CN113023739A - Spodumene powder suspension preheating calcination crystal form conversion process - Google Patents

Spodumene powder suspension preheating calcination crystal form conversion process Download PDF

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Publication number
CN113023739A
CN113023739A CN202110285515.0A CN202110285515A CN113023739A CN 113023739 A CN113023739 A CN 113023739A CN 202110285515 A CN202110285515 A CN 202110285515A CN 113023739 A CN113023739 A CN 113023739A
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spodumene
suspension
powder
alpha
type
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继明
崔冬梅
包先法
王仕群
焦鸿溢
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Hefei Cement Research and Design Institute Co Ltd
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Hefei Cement Research and Design Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/26Aluminium-containing silicates, i.e. silico-aluminates
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

Abstract

The invention discloses a spodumene powder suspension preheating calcination crystal form conversion process, and a finished product of beta-type spodumene powder with the crystal form conversion rate of more than or equal to 98% is obtained. The method comprises the following steps: firstly, taking alpha-spodumene as a raw material, carrying out mineral separation and crushing, and then grinding to prepare alpha-spodumene fine powder with the water content of less than 1%; then the suspension preheater preheats the alpha-type spodumene powder, the suspension calciner calcines the alpha-type spodumene powder at high temperature to perform crystal form conversion, and the cyclone separator and the automatic material distributing valve are used for realizing material circulation and re-calcination. And finally, the finished product of the beta-type spodumene powder out of the suspension calcining furnace system enters a suspension cooling system for cooling. The invention completes the whole processes of spodumene powder preheating, calcining, crystal transformation and finished product beta-type spodumene powder cooling in a suspension state. The invention has advanced process, green and energy-saving; the automation degree is high, and intellectualization can be realized; and can greatly improve the single-line production scale.

Description

Spodumene powder suspension preheating calcination crystal form conversion process
Technical Field
The invention relates to the technical field of spodumene lithium extraction, in particular to a spodumene powder suspension preheating calcination crystal form conversion process.
Background
Lithium is an indispensable key mineral raw material for new energy industry development, and is widely applied to the high and new technical field, particularly, the price of lithium salt is dramatically increased since the country strongly supports the development of the new energy industry. In 2018, the lithium consumption of the lithium battery industry accounts for 56% and exceeds the sum of the lithium consumption of other industries. Although the total amount of lithium bittern resources is dominant and the cost of lithium extraction from bittern is lower than that of lithium extraction from ore, the yield of lithium extraction from ore exceeds that of lithium extraction from bittern since 2018, and the ratio of the yield of lithium extraction from ore is still further improved in the future. Based on the weight of extracting lithium from ores, the invention of a new, economically feasible technical process for extracting lithium from spodumene concentrate has important significance.
In industry, spodumene is mainly used as a raw material for extracting lithium salt, but natural spodumene has a stable structure and is difficult to react with acid and alkali, and the spodumene needs to be subjected to roasting transformation treatment before being subjected to acidification treatment, namely, the spodumene is converted into beta-type spodumene from alpha-type spodumene.
In industrial production, rotary kiln roasting is commonly adopted for crystal form conversion, and the process comprises the following steps: finely crushing alpha-spodumene, roasting at 1000-1100 ℃ for 0.5-2 hours in a rotary kiln to convert the spodumene from alpha type to beta type, cooling the calcined material by a cooler, grinding the calcined material to about 0.15mm after cooling, mixing with concentrated sulfuric acid, acidizing and roasting at 250-350 ℃ for 0.5 hour in an acidizing rotary kiln to obtain lithium sulfate, dissolving the lithium sulfate by water leaching, and purifying and filtering to obtain the lithium-rich lithium sulfate solution. The main drawbacks presented by this roasting process are as follows:
(1) the rotary kiln has poor heat transfer (radiation heat transfer), long calcination time, great temperature control difficulty, low production capacity, high energy consumption of finished products, large occupied area of equipment, high equipment investment and high production cost.
(2) Because the rotary kiln has poor high-temperature calcination heat conductivity, the calcination transformation material can have local hard sintering blocks, kiln coatings are easy to form or large blocks are easy to produce, and the power consumption of a subsequent grinding section system is increased.
Therefore, a green, energy-saving and environment-friendly spodumene powder calcined crystal form conversion process is needed.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a spodumene powder suspension preheating calcination crystal form conversion process.
The invention is realized by the following technical scheme:
a spodumene powdery suspension preheating calcination crystal form conversion process specifically comprises the following steps:
(1) spodumene powder preparation, storage, metering and conveying
Crushing blocky alpha-type spodumene with the water content of less than 8 percent, grinding the blocky alpha-type spodumene by a spodumene grinding system to prepare alpha-type spodumene fine powder with the water content of less than 1 percent, collecting the alpha-type spodumene fine powder by a cyclone dust collector, sending the alpha-type spodumene fine powder into a powder homogenizing warehouse, and sending the homogenized alpha-type spodumene powder into a multistage suspension preheater connected in series after steady flow measurement;
(2) spodumene powder preheating
Preheating alpha-type spodumene powder by adopting a multi-stage suspension preheater connected in series: feeding alpha-spodumene powder into an inlet pipeline of a cyclone cylinder of a first-stage suspension preheater, and then gradually preheating the alpha-spodumene powder by other cyclone cylinders of a multi-stage suspension preheater and then feeding the alpha-spodumene powder into a suspension calciner;
(3) spodumene powder crystal type transition
The alpha-type spodumene powder preheated by the multistage series suspension preheaters is subjected to high-temperature calcination in the suspension calcining furnace by utilizing fuel to burn in a high-temperature air environment, so that the crystal form transformation is realized, and the beta-type spodumene powder is generated;
(4) suspension cooling of beta-spodumene powder
And (3) separating and collecting the beta-type spodumene powder out of the suspension calciner by a cyclone separator, feeding the beta-type spodumene powder into a multistage series suspension cooler for cooling, and obtaining a finished product of the beta-type spodumene powder with the transformed crystal form.
The granularity of the alpha-spodumene after crushing is less than 40 mm; the fineness of the alpha-spodumene fine powder is R0.08, and the residue on the sieve is 5-25%.
High-temperature waste gas at the outlet of the cyclone cylinder of the first-stage suspension preheater is sent to a waste gas dedusting system or a spodumene grinding system through a high-temperature fan after part of heat is recovered by a waste heat recovery device.
The calcination temperature in the suspension calciner is controlled to be 1050-1080 ℃, and the outlet temperature of a gooseneck of the suspension calciner is controlled to be 850-930 ℃.
The fuel used by the suspension calciner is one or more of coal, natural gas, fuel oil and petroleum coke.
The discharging pipe of the cyclone separator is provided with an automatic distributing valve, so that the calcined material can enter the suspension calcining furnace for cyclic re-calcination (the proportion of the calcined material is adjustable within 0-100%), and the conversion rate of the spodumene powder can be effectively controlled.
The lower end of the suspension calcining furnace is connected with an air inlet chamber through a necking, and the air inlet chamber is connected with an auxiliary combustion ignition chamber.
The invention has the advantages that: (1) the invention preheats, calcines and cools in suspension state, has high heat exchange efficiency and low heat consumption of the system;
(2) the powder suspension calcination of the invention has high heat exchange speed and high crystal transformation degree;
(3) the suspension calcining furnace has uniform and controllable temperature distribution, and the uniform stability of the product quality is greatly improved;
(4) the high-temperature process of the invention is carried out in a static device which does not operate, the operation is stable and reliable, and the operation rate is high;
(5) the invention has the advantages of easy large-scale production scale, low investment, comprehensive energy consumption and low cost;
(6) the invention has high automation degree and can realize intellectualization.
Drawings
Fig. 1 is a system flow diagram of a spodumene powder suspension calcination crystal form conversion process of the present invention.
In the figure, 1-auxiliary ignition chamber, 2-air inlet chamber, 3-suspension calcining furnace, 4-gooseneck, 5-cyclone separator, 5-1 automatic material distribution valve, 6-C4 cyclone cylinder, 7-C3 cyclone cylinder, 8-C2 cyclone cylinder, 9-C1 cyclone cylinder, 10-high temperature fan, 11-CL1 cyclone cylinder, 12-CL2 cyclone cylinder, 13-cooler exhaust fan, 14-air release valve, 15-waste gas treatment pipeline, A-alpha type spodumene powder and B-beta type spodumene powder.
Detailed Description
Example 1
As shown in figure 1, the invention discloses a spodumene powder suspension preheating calcination crystal form conversion process, which comprises the following steps:
the method comprises the steps of crushing blocky alpha-spodumene with the water content of less than 8% (the granularity is generally less than 40 mm), grinding to obtain alpha-spodumene fine powder with the water content of less than 1% (the fineness R is 0.08 and the screen residue is 5-25%), collecting the alpha-spodumene fine powder by a cyclone dust collector, conveying the alpha-spodumene fine powder into a powder homogenizing warehouse by a conveying device such as a bucket elevator, metering the homogenized alpha-spodumene powder by a steady flow, and conveying the alpha-spodumene powder into a suspension preheater by the bucket elevator.
Raw material alpha-spodumene powder A is fed into an inlet pipeline of a preheater C1 cyclone 9, is preheated step by preheaters C2-C4 cyclones 8, 7 and 6, is collected by a preheater C4 cyclone 6 and then enters a suspension calciner 3.
After part of heat of the high-temperature waste gas at the outlet of the C1 cyclone 9 is recovered by the waste heat recovery device, the high-temperature waste gas is sent to the waste gas dedusting system 15 or the spodumene grinding system by the high-temperature fan 10.
The preheated alpha-type spodumene powder A collected by a cyclone 6 of a preheater C4 enters a suspension calciner 3, the spodumene powder A is burnt at high temperature in the suspension calciner 3 by utilizing fuel under the high-temperature air environment to realize crystal form conversion and generate a beta-type spodumene powder finished product B, a cyclone separator 5 is arranged at an outlet of a gooseneck tube 4 to separate and collect the burnt beta-type spodumene powder B, and an automatic material distributing valve 5-1 is arranged on a discharging tube of the cyclone separator 5 to realize that a calcined material enters the suspension calciner to be circularly calcined.
The beta-spodumene powder B separated and collected by the cyclone separator 5 is fed into an inlet pipeline of a cyclone cylinder 11 of a secondary series suspension cooler CL1 through a blanking pipe, and is separated from the cyclone cylinder 11 of a secondary series suspension cooler CL1 through heat exchange; then feeding the air into the inlet pipeline of the secondary series suspension cooler CL2 cyclone 12, and the air enters the inlet pipeline of the CL2 cyclone 12 and is separated and collected by the heat exchange and the secondary series suspension cooler CL2 cyclone 12.
The finished product beta-type spodumene powder B is cooled by the two-stage series suspension cooler, the obtained hot air at the outlet of the CL1 cyclone 11 is mostly sent into the auxiliary combustion ignition chamber 1 for combustion supporting through the cooler exhaust fan 13, and in order to reasonably match the air volume of the cooling system and the calcining system, a small part of redundant hot air is sent into a pipeline of the waste gas dust removal system 15 through the air release valve 14.
In the embodiment, the calcining temperature in the suspension calciner 3 is controlled to be 1050-1080 ℃, and the outlet temperature of the gooseneck 4 is controlled to be 850-930 ℃.
In this embodiment, the fuel used by the suspension combustion furnace 3 is one or more of coal, natural gas, fuel oil, and petroleum coke.
In this embodiment, the lower end of the suspension calciner 3 is connected with an air inlet chamber 2 through a throat, the air inlet chamber is connected with an auxiliary combustion ignition chamber 1, and the auxiliary combustion ignition chamber 1 introduces combustion air, ignites and burns fuel for the suspension calciner to increase the temperature of the combustion air.
In this embodiment, the configuration of the preheater is four stages, i.e., the preheater C1-C4 cyclone, but is not limited thereto, and may be five stages or three stages.
In this embodiment, the number of series stages of the multistage series suspension coolers is two, that is, the two-stage series suspension cooler CL1-CL2 cyclone, but is not limited thereto, and may be three stages.
In this embodiment, the preheater is configured as a single series, i.e. the preheater C1-C4 has one row of cyclones, but not limited thereto, and may also have two rows in parallel.
In this embodiment, the multistage series suspension coolers are single series, i.e., the two-stage series suspension coolers CL1-CL2 cyclone, but not limited thereto, and may be two parallel rows.
In the embodiment, a small part of redundant hot air of the secondary suspension cooler can be introduced to the fuel grinding system to be used as a fuel drying heat source.
The embodiment of the present invention is described only for the preferred embodiment of the present invention, and not for the limitation of the concept and scope of the present invention, and the technical solution of the present invention is subject to various modifications and improvements by those skilled in the art without departing from the design concept of the present invention.

Claims (7)

1. A spodumene powder suspension preheating calcination crystal form conversion process is characterized in that: the method specifically comprises the following steps:
(1) spodumene powder preparation, storage, metering and conveying
Crushing blocky alpha-type spodumene with the water content of less than 8 percent, grinding the blocky alpha-type spodumene by a spodumene grinding system to prepare alpha-type spodumene fine powder with the water content of less than 1 percent, collecting the alpha-type spodumene fine powder by a cyclone dust collector, sending the alpha-type spodumene fine powder into a powder homogenizing warehouse, and sending the homogenized alpha-type spodumene powder into a multistage suspension preheater connected in series after steady flow measurement;
(2) spodumene powder preheating
Preheating alpha-type spodumene powder by adopting a multi-stage suspension preheater connected in series: feeding alpha-spodumene powder into an inlet pipeline of a cyclone cylinder of a first-stage suspension preheater, and then gradually preheating the alpha-spodumene powder by other cyclone cylinders of a multi-stage suspension preheater and then feeding the alpha-spodumene powder into a suspension calciner;
(3) spodumene powder crystal type transition
The alpha-type spodumene powder preheated by the multistage series suspension preheaters is burnt in a suspension calcining furnace by fuel under a high-temperature air environment to carry out high-temperature calcination on the alpha-type spodumene powder, so that crystal form transformation is realized, and beta-type spodumene powder is generated;
(4) suspension cooling of beta-spodumene powder
And (3) separating and collecting the beta-type spodumene powder out of the suspension calciner by a cyclone separator, feeding the beta-type spodumene powder into a multistage series suspension cooler for cooling, and obtaining a finished product of the beta-type spodumene powder with the transformed crystal form.
2. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: the granularity of the alpha-spodumene after crushing is less than 40 mm; the fineness of the alpha-spodumene fine powder is R0.08, and the residue on the sieve is 5-25%.
3. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: high-temperature waste gas at the outlet of the cyclone cylinder of the first-stage suspension preheater is sent to a waste gas dedusting system or a spodumene grinding system through a high-temperature fan after part of heat is recovered by a waste heat recovery device.
4. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: the calcination temperature in the suspension calciner is controlled to be 1050-1080 ℃, and the outlet temperature of a gooseneck of the suspension calciner is controlled to be 850-930 ℃.
5. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: the fuel used by the suspension calciner is one or more of coal, natural gas, fuel oil and petroleum coke.
6. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: the discharging pipe of the cyclone separator is provided with an automatic distributing valve.
7. The spodumene powdery suspension preheating calcination crystal form conversion process according to claim 1, characterized in that: the lower end of the suspension calcining furnace is connected with an air inlet chamber through a necking, and the air inlet chamber is connected with an auxiliary combustion ignition chamber.
CN202110285515.0A 2021-03-17 2021-03-17 Spodumene powder suspension preheating calcination crystal form conversion process Pending CN113023739A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115304073A (en) * 2022-07-14 2022-11-08 北京凯盛建材工程有限公司 Spodumene calcination transformation system and method

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU8611482A (en) * 1981-09-11 1983-03-17 Fuller Company Roasting ore
US4668182A (en) * 1985-04-01 1987-05-26 Cohen Sidney M Apparatus for calcining gypsum
CN103204510A (en) * 2013-04-24 2013-07-17 成都正远机电设备有限公司 Spodumene roasting transformation method
CN103922355A (en) * 2014-04-22 2014-07-16 四川卡森科技有限公司 Device for producing spodumene and preparation process
CN205773396U (en) * 2016-07-18 2016-12-07 沈阳鑫博工业技术股份有限公司 A kind of reduce the device of alpha-aluminium oxide content in metallurgical-grade aluminum oxide
CN107628627A (en) * 2017-10-16 2018-01-26 福州大学 A kind of method of natural spodumene circulation roasting crystal formation conversion
CN107739847A (en) * 2017-10-16 2018-02-27 福州大学 A kind of crystal formation conversion method of natural spodumene suspension roasting
CN111847466A (en) * 2020-08-24 2020-10-30 合肥水泥研究设计院有限公司 Black talc powder suspension calcining and whitening device and process

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU8611482A (en) * 1981-09-11 1983-03-17 Fuller Company Roasting ore
US4668182A (en) * 1985-04-01 1987-05-26 Cohen Sidney M Apparatus for calcining gypsum
CN103204510A (en) * 2013-04-24 2013-07-17 成都正远机电设备有限公司 Spodumene roasting transformation method
CN103922355A (en) * 2014-04-22 2014-07-16 四川卡森科技有限公司 Device for producing spodumene and preparation process
CN205773396U (en) * 2016-07-18 2016-12-07 沈阳鑫博工业技术股份有限公司 A kind of reduce the device of alpha-aluminium oxide content in metallurgical-grade aluminum oxide
CN107628627A (en) * 2017-10-16 2018-01-26 福州大学 A kind of method of natural spodumene circulation roasting crystal formation conversion
CN107739847A (en) * 2017-10-16 2018-02-27 福州大学 A kind of crystal formation conversion method of natural spodumene suspension roasting
CN111847466A (en) * 2020-08-24 2020-10-30 合肥水泥研究设计院有限公司 Black talc powder suspension calcining and whitening device and process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115304073A (en) * 2022-07-14 2022-11-08 北京凯盛建材工程有限公司 Spodumene calcination transformation system and method

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