CN106517267A - Preparation method of basic magnesium sulfate whiskers - Google Patents
Preparation method of basic magnesium sulfate whiskers Download PDFInfo
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- CN106517267A CN106517267A CN201610990061.6A CN201610990061A CN106517267A CN 106517267 A CN106517267 A CN 106517267A CN 201610990061 A CN201610990061 A CN 201610990061A CN 106517267 A CN106517267 A CN 106517267A
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- magnesium
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- magnesium hydroxide
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- 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
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- 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)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of basic magnesium sulfate whiskers. The preparation method comprises the following steps: S1, mixing a magnesium hydroxide source, a sulfate source and water to obtain a mixture, wherein the mass percent of magnesium hydroxide in the magnesium hydroxide source is not lower than 50%; S2, carrying out hydrothermal reaction on the mixture for 1-40 hours at the temperature of 100-300 DEG C, so as to obtain suspension; and S3, carrying out solid-liquid separation on the suspension, so as to obtain a solid phase and a liquid phase, washing, and drying the solid phase, so as to obtain the basic magnesium sulfate whiskers. According to the preparation method of the basic magnesium sulfate whiskers, the magnesium hydroxide source with relatively low magnesium hydroxide purity is taken as a preparation raw material; on one hand, the pollution and waste of byproduct magnesium hydroxide magnesium slag are reduced, and thus the magnesium harm problem is effectively controlled; and on the other hand, ammonia water, sodium hydroxide and the like are avoided from being used as a base source, and thus the preparation method is reduced. Meanwhile, the preparation method does not need other additives and is simple in technology; and the obtained basic magnesium sulfate product has high purity and good dispersibility.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, specifically, is related to one kind and prepares alkali formula sulphur using hydro-thermal method
The method of sour magnesium whisker.
Background technology
China is richly stored with extra large lake bittern water and ore magnesium resource, wherein 31.45 hundred million tons of magnesite ore reserves, accounts for the world total
The 22.5% of reserves, magnesite ore grade are high, reserves high concentration, and Liaoning and two province's reserves of Shandong account for national gross reserves
95.16%；Meanwhile, in China's salt lake bittern, magnesium resource particularly enriches, and is mainly distributed on Qinghai, Tibet, Xinjiang, Inner Mongol etc.
Ground, in salt lake bittern, magnesium salts reserves are 48.16 hundred million tons, wherein 31.43 hundred million tons of magnesium chloride, 16.73 hundred million tons of magnesium sulfate.
During magnesium resource is utilized, a considerable number of magnesium hydroxide of Some Enterprises by-product, due to by-product magnesium hydroxide (its
The quality of middle magnesium hydroxide is very not less than that 50%) purity is relatively low, and foreign ion species is more, it is impossible to directly using and it is most
Enterprise discards, and not only causes the pollution of environment, and causes the waste of resource, does not meet the green circulation economy of China's promotion.
Alkali magnesium sulfate crystal whisker is also known as Hydrous Magnesium Oxysulfate Whisker, has various existence forms, wherein be seen in report with
What morphology was prepared has MgSO4·5Mg(OH)2·3H2O、MgSO4·5Mg(OH)2·2H2O and 2MgSO4·Mg
(OH)2·3H2O, it is single needle-like or fan-shaped whisker under white powder, microscope that outward appearance is, is observed, alkali formula under ESEM
Magnesium sulfate crystal whisker length is 10 μm～200 μm, and 0.2 μm～1.0 μm of diameter, draw ratio are 50～1000, and relative density is 2.3,
Apparent density is 0.1, and specific surface is 10m2/g；Heat resistance is 300 DEG C, and oil absorption is 500mL/100g.Alkali magnesium sulfate crystal whisker
The characteristics of with high intensity, low-density and high elastic modulus, can increase as the reinforcement of the composites such as plastics, rubber and resin
Tough dose, improve the flexural strength and anti-impact force of base material.The light refractive index of alkali magnesium sulfate crystal whisker is 1.53, and each
The refractive index for planting resin is closest, thus very little is affected on the hue adjustment of composite, and polishing coloring is not almost hampered
Hinder, and good electrical insulation capability also assures which is applied in field of cables.
Numerous studies have been done in preparation for alkali magnesium sulfate crystal whisker both at home and abroad, summarize mainly in raw material and technique
Exist in process different.But, at present in the various techniques for preparing alkali magnesium sulfate crystal whisker, it is primarily present problems with：(1) exist
Use NaOH, ammoniacal liquor, magnesia, high purity magnesium hydroxide etc. as alkali source in the selection of raw material, cause production cost higher；
(2) adopt the magnesium salts of sea lake salt chemical industry by-product that magnesium hydroxide is prepared for raw material, then alkali magnesium sulfate crystalline substance is obtained with sulfuric acid reactant salt
Palpus；Or hydration reaction after low-grade magnesite is calcined, is carried out, add the prepared magnesium hydroxide of sulfuric acid solution mixed with magnesium sulfate
Liquid is closed, reaction obtains alkali magnesium sulfate crystal whisker；Although both approaches cost of material is relatively low, technical process is complex；(3)
Need to add the added regents such as crystal seed, surfactant, solubilizer, dispersant in preparation process；(4) raw material is needed at activation
Reason, makes that technique is increasingly complex, cost is higher.
Therefore, it is necessary to seeking, a kind of raw material is simple, with low cost, the process is simple side for preparing alkali magnesium sulfate crystal whisker
Method, meanwhile, the method can also solve the problems, such as the pollution of by-product magnesium hydroxide magnesium slag and waste.
The content of the invention
To solve the problems, such as above-mentioned prior art, the invention provides a kind of preparation side of alkali magnesium sulfate crystal whisker
Method, the magnesium hydroxide source that the preparation method only needs wherein magnesium hydroxide purity relatively low as alkali source and sulfuric acid root by lead to
Cross hydro-thermal reaction and obtain alkali magnesium sulfate crystal whisker, raw material is more single, process is simple.
In order to reach foregoing invention purpose, following technical scheme is present invention employs：
A kind of preparation method of alkali magnesium sulfate crystal whisker, including step：S1, magnesium hydroxide source, sulfuric acid root and water are mixed
Close, obtain mixture；In the magnesium hydroxide source, the mass percent of magnesium hydroxide is not less than 50%；S2, by the mixing
Thing carries out hydro-thermal reaction 1h～40h at 100 DEG C～300 DEG C, obtains suspension；Suspension described in S3, separation of solid and liquid, consolidate
Phase and liquid phase, washing, the drying solid phase, obtain the alkali magnesium sulfate crystal whisker.
Further, in the magnesium hydroxide source magnesium hydroxide and the amount of the material of sulfate radical in the sulfuric acid root ratio
For 0.1:1～10:1.
Further, in the mixture, the substance withdrawl syndrome of magnesium hydroxide is 0.05mol/L～10mol/L.
Further, in the magnesium hydroxide source, the mass percent of magnesium hydroxide is not less than 60%.
Further, the magnesium hydroxide source, sulfuric acid root, water-soluble magnesium salt and water are mixed, obtains the mixture.
Further, the water-soluble magnesium salt includes at least one in magnesium chloride, magnesium nitrate and magnesium sulfate.
Further, the sulfuric acid root includes at least one in sulfuric acid, water soluble sulfate.
Further, the water soluble sulfate is in magnesium sulfate, ammonium sulfate, sodium sulphate, potassium sulfate and aluminum sulfate
It is at least one.
Further, the liquid phase is back in step S1, for preparing the mixture.
Further, coproduct hydrogen of the magnesium hydroxide source in salt lake bittern, oil field water or magnesium ore deposit processing procedure
Magnesia.
The present invention is by magnesium hydroxide source (purity of wherein magnesium hydroxide is not less than 50%) is mixed simultaneously with sulfuric acid root
Carry out hydro-thermal reaction, you can prepare alkali magnesium sulfate crystal whisker；Meanwhile, the relatively low hydrogen-oxygen of the purity selected by the preparation method
Changing magnesium source can't affect the purity of alkali magnesium sulfate crystal whisker.Preparation method in compared to existing technology, in above-mentioned preparation process
In, on the one hand need not add the added regents such as crystal seed, surfactant, solubilizer, dispersant, reduce preparing raw material species,
Reduce preparation cost, simplify preparation technology；On the other hand the alkali source selected by be cheap magnesium hydroxide source, even can be with
For by-product magnesium hydroxide magnesium slag, preparation cost is not only reduced, also effectively reduce pollution and waste, reduced " magnesium evil " and ask
Topic.
Description of the drawings
By combining the following description that accompanying drawing is carried out, above and other aspect of embodiments of the invention, feature and advantage
Will become clearer from, in accompanying drawing：
Fig. 1 is the process chart of the preparation method of alkali magnesium sulfate crystal whisker of the invention；
Fig. 2 is the XRD piece of the alkali magnesium sulfate crystal whisker of embodiments in accordance with the present invention 1；
Fig. 3 is the SEM pictures of the alkali magnesium sulfate crystal whisker of embodiments in accordance with the present invention 1；
Fig. 4 is the SEM pictures of the alkali magnesium sulfate crystal whisker of embodiments in accordance with the present invention 4；
Fig. 5 is embodiments in accordance with the present invention 1, the alkali magnesium sulfate crystal whisker of embodiment 7 and alkali magnesium sulfate crystal whisker standard
The XRD contrast pictures of card.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to describing embodiments of the invention in detail.However, it is possible to come real in many different forms
Apply the present invention, and the present invention should not be construed as limited to the specific embodiment that illustrates here.On the contrary, there is provided these enforcements
Example is for the principle and its practical application of explaining the present invention, so that others skilled in the art are it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
It will be appreciated that although various materials can be described using term " first ", " second " etc. here, these
Material should not be limited by these terms.These terms are only used for making a distinction a material and another material.
Fig. 1 is the process chart of the preparation method of alkali magnesium sulfate crystal whisker of the invention.
With reference to Fig. 1, the preparation method of alkali magnesium sulfate crystal whisker of the invention comprises the steps：
S1, by magnesium hydroxide source, sulfuric acid root and water mix, obtain mixture.
Magnesium hydroxide source refers to that the mass percent of wherein magnesium hydroxide is not less than 50%, preferably not less than 60% thick hydrogen
Magnesia；Magnesium hydroxide source source can be the by-product magnesium hydroxide magnesium slag in salt lake bittern, oil field water or magnesium ore deposit processing procedure；
Certainly, in order to further improve the content of magnesium hydroxide in magnesium hydroxide source, the washable magnesium hydroxide source obtains magnesium hydroxide
Content is close to 100% purification magnesium hydroxide.
Preferably, also include water-soluble magnesium salt in mixture；That is, it is preferred that by magnesium hydroxide source, sulfuric acid root, water
Soluble magnesium salt and water mixing, obtain mixture.
Specifically, in magnesium hydroxide source, magnesium hydroxide and the ratio of the amount of the material of sulfate radical in sulfuric acid root are 0.1:1～
10:1；In the mixture, the substance withdrawl syndrome of magnesium hydroxide is 0.05mol/L～10mol/L.
More specifically, sulfuric acid root includes at least one in sulfuric acid, water soluble sulfate, wherein water soluble sulfate
Can be magnesium sulfate, ammonium sulfate, sodium sulphate, potassium sulfate, at least one in aluminum sulfate；Water-soluble magnesium salt includes magnesium chloride, nitre
At least one in sour magnesium, magnesium sulfate.
S2, mixture is carried out at 100 DEG C～300 DEG C hydro-thermal reaction 1h～40h, obtain suspension.
During hydro-thermal reaction, generally require and stir under 200rpm～1000rpm.
S3, separation of solid and liquid suspension, obtain solid phase and liquid phase, wash, be dried solid phase, obtain alkali magnesium sulfate crystal whisker.
Still there is the reactant not reacted completely in the liquid phase obtained after reaction and separation of solid and liquid, therefore can be by which
Collect, and be used for preparating mixture in next production process in being back to step S1.
It is preferred that be washed with deionized solid phase three times, obtain wash water, a secondary wash water after three washings respectively, wash for three times
Water, to economize on resources, a wash water can be back in step S1 is used for preparating mixture in next production process；Meanwhile,
By secondary wash water and the mixing of three wash waters, as washing solid phase for the first time in next production process.
Solid phase after scrubbed is preferably dried 4h～10h at 100 DEG C～140 DEG C.
Hereinafter, the preparation method of alkali magnesium sulfate crystal whisker of the invention will be carried out in detail with reference to specific embodiment
Description, for convenience of contrasting to each embodiment, each embodiment of analysis contrast in table form.In embodiment 1-8
Comparing result under different experiments parameter is as shown in table 1.
Contrast of 1 embodiments in accordance with the present invention 1-8 of table under different experiments parameter
Note：In table 1, content refers to the mass percent of magnesium hydroxide in magnesium hydroxide source；During concentration refers to mixture
The substance withdrawl syndrome of magnesium hydroxide；Dense H2SO4Refer to the aqueous sulfuric acid that mass percent is 98%；Mol ratio refers to hydrogen-oxygen
Change the ratio of magnesium hydroxide and the amount of the material of sulfate radical in sulfuric acid root in magnesium source.
X-ray diffraction test (abbreviation XRD) is carried out to the product that embodiment 1 is obtained, its XRD piece is as shown in Figure 2.From
As can be seen that the product that embodiment 1 is obtained is alkali magnesium sulfate crystal whisker in Fig. 2, in its XRD piece, characteristic peak is sharp, illustrates knot
Brilliant degree is higher, and product purity is also higher.Respectively the alkali magnesium sulfate crystal whisker that embodiment 1 and embodiment 4 are obtained is carried out
Sem test (abbreviation SEM), its SEM picture can be seen that respectively as shown in Figure 3 and Figure 4, from Fig. 3 and Fig. 4 and obtained
Alkali magnesium sulfate crystal whisker good dispersion, its a diameter of 0.1 μm～1 μm, draw ratio be 100～700.The yield of above-described embodiment
90% is not less than.XRD tests have equally been carried out to the product that embodiment 7 is obtained, the product of its XRD piece and embodiment 1
As shown in figure 5, in Figure 5, a represents the XRD piece of the product of embodiment 7 to the comparison diagram of XRD piece, and b represents the product of embodiment 1
The XRD piece of thing；From figure 5 it can be seen that the purity of obtained product alkali magnesium sulfate crystal whisker is higher, while also illustrate that nothing
It is raw material by the magnesium hydroxide source if the magnesium hydroxide purity in embodiment 1 is 70% is taken, still takes as in embodiment 7
The purification magnesium hydroxide of the magnesium hydroxide purity almost 100% through purifying is raw material, alkali magnesium sulfate of the invention
Preparation method do not interfere with final acquisition alkali magnesium sulfate purity, thus, can be by the alkali magnesium sulfate of the present invention
Preparation method be used for the recycling of by-product magnesium hydroxide magnesium slag during, reduce pollution and waste, increase economic by-product value.
Although illustrating and describing the present invention with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case of without departing from the spirit and scope of the present invention limited by claim and its equivalent, can here carry out form and
Various change in details.
Claims (10)
1. a kind of preparation method of alkali magnesium sulfate crystal whisker, it is characterised in that including step：
S1, by magnesium hydroxide source, sulfuric acid root and water mix, obtain mixture；In the magnesium hydroxide source, magnesium hydroxide
Mass percent is not less than 50%；
S2, the mixture is carried out at 100 DEG C～300 DEG C hydro-thermal reaction 1h～40h, obtain suspension；
Suspension described in S3, separation of solid and liquid, obtains solid phase and liquid phase, and washing, the drying solid phase obtain the alkali magnesium sulfate
Whisker.
2. preparation method according to claim 1, it is characterised in that magnesium hydroxide and the sulphur in the magnesium hydroxide source
In acid group source, the ratio of the amount of the material of sulfate radical is 0.1:1～10:1.
3. preparation method according to claim 1, it is characterised in that in the mixture, the material of magnesium hydroxide
Amount concentration is 0.05mol/L～10mol/L.
4. preparation method according to claim 1, it is characterised in that in the magnesium hydroxide source, the matter of magnesium hydroxide
Amount percentage is not less than 60%.
5. according to the arbitrary described preparation method of claim 1-4, it is characterised in that by the magnesium hydroxide source, sulfuric acid root,
Water-soluble magnesium salt and water mixing, obtain the mixture.
6. preparation method according to claim 5, it is characterised in that the water-soluble magnesium salt is selected from magnesium chloride, magnesium nitrate
With at least one in magnesium sulfate.
7. preparation method according to claim 5, it is characterised in that the sulfuric acid root includes sulfuric acid, water-soluble sulfuric acid
At least one in salt.
8. preparation method according to claim 7, it is characterised in that the water soluble sulfate is selected from magnesium sulfate, sulfuric acid
At least one in ammonium, sodium sulphate, potassium sulfate and aluminum sulfate.
9. preparation method according to claim 1, it is characterised in that the liquid phase is back in step S1, is used for
Prepare the mixture.
10. preparation method according to claim 1, it is characterised in that the magnesium hydroxide source derives from salt lake bittern, oil
By-product magnesium hydroxide in water in field or magnesium ore deposit processing procedure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108002413A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | Salt lake puies forward the method for comprehensive utilization of lithium solid by-product |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN109797435A (en) * | 2017-11-17 | 2019-05-24 | 华东理工大学 | A kind of new method of low cost synthesis alkali magnesium sulfate crystal whisker |
| CN109879655A (en) * | 2019-04-09 | 2019-06-14 | 辽宁科大中驰镁建材科技有限公司 | A method of hydraulicity magnesite board is prepared based on medium temperature mould pressing process |
| CN110436490A (en) * | 2019-08-06 | 2019-11-12 | 东北大学 | A method of magnesium oxysulfide short fiber material is prepared using magnesium method flue gas desulphurization product magnesium sulfite one-step method |
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| CN102976369A (en) * | 2012-11-12 | 2013-03-20 | 沈阳化工大学 | Method for preparing ultrafine magnesium hydroxide and basic magnesium sulfate whiskers from low-grade magnesite |
| US20140045982A1 (en) * | 2011-03-02 | 2014-02-13 | Ube Material Industries, Ltd. | Fibrous basic magnesium sulfate powder and method for producing same |
| CN105603504A (en) * | 2014-11-21 | 2016-05-25 | 合肥杰事杰新材料股份有限公司 | Method for preparing needle-like basic magnesium sulfate whiskers by ultrasonic assistance |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1536102A (en) * | 2003-04-10 | 2004-10-13 | 大连晶须材料有限公司 | Method for synthesizing magnesium salt whiskers |
| US20140045982A1 (en) * | 2011-03-02 | 2014-02-13 | Ube Material Industries, Ltd. | Fibrous basic magnesium sulfate powder and method for producing same |
| CN102976369A (en) * | 2012-11-12 | 2013-03-20 | 沈阳化工大学 | Method for preparing ultrafine magnesium hydroxide and basic magnesium sulfate whiskers from low-grade magnesite |
| CN105603504A (en) * | 2014-11-21 | 2016-05-25 | 合肥杰事杰新材料股份有限公司 | Method for preparing needle-like basic magnesium sulfate whiskers by ultrasonic assistance |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109797435A (en) * | 2017-11-17 | 2019-05-24 | 华东理工大学 | A kind of new method of low cost synthesis alkali magnesium sulfate crystal whisker |
| CN108002413A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | Salt lake puies forward the method for comprehensive utilization of lithium solid by-product |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN109879655A (en) * | 2019-04-09 | 2019-06-14 | 辽宁科大中驰镁建材科技有限公司 | A method of hydraulicity magnesite board is prepared based on medium temperature mould pressing process |
| CN109879655B (en) * | 2019-04-09 | 2022-01-25 | 辽宁科大中驰镁建材科技有限公司 | Method for preparing hydraulic magnesite process plate based on medium-temperature die pressing process |
| CN110436490A (en) * | 2019-08-06 | 2019-11-12 | 东北大学 | A method of magnesium oxysulfide short fiber material is prepared using magnesium method flue gas desulphurization product magnesium sulfite one-step method |
| CN110436490B (en) * | 2019-08-06 | 2020-10-30 | 东北大学 | Method for preparing magnesium oxysulfate short fiber material by using magnesium method flue gas desulfurization product magnesium sulfite one-step method |
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Application publication date: 20170322 |