WO2012146111A1 - Procédé et système pour la préparation de carbonate de calcium précipité - Google Patents

Procédé et système pour la préparation de carbonate de calcium précipité Download PDF

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Publication number
WO2012146111A1
WO2012146111A1 PCT/CN2012/073086 CN2012073086W WO2012146111A1 WO 2012146111 A1 WO2012146111 A1 WO 2012146111A1 CN 2012073086 W CN2012073086 W CN 2012073086W WO 2012146111 A1 WO2012146111 A1 WO 2012146111A1
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WO
WIPO (PCT)
Prior art keywords
carbon dioxide
stream
suspension
carbon
distributor
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.)
Ceased
Application number
PCT/CN2012/073086
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English (en)
Chinese (zh)
Inventor
修国华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Linde GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to BR112013027163A priority Critical patent/BR112013027163A2/pt
Publication of WO2012146111A1 publication Critical patent/WO2012146111A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C01F11/18—Carbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

Definitions

  • the present invention is directed to environmental issues arising from the manufacturing process of conventional precipitated carbonium.
  • a method of preparing a precipitated carbonium t ⁇ is carried out which transfers a carbon dioxide gas stream to a 7j suspension of a hydroxide face to achieve the purpose of reacting with a hydroxide face and stirring the suspension.
  • high carbon dioxide carbonation efficiency is obtained in the preparation of high-purity carbonic acid noodles by this method.
  • Calcium carbonate is a carbonate that has been found in many industrial products and everyday necessities, for example as an additive or modifier in paper, dyes, inks, adhesives and pharmaceuticals. In plastics, the carbonic acid surface is primarily used as a filler to replace relatively expensive polymers.
  • a typical process for preparing precipitated carbonium « begins with a calcination process in which a mixture of calcined limestone and coke/anthracite is produced to produce calcium oxide.
  • Low quality carbon dioxide is co-generated and stored during the calcination process, which is typically used for subsequent precipitation of the carbonic acid surface after simple purification.
  • the natural gas replaces the coke/anthracite to be burned to carry out the precipitation process.
  • the obtained oxidation surface (raw stone ash) is then aged with water to prepare a hydroxide surface liquid.
  • the impurities in the resulting liquid such as unburned or overburned lime, are mainly removed by passing the liquid through the wire mesh.
  • the hydroxide surface suspended in water reacts with carbon dioxide.
  • the carbonization process is carried out by adding carbon dioxide gas to the aqueous suspension of the hydroxide surface, during which the carbonization temperature and the carbon dioxide concentration are maintained within a suitable range to form the desired calcium carbonate particles in the aqueous phase.
  • the obtained calcium carbonate liquid again passes through the wire mesh to remove any residual impurities.
  • a centrifugal device separates water from the precipitated product to form a carbon ⁇ « ⁇ ⁇ body.
  • the carbon ⁇ « block is then dried by hot air and pulverized to obtain the desired product.
  • the production method of a new precipitated carbonium « described in the present application avoids many of the defects inherent in the conventional precipitation of carbonium «the preparation process.
  • a flow chart of this new method is shown in Figure 1.
  • the system for preparing a precipitated carbonated surface comprises a vessel containing a suspension of aqueous hydroxide surface and two gas distributors providing carbon dioxide to the vessel.
  • the production of precipitated carbonated surfaces involves heterogeneous reactions in the gas, liquid and solid phases and their interfaces, such as the absorption of carbon dioxide gas, the dissolution of Ca(OH) 2 solids, the nucleation and growth of CaCO 3 powder, and the carbon Precipitation of CaC0 3 at all stages of the ⁇ t3 ⁇ 4 process.
  • reverse mixing is applied as the primary method in the container.
  • the specific surface area of the bubbling carbon dioxide increases because this is critical for the reaction between the gas phase and the liquid phase.
  • the preparation of precipitated carbonium « disclosed in the present invention provides for the supply of two streams of carbon dioxide to the aqueous suspension of calcium hydroxide for different purposes.
  • the first stream of gaseous carbon dioxide is intended to react with the calcium hydroxide, and as shown in Figure 2, a second stream of carbon dioxide is injected into the vessel with the primary purpose of agitating the aqueous suspension of the hydroxide surface.
  • the turbulent flow of carbon dioxide is introduced into the suspension from a microporous hose or a set of microporous hoses, and the second gas stream is from a primary orifice distributor.
  • the microporous hose can be self-sealing for ease of maintenance.
  • the resulting carbonic acid earning night is subsequently processed to obtain the desired sodium carbonate product, including separating the water from the carbonium, drying, cooling and crushing the carbonium.
  • the resulting carbonated liquid is supplied directly to the application without the need to completely remove water, such as when it is directly mixed with the paper.
  • the weight ratio of the hydroxide surface to the water is from 1:1 to 1:30, and the initial carbonation temperature of the 7j suspension ranges from 20 ° C to 60 ° C.
  • a method of preparing precipitated calcium carbonate includes the steps of:
  • a system for producing precipitated calcium carbonate includes a vessel containing a suspension of aqueous hydroxide surface, providing carbon dioxide to the first distributor of the vessel and providing carbon dioxide to the vessel. Second distributor.
  • the first distributor is a self-sealing microporous hose and the second distributor is an injection distributor.
  • the system further includes a device for separating carbon ⁇ from water, a drying unit for removing water from the calcium carbonate, a cooling unit for cooling the separated calcium carbonate, and a preparation for precipitating carbon Spoon crushing unit.
  • Figure 1 is a schematic illustration of the production process for precipitating calcium carbonate in accordance with the process of the present invention.
  • Figure 2 is a schematic of a heterogeneous reaction system.
  • Figure 3 is a schematic diagram of a carbon dioxide distribution system of the present invention, wherein 10, pH probe; 20, temperature 3 ⁇ 41; 30, C0 2 micro-L distributor; 40, C0 2 injection 3 ⁇ 4 j cloth; 50, reactor; 60 , the discharge of the reaction mixture.
  • Figure 4 is a graph of temperature versus time for an aqueous suspension solution.
  • Figure 5 is a graph of pH versus time for an aqueous suspension solution.
  • Scheme 1 describes the preparation of a new precipitated carbonium. Any suitable grade of quicklime can be supplied to the aqueous suspension tank A via line 1, where it reacts with water to form a calcium hydroxide liquid. The calcium hydroxide water is then supplied to the carbonized tank B via line 2. The carbonized tank B
  • Line 1 receives carbon dioxide from a carbon dioxide tank that is not shown in the schematic.
  • the carbon dioxide gas stream supplied to tank B through line 3 is divided into two streams having different functions.
  • the primary function of the first gas stream is to react with an aqueous suspension of calcium hydroxide to form carbon ⁇ .
  • a second gas stream is supplied to the carbonation tank B for agitating the suspension. All participating substances and multiphase and interfacial reactions are listed in Figure 2.
  • the aqueous suspension containing the carbonated surface 1 line 4 is sent to a centrifugal separation system C where the carbon ⁇ «separates from the water.
  • the resulting composition comprising about 30% by weight of water is then conveyed via line 5 to a drying unit D, through line 6 to cooling unit E, and to line 7 to the pulverizer.
  • the pulverized carbon crucible line 8 is then directly commercialized or otherwise processed.
  • FIG 3 is a schematic illustration of a carbon dioxide distribution system in accordance with the present invention.
  • Reactor 50 includes a pH probe 10 and a sensor 20. Either or both of these devices can be used to determine the progress of the reaction in the carbon ⁇ t3 ⁇ 4 reactor B shown in Fig. 1.
  • Carbon dioxide is supplied to tank B through two different distributors.
  • the first gas distributor is a self-sealing or non-self-sealing carbon dioxide micropore distributor 30 which can be used to inject the necessary amount of carbon dioxide into the carbonation tank to react with the hydrazine hydroxide present in the solution.
  • a carbon dioxide gas « 1 carbon dioxide injection distributor 40 is supplied to the carbon crucible t3 ⁇ 4 tank B of Figure 1, and the carbon dioxide provides an agitated water suspension for agitating the hydroxide surface.
  • the carbon dioxide is fed to the reactor through two 3 ⁇ 4 gas distributors, the «distributor and the injection distributor.
  • the volume of bubbling carbon dioxide is 1 Nm 3 /hr/m at 6 bar
  • the carbon dioxide micro-distributor with a total length of 15 m has a carbon dioxide distribution capacity of up to 15 Nm 3 /hr at 6 bar.
  • the distribution of the touch of smoke is three layers, each layer is a series of circular concentric rings.
  • Injection score The cloth has 13 holes. Each hole has a diameter of 1 mm, and the total volume of carbon dioxide distributed by the injection distributor at the time of the bar is 30 Nm 3 /hr.
  • both types of distributors are used to distribute carbon dioxide and agitate the suspension.
  • the experimental results are shown in Figures 4 and 5.
  • Figure 4 depicts the change in solution temperature over time
  • Figure 5 depicts the solution pH as a function of time.
  • the temperature of the suspension increased to about 73 °C before it decreased, and the reaction was near completion at the inflection point of the temperature.
  • the temperature of the suspension is 53 from the beginning before it is lowered.
  • C gradually rises to about 73 V.
  • a thymol citrate-base pH meter was also used to indicate if the reaction was complete. Relative to the change, the pH shows a change in the opposite trend before the reaction is completed. However, with a peak of about 73 °C, the change in pH showed a similar trend, rapidly dropping from 11 to 9.2. The reaction is completed in 90 years, during which the pressure of carbon dioxide changes from 2 bar to 6 bar at different times of the reaction, but the total carbon dioxide consumption is recorded as budgeted.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

La présente invention concerne un procédé et un système pour la préparation de carbonate de calcium précipité. Un premier flux et un second flux de dioxyde de carbone sont fournis à une suspension aqueuse d'oxyde de calcium pour former du carbonate de calcium. Le premier flux de dioxyde de carbone provient d'un tube en caoutchouc microporeux, et le second flux de dioxyde de carbone provient d'un distributeur d'injection. La suspension de carbonate de calcium obtenue est séparée, séchée, refroidie, et pulvérisée pour récupérer du carbonate de calcium précipité.
PCT/CN2012/073086 2011-04-25 2012-03-27 Procédé et système pour la préparation de carbonate de calcium précipité Ceased WO2012146111A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
BR112013027163A BR112013027163A2 (pt) 2011-04-25 2012-03-27 processo e sistema para a produção de carbonato de cálcio precipitado

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201110159429.1 2011-04-25
CN2011101594291A CN102757074A (zh) 2011-04-25 2011-04-25 制备沉淀碳酸钙的方法和系统

Publications (1)

Publication Number Publication Date
WO2012146111A1 true WO2012146111A1 (fr) 2012-11-01

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PCT/CN2012/073086 Ceased WO2012146111A1 (fr) 2011-04-25 2012-03-27 Procédé et système pour la préparation de carbonate de calcium précipité

Country Status (3)

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CN (1) CN102757074A (fr)
BR (1) BR112013027163A2 (fr)
WO (1) WO2012146111A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104418376B (zh) * 2013-09-03 2016-08-17 井陉县京华钙业有限公司 一种沉淀碳酸钙的生产工艺

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1634645A (zh) * 2003-12-31 2005-07-06 淄博矿业集团有限责任公司 循环流化反应器
CN1806906A (zh) * 2005-01-18 2006-07-26 中国石化上海石油化工股份有限公司 气流搅拌的制备对苯二甲酸的氧化反应装置
CN101172636A (zh) * 2007-10-16 2008-05-07 陈杰 纳米碳酸钙制备方法
CN101575114A (zh) * 2009-03-30 2009-11-11 上海东升新材料有限公司 轻质碳酸钙碳化装置及工业应用
CN201613129U (zh) * 2010-02-08 2010-10-27 建德市天石碳酸钙有限责任公司 气液均匀混合的碳化塔

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1634645A (zh) * 2003-12-31 2005-07-06 淄博矿业集团有限责任公司 循环流化反应器
CN1806906A (zh) * 2005-01-18 2006-07-26 中国石化上海石油化工股份有限公司 气流搅拌的制备对苯二甲酸的氧化反应装置
CN101172636A (zh) * 2007-10-16 2008-05-07 陈杰 纳米碳酸钙制备方法
CN101575114A (zh) * 2009-03-30 2009-11-11 上海东升新材料有限公司 轻质碳酸钙碳化装置及工业应用
CN201613129U (zh) * 2010-02-08 2010-10-27 建德市天石碳酸钙有限责任公司 气液均匀混合的碳化塔

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CN102757074A (zh) 2012-10-31
BR112013027163A2 (pt) 2017-01-17

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