WO2017176164A1 - Installation destinée à la production combinée de sels de phosphate et de sulfate de potassium - Google Patents

Installation destinée à la production combinée de sels de phosphate et de sulfate de potassium Download PDF

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Publication number
WO2017176164A1
WO2017176164A1 PCT/RU2017/000191 RU2017000191W WO2017176164A1 WO 2017176164 A1 WO2017176164 A1 WO 2017176164A1 RU 2017000191 W RU2017000191 W RU 2017000191W WO 2017176164 A1 WO2017176164 A1 WO 2017176164A1
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WO
WIPO (PCT)
Prior art keywords
hydrochloric acid
phosphate
unit
leaching
producing
Prior art date
Application number
PCT/RU2017/000191
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English (en)
Russian (ru)
Inventor
Александр Владимирович ТУГОЛУКОВ
Дмитрий Владимирович ВАЛЫШЕВ
Олег Львович ЕЛИН
Original Assignee
Акционерное общество "Минерально-химическая компания "ЕвроХим"
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Filing date
Publication date
Application filed by Акционерное общество "Минерально-химическая компания "ЕвроХим" filed Critical Акционерное общество "Минерально-химическая компания "ЕвроХим"
Priority to CN201780009438.8A priority Critical patent/CN108602673B/zh
Publication of WO2017176164A1 publication Critical patent/WO2017176164A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
    • C01D1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D1/00—Fertilisers containing potassium

Definitions

  • the present invention relates to the field of chemical technology, in particular to a plant for the combined production of phosphate salts, for example dicalcium phosphate and / or tricalcium phosphate, and potassium sulfate.
  • phosphate salts for example dicalcium phosphate and / or tricalcium phosphate, and potassium sulfate.
  • Phosphate salts and potassium sulfate are widely demanded products in the modern market of mineral fertilizers.
  • the former are used for the production of various phosphate fertilizers, and potassium sulfate itself is a potash non-chlorine fertilizer. Therefore, the development of effective and highly cost-effective equipment for their production seems to be an urgent topic of modern chemical technology.
  • Closest to the claimed invention is a plant for the production of phosphates containing a hydrochloric acid leaching unit, an apparatus for preparing a solution for neutralization, a unit for neutralizing the liquid phase and precipitating phosphates, a filter for separating phosphates, apparatus for washing and drying phosphates (see Jafarov IF Production of precipitate. Moscow, Food Industry Publishing House, 1975, S. 5-57).
  • the known installation is designed to produce dicalcium phosphate, used as feed phosphate, from bone meal by the method of hydrochloric acid leaching.
  • the hydrochloric acid leaching unit is made in the form of reactors (maceration devices), sequentially combined into cascades (groups) or batteries using a satellite stream of hydrochloric acid and hydrochloric acid leaching products, and the unit for neutralizing the liquid phase and precipitating phosphates is made in the form of several reactors (precipitators) subsequently combined with each other to ensure the continuity of the process and equipped with a tank for collecting and averaging the composition of the phosphate pulp, an apparatus for preparing a solution for neutralization is an apparatus for the preparation of milk of lime, which makes it possible to process high-quality phosphate raw materials (bone meal) well without using additional devices for separating solid and liquid phases at the leaching stage (semi-solid organic waste is removed from the reactors by vacuum suction).
  • the objective of the invention was to create a plant for the decomposition of phosphate raw materials, which includes a unit for producing hydrochloric acid necessary for the process, and which allows to simultaneously obtain phosphate salts and potassium sulfate.
  • a unit for producing potassium sulfate and hydrochloric acid from potassium chloride and sulfuric acid which contains a furnace for producing potassium sulfate, an apparatus for producing anhydrous hydrochloric acid and a unit for preparing hydrochloric acid for leaching, and
  • a unit for the production of phosphates from phosphate feedstock which contains a hydrochloric acid leach unit, a neutralization solution preparation apparatus, a neutralization unit for the liquid phase and a precipitation of phosphates connected to it by a pipeline, a filter for phosphorus separation connected in series behind it and connected by transport lines - tov, phosphate washing unit and apparatus for drying phosphates, moreover, between the hydrochloric acid leaching unit and the unit for neutralizing the liquid phase and the precipitation of phosphates there is a device for separating solid and liquid phases after leaching, which is connected to them by pipelines, and the furnace for producing potassium sulfate is connected via a gas outlet to the apparatus for obtaining hydrochloric acid, and the latter is connected by pipelines through the hydrochloric acid preparation unit for leaching to the hydrochloric acid leaching unit.
  • the main technical result of the present invention is the possibility of producing phosphates from phosphate raw materials of different quality by optimizing production conditions and conditions that are optimal for this raw material, while at the same time obtaining valuable mineral fertilizer — potassium sulfate — at the plant.
  • the installation according to the invention can significantly reduce the cost of transporting the necessary raw materials and optimize energy costs.
  • the apparatus according to the invention is intended for the production of the following phosphates: dicalcium phosphate, tricalcium phosphate, mixtures thereof, as well as mixtures of dicalcium phosphate, tricalcium phosphate with minerals containing phosphates, for example fluoroappatite.
  • Phosphate ore (phosphorite, apatite) with a phosphorus pentoxide content of more than 20% is used for the production of phosphates.
  • the inventive installation allows you to get a marketable product (phosphate) - dry phosphate salt when used for leaching (decomposition of phosphate ore) of hydrochloric acid produced by the installation.
  • the production of hydrochloric acid using sulfuric acid leads to the production of a valuable chlorine-free potassium fertilizer - potassium sulfate.
  • the amount of saline acid the slots required for leaching are directly proportional to the production volume of potassium sulfate, and its concentration can reach 33% by weight, which allows you to choose the optimal leaching regimes depending on the type and quality of phosphate raw materials, in particular, choose the optimal concentration and acid consumption rates for most types of phosphate feedstocks.
  • the presence of an apparatus for preparing a solution for neutralization and a unit for neutralizing the liquid phase and the precipitation of phosphates in the unit for producing phosphates from phosphate raw materials makes it possible to obtain the required qualitative and quantitative composition of phosphate salts in the phosphate product, as well as the introduction of an apparatus for the separation of solid and liquid phases after leaching.
  • the apparatus for separating solid and liquid phases after leaching, a filter for the separation of phosphates, a phosphate washing unit ensure high purity of the product, and the drying apparatus completes the production of phosphates in the marketable form. Due to the indicated combination of features, the proposed installation provides for the production of commercial phosphates from raw materials of different qualitative and quantitative composition with a continuous process and its high productivity.
  • the invention for the first time allows you to create an installation for the production of marketable phosphates from phosphate raw materials of various quality by optimizing modes and operating conditions of with respect to the raw material or type of the final product when using the leaching of phosphate raw materials of abhase hydrochloric acid obtained in the installation itself, and to obtain a new product for such plants and a valuable product - potassium sulfate.
  • hydrochloric acid in the claimed installation sulfuric acid and potassium chloride are used, which are affordable and cheap raw materials, which allows the implementation of this installation on an industrial scale.
  • FIG. 1 schematically illustrates the design and operation of the proposed installation.
  • the installation for the production of phosphate salts and potassium sulfate contains a phosphate B production unit, which includes a hydrochloric acid leach unit 4 with inputs for phosphate feed and hydrochloric acid, an apparatus for separating solid and liquid phases after leaching 5, a unit for neutralizing the liquid phase and sedimentation - phosphate 6, an apparatus for preparing a solution for neutralization 7, a filter for separating phosphates 8, a washing unit for phosphates 9, an apparatus for drying phosphates 10, as well as a unit for producing potassium sulfate and hydrochloric acid A, which contains for producing potassium sulfate 1, an apparatus for producing abdominal hydrochloric acid 2 and a unit for preparing hydrochloric acid for leaching 3.
  • a phosphate B production unit which includes a hydrochloric acid leach unit 4 with inputs for phosphate feed and hydrochloric acid, an apparatus for separating solid and liquid phases
  • the output of the hydrochloric acid leaching unit 4 is connected by a pipeline to the input of the apparatus for separating solid and liquid phases after leaching 5, the output apparatus 5 in the solid phase is the output of the plant for solid waste, and its output in the liquid phase is connected by a pipe to the inlet of the liquid phase of leaching the neutralization unit of the liquid phase and the precipitation of phosphates 6, the inlet for solution eytralizatsii block neutralization liquid phase and co-precipitation of phosphate 6 it is single by a pipeline with the outlet of the apparatus for preparing the solution for neutralization 7, the output of the unit for neutralizing the liquid phase and the precipitation of phosphates 6 is connected by a pipeline to the inlet of the filter for the separation of phosphates 8, the outlet of which is filtered by the filtrate and the phosphate outlet of by means of a vehicle through a phosphate washing unit 9 with a phosphate drying apparatus 10, the output of the apparatus 10 is the output of the unit's product, the furnace for producing potassium
  • hydrochloric acid is diluted to a predetermined concentration and hydrochloric acid is accumulated to a predetermined concentration in an amount necessary for the operation of the unit.
  • the neutralizing agent is mixed with water and a solution is obtained to neutralize the given concentration (milk of lime, suspension of calcium carbonate, etc.).
  • Phosphate raw materials of the required degree of dispersion for example, in the form of phosphorite flour, are supplied in the required amount to the hydrochloric acid leaching unit 4, at the same time hydrochloric acid of the required concentration and in the specified quantity from node 3 is fed there.
  • node 4 phosphates transfer to the solution under the influence of hydrochloric acid and the formation at the outlet of the pulp, containing mainly monocalcium phosphate, soluble metal chlorides and solid impurities.
  • the pulp is separated into a solid phase, which is removed from the unit as solid waste, and a liquid phase in the form of an acidic solution containing predominantly monocalcium phosphate and soluble impurities.
  • the acidic solution of phosphates and soluble impurities which arrived at the site of neutralization and precipitation of phosphates 6, is mixed with the solution for neutralization, received in the required amount from the device for preparing the solution for neutralization 7, with increasing the pH of the mixture to the required values, monocalcium phosphate is converted to dicalcium phosphate (and when choosing the appropriate regimen in tricalcium phosphate or in a mixture of phosphates), which precipitates.
  • the phosphate pulp obtained in block 6 enters the filter to separate phosphates 8.
  • the filtrate from filter 8 is mainly collected in the form of solutions of calcium, magnesium chloride and other impurities as liquid waste, and a solid precipitate of dicalcium phosphate (or corresponding other phosphate) is sent to the phosphate washing unit 9, where it is washed with water and re-filtered or separated in phase (the contaminated washing liquid is drained as liquid waste), and then it is fed to the apparatus for drying phosphate 10, from the output of which receive the finished product - phosphate.
  • the gases emitted in the blocks of hydrochloric acid leaching 4 and neutralization and sedimentation 6 are absorbed and purified in the corresponding apparatuses (not shown in the figure).
  • the concentration of hydrochloric acid that is optimal for the feedstock is prepared, which, in the required amount, proportional to the amount and quality of the feed, is sent to leaching unit 4, at the same time in the apparatus for preparing the solution for neutralization 7, the preparation of the neutralization solution of the required concentration and quantity is carried out, therefore optimal conditions and modes of phosphate production.
  • Solid waste obtained from the apparatus for separating solid and liquid phases after leaching 5 is disposed of.
  • Liquid wastes from the filter for the separation of phosphates 8 and from the washing unit 9 are discharged into the sea, and if this is not possible, they are processed into solid waste or commercial products by known methods, for example, evaporation.
  • Potassium sulfate obtained in furnace 8 is sold as a valuable fertilizer separately or as part of mixed or complex fertilizers.
  • Blocks, devices and installation units are implemented in a known manner.
  • So nodes hydrochloric acid leaching 4 and the neutralization of the liquid phase and the precipitation of phosphates 6 can be implemented in the form of one or more successively installed modified reactors (hereinafter, the reactor is a container with a stirrer with nozzles for introducing the liquid phase and withdrawing the pulp, a nozzle or manhole (tray and conveyor) for feeding dispersed phosphate raw materials or a neutralizing solution), the reactors can be combined into cascades or batteries, including by the principle of a spiral flow, with the supply of raw materials, or, respectively, a neutralizing solution to the first or several reactors of the cascade (battery) of unit 4 or 6.
  • Nodes 4, 6 can be implemented on the basis of multi-section reactors (extractors).
  • a prerequisite for continuous operation of the installation is the presence of a storage reactor in units 4, 6 — a tank with a stirrer or a storage tank without a stirrer, in which the composition and leaching of the leaching pulp or phosphate pulp are collected and averaged before separation, respectively, in apparatus 5 or on the filter 8.
  • the nodes 4, 6 may contain devices for distributing the phosphate feed or neutralization solution, respectively, to the reactors, which, for example, can be made in the form of a tank (reactor), which It has one input and several outputs connected by pipelines to reactors, and instrumentation and control equipment.
  • the apparatus for preparing the solution for neutralization 7 can be made in the form of a mixer (reactor with a stirrer) into which the set values of the solid neutralizing agent and water are dosed.
  • the node for the preparation of hydrochloric acid for leaching 3 can be implemented in the form of several storage tanks, tanks with a mixer (reactor), equipped with pumping, control, measuring and regulating equipment, combined by pipelines.
  • a mixer reactor
  • the apparatus for separating solid and liquid phases after leaching 5 can be made in the form of traditional separation devices (separators, filtering apparatuses), for example, in the form of a filter press.
  • the filter for the separation of phosphates 8 is also implemented in the traditional way in the form of filtering apparatuses of various types, for example filter presses, including those including a washing unit (carousel, belt filters). So, when using a belt filter 8 as a filter, phosphate washing is carried out by supplying water to a part of the belt filter. A drum vacuum filter or the like can be used to filter and rinse the phosphates.
  • the phosphate washing unit 9 and the phosphate drying apparatus 10 are also implemented in a known manner. So, as a separate washing unit, a container with a stirrer and settling can be used. Fluid bed dryers, drum, tunnel dryers and other structures for washing and drying traditionally used in the production of precipitate can also be used.
  • a muffle furnace heated by a gas torch and other types of furnaces can be used.
  • the apparatus for producing abdominal hydrochloric acid 2 can be implemented in the form of gas coolers connected in series with each other, for example, an adiabatic type, a series of absorbers, for example, in the form of an absorption column, collector storage of abdominal hydrochloric acid.
  • the plant uses traditional control and measuring and pumping equipment, and conveyors, pneumatic conveying and other equipment can be used to supply solid raw materials, remove products and waste.
  • the proposed installation can be implemented and used in industry.
  • Dry potassium chloride in the amount of 51 kg / h was loaded into the furnace with heated arch 1 of the hydrochloric acid production unit A, and dosing of sulfuric acid with a concentration of 98% in the amount of 35 kg / h was carried out in the reaction zone.
  • the process was carried out at a temperature of 400 ° C, with the formation of potassium sulfate in the amount of 62 kg / h, which is a non-chlorine potash fertilizer.
  • the released hydrogen chloride in the form of a gas was sent for absorption by water, where 78 kg / h of 31% hydrochloric acid was formed in three successive absorption columns.
  • hydrochloric acid in an amount of 200 kg / h was sent to the block for the production of phosphates from phosphate raw materials B.
  • 44 kg / h of phosphate flour was sent to the first reactor from the cascade of ore decomposition reactors.
  • 12% hydrochloric acid was supplied there in an amount of 200 kg / h. The process was carried out at a temperature of 60 ° C and atmospheric pressure.
  • the pulp from the reactor containing 4.1% phosphates in terms of phosphorus pentoxide was sent to the filtration, where the solid phosphate salt was separated and in the amount of 26 kg / h on a dry product in the form of a wet cake was sent for washing with water until the content of chlorine ions was not more than 0, 1%, and then dried to a moisture content of 5%.
  • a solution of 18% calcium chloride separated in the filtration process was sent for disposal.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Fertilizers (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Treating Waste Gases (AREA)

Abstract

L'invention concerne le domaine de la technologie chimique et notamment une installation pour la production combinée de sels de phosphate et de sulfate de potassium, par exemple, de phosphate dicalcique et/ou de phosphate tricalcique et de sulfate de potassium comprend une unité de production de sulfate de potassium et d'acide chlorhydrique à partir de chlorure de potassium et d'acide sulfurique qui comprend un four pour la production de sulfate de potassium, un appareil pour produire de l'acide chlorhydrique de gaz d'échappement et une unité de préparation de l'acide chlorhydrique à la lixiviation, de même qu'une unité de production de phosphates à partir d'une matière première à base de phosphates qui comprend une unité de lixiviation à l'acide chlorhydrique, un appareil de préparation d'une solution de neutralisation puis, relié à ce dernier par une conduite, une unité de neutralisation de phase liquide et de sédimentation de phosphates, une unité de rinçage de phosphates et un appareil de séchage de phosphates, la zone entre l'unité de lixiviation à l'acide chlorhydrique et l'unité de neutralisation de phase liquide et de sédimentation de phosphates comprend un appareil de séparation des phases solide et liquide après lixiviation, qui y est relié par des conduites, et le four pour la production de sulfate de potassium est relié par sa sortie des gaz, au moyen de tuyaux, à l'appareil pour produire de l'acide chlorhydrique de gaz d'échappement, ce dernier étant relié par des tuyaux via l'unité de production d'acide chlorhydrique pour la lixiviation à l'unité de lixiviation à l'acide chlorhydrique.
PCT/RU2017/000191 2016-04-04 2017-03-31 Installation destinée à la production combinée de sels de phosphate et de sulfate de potassium WO2017176164A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201780009438.8A CN108602673B (zh) 2016-04-04 2017-03-31 用于磷酸盐和硫酸钾的联合生产的装置

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RU2016112592 2016-04-04
RU2016112592A RU2616061C1 (ru) 2016-04-04 2016-04-04 Установка для комбинированного получения фосфатных солей и сульфата калия

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CN111232940A (zh) * 2020-03-12 2020-06-05 连云港树人科创食品添加剂有限公司 一种磷酸三钙联产氯化钾的制备方法

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CN111232940A (zh) * 2020-03-12 2020-06-05 连云港树人科创食品添加剂有限公司 一种磷酸三钙联产氯化钾的制备方法

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CN108602673B (zh) 2022-12-09
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RU2616061C1 (ru) 2017-04-12

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