CN115572080B - Preparation method of feed-grade magnesium oxide - Google Patents

Preparation method of feed-grade magnesium oxide Download PDF

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CN115572080B
CN115572080B CN202211400662.9A CN202211400662A CN115572080B CN 115572080 B CN115572080 B CN 115572080B CN 202211400662 A CN202211400662 A CN 202211400662A CN 115572080 B CN115572080 B CN 115572080B
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magnetic separation
magnesium oxide
magnesite
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temperature
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CN115572080A (en
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王新
杨云洪
李晓燕
李长龙
李红
车太龙
张家俊
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Yingkou Magnesite Chemical Ind Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2/00Lime, magnesia or dolomite
    • C04B2/10Preheating, burning calcining or cooling
    • C04B2/102Preheating, burning calcining or cooling of magnesia, e.g. dead burning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • B03C1/30Combinations with other devices, not otherwise provided for
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C7/00Separating solids from solids by electrostatic effect
    • B03C7/02Separators
    • 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
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention belongs to the field of feed additives, and particularly relates to a preparation method of feed-grade magnesium oxide, which takes magnesite as a raw material, and high-purity magnesium oxide is obtained through low-temperature calcination and purification, wherein the purification comprises magnetic separation and electric separation. The invention solves the defects of the prior art, takes low-grade magnesite as a raw material, utilizes layer-by-layer assistance of low-temperature calcination, double magnetic separation and electroseparation, realizes secondary recycling of mineral substances, reduces cost, realizes effective control of elements such as silicon, calcium, iron and the like in magnesium oxide, and provides safety guarantee for subsequent use in feed additives and mixed feed additives.

Description

Preparation method of feed-grade magnesium oxide
Technical Field
The invention belongs to the field of feeds, and particularly relates to a preparation method of feed-grade magnesium oxide.
Background
Magnesium oxide belongs to mineral nutrient elements, magnesium element is an indispensable factor in the livestock and poultry body when participating in the bone making process and muscle contraction, is an activator of various enzymes in the livestock and poultry body, and plays an extremely important role in the metabolism of substances and the nerve function in the livestock and poultry body. Meanwhile, magnesium oxide is a special feed additive for ruminants, is an inorganic magnesium source which is most excellent to be applied in ruminant feed, belongs to an alkalizing agent, and can be beneficial to improving the rumen pH value of ruminants, improving the intake of mammary gland to blood metabolites and improving the milk fat rate. If the livestock and poultry body lacks magnesium, the livestock and poultry body can cause substance metabolism and nerve dysfunction, supply disturbance, influence the growth and development of the livestock and poultry and even cause death.
Magnesite is one of the important inorganic magnesium sources, the main chemical component being magnesium carbonate (MgCO 3 ) The MgO content in the low-grade magnesite is 36-42%, and the low-grade magnesite contains elements such as calcium (Ca), silicon (Si), iron (Fe) and the like, the purity of the magnesium oxide serving as a feed additive is more than or equal to 96.5% in the prior art, and the method of calcining the magnesite into common magnesium oxide and then calcining the common magnesium oxide after hydration reaction to precipitate magnesium is generally adopted at home and abroad at present. On the other hand, in order to add calcium (Ca) and silicon (Si), the feed premix enterprises prepare mixed feed additive magnesia with MgO of not less than 45% and other different specification contents by using MgO of not less than 96.5% and adding diluent carriers such as zeolite powder and talcum powder, and the like, so that hazardous impurities are easy to introduce for the second time, and the use of the feed additive magnesia has safety risks.
Disclosure of Invention
Aiming at the problems existing in the prior art, the preparation method of the feed-grade magnesium oxide provided by the invention takes low-grade magnesite as a raw material, and utilizes low-temperature calcination, double magnetic separation and layer-by-layer assistance of electrowinning to realize secondary recycling of mineral substances, reduce cost, realize effective control of elements such as silicon, calcium, iron and the like in the magnesium oxide, and provide safety guarantee for subsequent use in feed additives and mixed feed additives.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a process for preparing feed-class magnesium oxide includes such steps as calcining magnesite as raw material at low temp. and purifying to obtain high-purity magnesium oxide, and includes magnetic separation and electric separation.
The preparation method comprises the following steps:
step 1, crushing magnesite to obtain crushed magnesite; the granularity of the magnesite crushed ore is smaller than 10mm; the magnesite is finely crushed by crushing treatment, large particles are finely crushed, and the surface of magnesium carbonate is improved to be exposed; the magnesite is low-grade magnesite, the MgO content is 36-42%, and the SiO is the mixture of the magnesite and the MgO 2 5-10%, caO 1-5%, fe 2 O 3 The content is 1-3%.
Step 2, carrying out low-temperature suspension roasting on the magnesite crushed ore, and slowly cooling to obtain a roasting material; the low-temperature suspension roasting is carried out in a suspension roasting furnace, and the roasted gas is turned back into the suspension roasting furnace through a turning pipeline, wherein the temperature of the roasting furnace is 600-650 ℃ and the time is 6-8min; the method comprises the steps of adopting a low-temperature suspension calcination mode to decompose magnesium carbonate, wherein the magnesium carbonate is incompletely decomposed to form carbon monoxide, and simultaneously, the carbon monoxide returns to a roasting furnace again in a rotary pipeline to reduce weak magnetic iron minerals in magnesite into strong magnetic iron minerals; furthermore, the low-temperature suspension roasting adopts a microwave heating technology, the microwave heating technology can heat the crushed magnesite to form internal and external heating, the internal magnesium carbonate is subjected to temperature influence to generate internal partial decomposition while the external magnesium carbonate is subjected to decomposition reaction, CO is wrapped inside to generate internal reduction reaction, and the internal holes of the crushed magnesite are increased while the iron ore is converted, so that conditions are provided for subsequent second crushing;
step 3, secondarily crushing and grinding the roasting material, screening to obtain fine powder, then placing the fine powder into a suspension roasting furnace for secondary low-temperature suspension roasting, and cooling to obtain secondary roasting material, wherein the granularity of the fine powder is not more than 3mm, the secondary low-temperature suspension roasting is performed in the suspension roasting furnace, and the roasted gas is rotated into the suspension roasting furnace through a rotation pipeline, and the temperature of the roasting furnace is 620-670 ℃ for 10-15min; based on the roasting material itself belonging to crushed ore materials, a magnesium carbonate decomposition system from outside to inside is formed in the roasting process, magnesium carbonate on the surface can be decomposed, the decomposition of magnesium carbonate in the surface is avoided, meanwhile, the calcined magnesite forms a certain porosity and the strength of mineral substances is reduced, so that the roasting material is subjected to secondary crushing and powder treatment to refine particles, high-quality fine powder is achieved, the magnesium carbonate in the roasting material is fully exposed, the roasting time is prolonged, the decomposition of the magnesium carbonate is ensured, meanwhile, CO generated after the decomposition is reacted again in a reflux way, and the reduction of the weak magnetic iron mineral into the strong magnetic iron mineral is ensured; the self particles of the roasting material after the secondary low-temperature roasting treatment are smaller, and the magnesium carbonate is subjected to secondary crushing to form refined powder, so that the self particles are miniaturized and made porous;
step 4, carrying out primary magnetic separation treatment on the secondary roasting material to obtain magnetic concentrate and magnetic tailings; then crushing the magnetic separation tailings to obtain magnetic separation tailings powder; the magnetic separation adopts a dry magnetic separator, the magnetic field intensity is 0.8-1.0T, the iron ore is separated by magnetic separation to form magnetic separation tailings and magnetic separation concentrate, and the magnetic separation tailings are further crushed by a porous structure formed by secondary roasting to form powder with finer particles; the particle size of the magnetic separation tailing powder is not more than 75 mu m;
step 5, carrying out secondary magnetic separation treatment on the magnetic separation tailings powder to obtain secondary magnetic separation concentrate and secondary magnetic separation tailings, wherein the magnetic field intensity of the secondary magnetic separation treatment is 1.0-1.1T; according to the method, the fine powder is subjected to magnetic separation treatment by utilizing a secondary magnetic separation mode, so that the internal iron ore is further removed, the content of iron element is effectively reduced, and the removal rate of the iron element is improved;
step 6, placing the secondary magnetic separation tailings into a triboelectric separator for electric separation treatment to obtain concentrate products, wherein the electric separation voltage is 18-20kV; the electric separator utilizes a charge system to separate, and is matched with the charge characteristic of the secondary magnetic separation tailing material, so that impurities can be effectively separated, and the content of magnesium oxide is improved;
and 7, calcining the concentrate product, and cooling to room temperature to obtain a magnesium oxide product, wherein the calcining temperature is 700-750 ℃.
And (3) absorbing the tail gas in the step (2) and the step (3) by adopting a carbon dioxide tail gas device.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the defects of the prior art, utilizes a low-temperature roasting mode to promote incomplete decomposition of magnesium carbonate to generate carbon monoxide gas, and utilizes a recycling mode to recycle carbon monoxide, thereby providing conditions for magnetic separation.
2. According to the invention, magnesium carbonate is used as a pore-forming agent, so that multiple pores are formed in the decomposition process, the strength of magnesite is reduced, conditions are provided for subsequent further reduction, and meanwhile, the crushed magnesite is subjected to magnetic separation and electroseparation to form a more refined separation system, so that the aim of improving the quality of magnesium oxide is fulfilled.
3. The invention takes low-grade magnesite as raw material, utilizes layer-by-layer assistance of low-temperature roasting, double magnetic separation and electroseparation, realizes secondary recycling of mineral substances, reduces cost, realizes effective control of elements such as silicon, calcium, iron and the like in magnesium oxide, and provides safety guarantee for the field of subsequent feed additives and mixed feed additives.
4. The method realizes the high quality of magnesium oxide, the purity reaches 96.5%, and the whole process has strong controllability and good repeatability, and can be used in high-end fields such as feed.
Detailed Description
The invention is described in detail with reference to examples, but without any limitation to the claims of the invention.
Example 1
A process for preparing feed-class magnesium oxide includes such steps as calcining magnesite as raw material at low temp. and purifying to obtain high-purity magnesium oxide.
The preparation method comprises the following steps:
step 1, crushing magnesite to obtain crushed magnesite; the granularity of the magnesite powder is smaller than 10mm; the magnesite is low-grade magnesite, the MgO content is 41.08%, and the SiO is 2 The content of the additive is 7.01%, the content of CaO is 3.22%, and Fe 2 O 3 The content is 2.65%;
step 2, carrying out low-temperature suspension roasting on the magnesite crushed ore, and slowly cooling to obtain a roasting material; the low-temperature suspension roasting is performed in a suspension roasting furnace, and the roasted gas is turned back into the suspension roasting furnace through a turning pipeline, wherein the temperature of the roasting furnace is 600 ℃, and the time is 6min;
step 3, secondarily crushing and grinding the roasting material, screening to obtain fine powder, then placing the fine powder into a suspension roasting furnace for secondary low-temperature suspension roasting, and cooling to obtain secondary roasting material, wherein the granularity of the fine powder is not more than 3mm, the secondary low-temperature suspension roasting is performed in the suspension roasting furnace, and the roasted gas is rotated into the suspension roasting furnace through a rotation pipeline, and the temperature of the roasting furnace is 620 ℃ and the time is 10min;
step 4, carrying out primary magnetic separation treatment on the secondary roasting material to obtain magnetic concentrate and magnetic tailings; then crushing the magnetic separation tailings to obtain magnetic separation tailings powder; the magnetic separation adopts a dry magnetic separator, and the magnetic field strength is 0.8T; the particle size of the magnetic separation tailing powder is not more than 75 mu m
Step 5, carrying out magnetic separation treatment on the magnetic separation tailings powder to obtain secondary magnetic separation concentrate and secondary magnetic separation tailings, wherein the magnetic field intensity of the secondary magnetic separation treatment is 1.0T;
step 6, placing the secondary magnetic separation tailings into a friction electric separator for electric separation treatment to obtain concentrate products, wherein the electric separation voltage is 18kV;
and 7, carrying out secondary calcination on the concentrate product, and cooling to room temperature to obtain a magnesium oxide product, wherein the calcination temperature is 700 ℃.
And (3) absorbing the tail gas in the step (2) and the step (3) by adopting a carbon dioxide tail gas device.
In the feed-grade magnesium oxide prepared in this example, the MgO content was 96.93%, the CaO content was 0.56%, and the SiO content was 2 The content is 0.30 percent, fe 2 O 3 The content is 0.11%.
Example 2
A process for preparing feed-class magnesium oxide includes such steps as calcining magnesite as raw material at low temp. and purifying to obtain high-purity magnesium oxide.
The preparation method comprises the following steps:
step 1, crushing magnesite to obtain crushed magnesite; the granularity of the magnesite crushed ore is smaller than 10mm; the magnesite is low-grade magnesite, the MgO content is 41.08%, and the SiO is 2 The content of the additive is 7.01%, the content of CaO is 3.22%, and Fe 2 O 3 The content is 2.65%; the method comprises the steps of carrying out a first treatment on the surface of the
Step 2, carrying out low-temperature suspension roasting on the magnesite crushed ore, and slowly cooling to obtain a roasting material; the low-temperature suspension roasting is performed in a suspension roasting furnace, and the roasted gas is turned back into the suspension roasting furnace through a turning pipeline, wherein the temperature of the roasting furnace is 650 ℃, and the time is 8min;
step 3, secondarily crushing and grinding the roasting material, screening to obtain fine powder, then placing the fine powder into a suspension roasting furnace for secondary low-temperature suspension roasting, and cooling to obtain secondary roasting material, wherein the granularity of the fine powder is not more than 3mm, the secondary low-temperature suspension roasting is performed in the suspension roasting furnace, and the roasted gas is rotated into the suspension roasting furnace through a rotation pipeline, and the temperature of the roasting furnace is 670 ℃ and the time is 15min;
step 4, carrying out primary magnetic separation treatment on the secondary roasting material to obtain magnetic concentrate and magnetic tailings; then crushing the magnetic separation tailings to obtain magnetic separation tailings powder; the magnetic separation adopts a dry magnetic separator, and the magnetic field strength is 1.0T; the particle size of the magnetic separation tailing powder is not more than 75 mu m
Step 5, carrying out secondary magnetic separation treatment on the magnetic separation tailings powder to obtain secondary magnetic separation concentrate and secondary magnetic separation tailings, wherein the magnetic field intensity of the secondary magnetic separation treatment is 1.1T;
step 6, placing the secondary magnetic separation tailings into a friction electric separator for electric separation treatment to obtain concentrate products, wherein the electric separation voltage is 20kV;
and 7, calcining the concentrate product, and cooling to room temperature to obtain a magnesium oxide product, wherein the calcining temperature is 750 ℃.
And (3) absorbing the tail gas in the step (2) and the step (3) by adopting a carbon dioxide tail gas device.
In the feed-grade magnesium oxide prepared in this example, the MgO content was 97.51%, the CaO content was 0.53%, and the SiO content was 2 The content is 0.27 percent, fe 2 O 3 The content was 0.09%.
Example 3
A process for preparing feed-class magnesium oxide includes such steps as calcining magnesite as raw material at low temp. and purifying to obtain high-purity magnesium oxide.
The preparation method comprises the following steps:
step 1, crushing magnesite to obtain crushed magnesite; the granularity of the magnesite crushed ore is smaller than 10mm; the magnesite is low-grade magnesite, the MgO content is 41.08%, and the SiO is the mixture of the low-grade magnesite and the MgO 2 The content of the additive is 7.01%, the content of CaO is 3.22%, and Fe 2 O 3 The content is 2.65%;
step 2, carrying out low-temperature suspension roasting on the magnesite crushed ore, and slowly cooling to obtain a roasting material; the low-temperature suspension roasting is performed in a suspension roasting furnace, and the roasted gas is turned back into the suspension roasting furnace through a turning pipeline, wherein the temperature of the roasting furnace is 640 ℃, and the time is 7min;
step 3, secondarily crushing and grinding the roasting material, screening to obtain fine powder, then placing the fine powder into a suspension roasting furnace for secondary low-temperature suspension roasting, and cooling to obtain secondary roasting material, wherein the granularity of the fine powder is not more than 3mm, the secondary low-temperature suspension roasting is performed in the suspension roasting furnace, and the roasted gas is rotated into the suspension roasting furnace through a rotation pipeline, and the temperature of the roasting furnace is 650 ℃ for 15min;
step 4, carrying out primary magnetic separation treatment on the secondary roasting material to obtain magnetic concentrate and magnetic tailings; then crushing the magnetic separation tailings to obtain magnetic separation tailings powder; the magnetic separation adopts a dry magnetic separator, and the magnetic field strength is 0.9T; the particle size of the magnetic separation tailing powder is not more than 75 mu m
Step 5, carrying out secondary magnetic separation treatment on the magnetic separation tailings powder to obtain secondary magnetic separation concentrate and secondary magnetic separation tailings, wherein the magnetic field intensity of the secondary magnetic separation treatment is 1.1T;
step 6, placing the secondary magnetic separation tailings into a triboelectric separator for electric separation treatment to obtain concentrate products, wherein the electric separation voltage is 19kV;
and 7, calcining the concentrate product, and cooling to room temperature to obtain a magnesium oxide product, wherein the calcining temperature is 740 ℃.
And (3) absorbing the tail gas in the step (2) and the step (3) by adopting a carbon dioxide tail gas device.
In the feed-grade magnesium oxide prepared in this example, the MgO content was 97.29%, the CaO content was 0.51%, and the SiO content was 2 The content is 0.29 percent, fe 2 O 3 The content is 0.10%.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.

Claims (7)

1. A preparation method of feed-grade magnesium oxide is characterized in that: using magnesite as a raw material, and calcining at low temperature and purifying to obtain high-purity magnesium oxide, wherein the purification comprises magnetic separation and electric separation;
the preparation method comprises the following steps:
step 1, crushing magnesite to obtain crushed magnesite;
step 2, carrying out low-temperature suspension roasting on the magnesite crushed ore, and slowly cooling to obtain a roasting material; the low-temperature suspension roasting is carried out in a suspension roasting furnace, the roasted gas is turned back into the suspension roasting furnace through a turning pipeline, the temperature of the roasting furnace is 600-650 ℃, the time is 6-8min, and the low-temperature suspension roasting adopts a microwave heating technology;
step 3, secondarily crushing and grinding the roasting material, screening to obtain fine powder, then placing the fine powder into a suspension roasting furnace for secondary low-temperature suspension roasting, and cooling to obtain secondary roasting material; the granularity of the fine powder is not more than 3mm, the secondary low-temperature suspension roasting is carried out in a suspension roasting furnace, and the roasted gas is rotated into the suspension roasting furnace through a rotation pipeline, wherein the temperature of the roasting furnace is 620-670 ℃ and the time is 10-15min;
step 4, carrying out primary magnetic separation treatment on the secondary roasting material to obtain magnetic concentrate and magnetic tailings; then crushing the magnetic separation tailings to obtain magnetic separation tailings powder;
step 5, carrying out secondary magnetic separation treatment on the magnetic separation tailings powder to obtain secondary magnetic separation concentrate and secondary magnetic separation tailings;
step 6, placing the secondary magnetic separation tailings into a triboelectric separator for electric separation treatment to obtain concentrate products;
step 7, calcining the concentrate product, and cooling to room temperature to obtain a magnesium oxide product;
2. the method for preparing the feed-grade magnesium oxide according to claim 1, wherein: the granularity of the magnesite crushed ore in the step 1 is smaller than 10mm; the magnesite is low-grade magnesite, the MgO content is 36-42%, and the SiO is the mixture of the magnesite and the MgO 2 5-10%, caO 1-5%, fe 2 O 3 The content is 1-3%.
3. The method for preparing the feed-grade magnesium oxide according to claim 1, wherein: the magnetic separation in the step 4 adopts a dry magnetic separator, and the magnetic field intensity is 0.8-1.0T; the particle size of the magnetic separation tailing powder is not more than 75 mu m.
4. The method for preparing the feed-grade magnesium oxide according to claim 1, wherein: the magnetic field intensity of the secondary magnetic separation treatment in the step 5 is 1.0-1.1T.
5. The method for preparing the feed-grade magnesium oxide according to claim 1, wherein: the voltage of the electric selection in the step 6 is 18-20kV.
6. The method for preparing the feed-grade magnesium oxide according to claim 1, wherein: the calcination temperature in step 7 is 700-750 ℃.
7. The method for preparing the feed-grade magnesium oxide according to claim 1, wherein: and (3) absorbing the tail gas in the step (2) and the step (3) by adopting a carbon dioxide tail gas device.
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