance and economic benefits, and has broad market prospects.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)

Abstract

Les modes de réalisation de la présente invention concernent un procédé de préparation, à l'aide d'une matière première de résidu de sable bitumineux, d'un pigment composite et d'une charge pour un revêtement. Le procédé comprend les étapes suivantes : soumettre une matière première de résidu de sable bitumineux à un traitement thermique, le traitement thermique comprenant le séchage du matériau brut de résidu de sable bitumineux et la calcination du matériau brut de résidu de sable bitumineux, de telle sorte que, sur la surface de la matière première de résidu de sable bitumineux, de l'asphalte enveloppe des particules d'un résidu de sable bitumineux et est carbonisé ; réaliser un broyage grossier sur le résidu de sable bitumineux traité thermiquement ; et réaliser un traitement superfin sur un mélange du résidu de sable bitumineux broyé grossièrement et d'un toner, de telle sorte que le résidu de sable bitumineux traité superfin est utilisé en tant que pigment composite et charge.
PCT/CN2021/090847 2021-04-29 2021-04-29 Procédé de préparation, à l'aide de résidus de sable bitumineux, de pigment composite et de charge pour revêtement WO2022226863A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202180013962.9A CN115443314B (zh) 2021-04-29 2021-04-29 利用油砂尾砂制备涂料用复合颜填料的方法
PCT/CN2021/090847 WO2022226863A1 (fr) 2021-04-29 2021-04-29 Procédé de préparation, à l'aide de résidus de sable bitumineux, de pigment composite et de charge pour revêtement

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PCT/CN2021/090847 WO2022226863A1 (fr) 2021-04-29 2021-04-29 Procédé de préparation, à l'aide de résidus de sable bitumineux, de pigment composite et de charge pour revêtement

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101020765A (zh) * 2007-03-16 2007-08-22 中国地质大学（武汉） 一种利用油页岩固体废弃物制备天然橡胶填料的方法
US20090020735A1 (en) * 2007-07-16 2009-01-22 Conocophillips Company Flame retardant composition employing oil sand tailings
CN102504368A (zh) * 2011-11-10 2012-06-20 吉林大学 用油页岩灰渣改性橡胶及其方法
CA2829482A1 (fr) * 2013-10-09 2015-04-09 Imperial Oil Resources Limited Traitement des residus de sables bitumineux au moyen d'un liant et d'un absorbant
CN106867065A (zh) * 2017-03-08 2017-06-20 吉林大学 一种利用改性油页岩半焦制备橡胶填料的方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4590056A (en) * 1985-03-01 1986-05-20 Ohio University Method of making carbon black having low ash content from carbonaceous materials
CA2794587A1 (fr) * 2012-11-04 2014-05-04 Guoxing Gu Composition et procede pour produire des materiaux de construction en ceramique au moyen de residus des sables bitumineux de l'alberta
CA2909029C (fr) * 2015-10-14 2018-02-27 Imperial Oil Resources Limited Une methode de controle d'un traitement de residus de sables bitumineux
CN112430400A (zh) * 2020-11-23 2021-03-02 山西奇色环保科技股份有限公司 一种以煤气化渣为原料制备橡胶填料的方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101020765A (zh) * 2007-03-16 2007-08-22 中国地质大学（武汉） 一种利用油页岩固体废弃物制备天然橡胶填料的方法
US20090020735A1 (en) * 2007-07-16 2009-01-22 Conocophillips Company Flame retardant composition employing oil sand tailings
CN102504368A (zh) * 2011-11-10 2012-06-20 吉林大学 用油页岩灰渣改性橡胶及其方法
CA2829482A1 (fr) * 2013-10-09 2015-04-09 Imperial Oil Resources Limited Traitement des residus de sables bitumineux au moyen d'un liant et d'un absorbant
CN106867065A (zh) * 2017-03-08 2017-06-20 吉林大学 一种利用改性油页岩半焦制备橡胶填料的方法

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CN115443314B (zh) 2024-06-28

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