CN103803591B - The magnesian preparation method of a kind of ultralow bulk density - Google Patents
The magnesian preparation method of a kind of ultralow bulk density Download PDFInfo
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- CN103803591B CN103803591B CN201310733876.2A CN201310733876A CN103803591B CN 103803591 B CN103803591 B CN 103803591B CN 201310733876 A CN201310733876 A CN 201310733876A CN 103803591 B CN103803591 B CN 103803591B
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Abstract
The magnesian preparation method of a kind of ultralow bulk density, relates to nano magnesia.Preparation soluble magnesium salt brine solution and aqueous sodium hydroxide solution; Soluble magnesium salt brine solution is under agitation added in aqueous sodium hydroxide solution with constant speed; After reaction terminates, by the white precipitate washing obtained, centrifugal or filter, organic solvent soaks, guard aperture is dry; By the roasting of dried ultralow bulk density magnesium hydroxide white powder, obtain extremely-low density magnesium oxide.The ultralow bulk density magnesium oxide of preparation, its bulk density is less than 0.1g/ml, is especially less than 0.04g/ml.Be suitable as sorbent material, catalyzer and support of the catalyst, can be used for taking off ammonium dephosphorization etc. in flue gas desulfurization in inorganic combustion inhibitor, environmental protection, wastewater treatment, and press down in cigarette coating and biological and pharmaceutical preparation at acid rain soil remediation, food and fodder additives, oil dope, agricultural fertiliser containing magnesium, cigarette tissue, have broad application prospects in the field such as pottery, paint, medical science, microtronics.
Description
Technical field
The present invention relates to nano magnesia, especially relate to the magnesian preparation method of a kind of ultralow bulk density.
Background technology
Nano magnesia is a kind of Multifunction inorganic materials, has the specific function of the heat being different from bulk material, optical, electrical, mechanics and chemical aspect due to its grain refine.The nano magnesia performance that specific inductivity is low because having, thermal expansivity is high, makes it in microwave and the manufacture of photoelectric nano components and parts, have important using value.Magnesium oxide, because of in weakly alkaline, is widely used as catalyzer and carrier.Meanwhile, due to mgo surface there is a large amount of defect, limit, angle, step isoreactivity position make it can as the sorbent material of the compounds such as toxic and harmful and metal ion and chloride, phosphorus.The characteristic that magnesian low-temperature sintering is good makes it can as the sintering aid of high-grade ceramic and stablizer.
Compare with magnesium oxide prepared by ordinary method, ultralow bulk density magnesium oxide is dispersed better in the solution, have more effectively contact area, thus surfactivity is higher, catalysis and absorption property stronger.About magnesian drying means, conventional is vacuum-drying, and its maximum shortcoming is that sample easily lumps, and after grinding, product cut size is uneven, have impact on magnesian properties.[the Li Chunhu such as Li Chunhu, Zhao Jiusheng, Wang great Xiang etc. the UV absorber [J] of nano-MgO and MgAl2O4 spinel. Journal of Inorganic Materials, 1996,11 (3): 557 ?560] utilize Supercritical Ethanol dry technology to prepare the nano magnesia that bulk density is 0.2085g/ml, but its particle size distribution is uneven, loosely organized.[the Liu Xiaoming such as Liu Xiaoming, Yue Yanjun, Zhou Yingchun, Song Yanling. molten glue ?gel method prepares nano magnesia [J], Liaoning chemical industry, 2005,34(9): 380 ?381] utilize flowing nitrogen desiccating method dry hydrogen magnesium oxide alcogel, after roasting, obtain the less nano magnesia of particle diameter, time of drying, 5h, did not report about size and the concrete numerical value of bulk density.[the Suchada Utamapanya such as Suchada Utamapanya, Kenneth J.Klabunde, John R.Schlup, Chem.Mater., 1991,3,175 ?181] utilize magnesium methylate for presoma, make its Jia Chun ?toluene mixed solvent in be hydrolyzed, then by solvothermal to supercritical state, obtain dry sample after venting, obtain magnesium oxide through calcining.This method operating process more complicated, needs to carry out under the high temperature of 265 DEG C.King is precious and wait [Wang Baohe, Yu Caiyuan, Zhang Wenbo, Zhang Wei. all even heavy shallow lake ?supercritical co desiccating method prepares the method for nano magnesia, China, CN1597520,2005] precipitate under dispersion agent using urea, magnesium salts at polyoxyethylene glycol, sodium laurylsulfonate etc., and prepared nano magnesia through supercritical co drying.
In document and patent, so far there are no about the magnesian relevant report of the ultralow bulk density of preparation.
Summary of the invention
The object of the present invention is to provide the magnesian preparation method of a kind of ultralow bulk density.
The present invention includes following steps:
1) soluble magnesium salt brine solution and aqueous sodium hydroxide solution is prepared;
2) soluble magnesium salt brine solution is under agitation added in aqueous sodium hydroxide solution with constant speed;
3) after reaction terminates, by the white precipitate washing obtained, centrifugal or filter, organic solvent soaks, guard aperture is dry;
4) by the roasting of dried ultralow bulk density magnesium hydroxide white powder, extremely-low density magnesium oxide is obtained.
In step 1), optional any one in magnesium nitrate, magnesium chloride, magnesium sulfate etc. of described solubility magnesium salts; The concentration of described soluble magnesium salt brine solution can be 0.1 ~ 2.0mol/L, preferred 0.5mol/L; The temperature of described aqueous sodium hydroxide solution is between 25 ~ 100 DEG C, and the concentration of aqueous sodium hydroxide solution can be 0.2 ~ 4.0mol/L, preferred 1.0mol/L.
In step 2) in, the speed of described stirring can be 100 ~ 600r/min, preferred 400r/min; The described equipment added in aqueous sodium hydroxide solution can adopt syringe pump or other suitable equipment, and the injection needles diameter of described syringe pump can be 0.45 ~ 4mm, preferred 1.2mm; The described speed added in aqueous sodium hydroxide solution can be 50 ~ 400ml/h, preferred 200ml/h, and the pH of reaction system can be 11 ~ 12.
In step 3), described organic solvent can be selected from the one in methyl alcohol, ethanol, Virahol etc., preferred alcohol; Described guard aperture drying can adopt vacuum-drying, lyophilize, spraying dry or supercritical drying etc., the preferred supercritical co of described supercritical drying is dry, temperature in described supercritical co drying process can be 35 ~ 80 DEG C, preferably 60 DEG C, pressure is 8 ~ 30MPa, preferred 15MPa, time of drying is 0.5 ~ 3h, preferred 1h.
In step 4), described dried ultralow bulk density magnesium hydroxide white powder, its bulk density is less than its bulk density and is less than 0.1g/ml, is especially less than 0.04g/ml; Described roasting, the roasting in retort furnace of magnesium hydroxide white powder can be obtained ultralow bulk density magnesium hydroxide, the temperature of roasting can be 500 ~ 900 DEG C, preferably 600 DEG C.
Ultralow bulk density magnesium oxide prepared by the present invention, its bulk density is less than 0.1g/ml, is especially less than 0.04g/ml.
The present invention take water as solvent, and using solubility magnesium salts as magnesium source, sodium hydroxide is precipitation agent.
The magnesium oxide of ultralow bulk density prepared by the present invention is suitable as sorbent material, catalyzer and support of the catalyst, can be used for taking off ammonium dephosphorization etc. in flue gas desulfurization in inorganic combustion inhibitor, environmental protection, wastewater treatment, and the application all had in cigarette coating and biological and pharmaceutical preparation is in various degree pressed down at acid rain soil remediation, food and fodder additives, oil dope, agricultural fertiliser containing magnesium, cigarette tissue, also can be used as catalyzer or support of the catalyst, and have broad application prospects in the field such as pottery, paint, medical science, microtronics.
The present invention has the following advantages: (1) the present invention adopts raw material cheap and easy to get, does not need to add template; (2) process adopts syringe pump or relevant device to control, and reaches the object facilitating control ph with its flow velocity, and without the need to additional acid alkali reagent again, obtains suitable preparation condition; (3) magnesium oxide prepared by and magnesium hydroxide do not lump, and bulk density is extremely low, not yet have document openly to report magnesium oxide and the magnesium hydroxide of so low bulk density.
Accompanying drawing explanation
Fig. 1 is the magnesian XRD spectra obtained after the XRD spectra of the magnesium hydroxide that in the present invention, embodiment 1 obtains and roasting thereof.
Fig. 2 is the magnesian transmission electron microscope photo of ultralow bulk density prepared by the embodiment of the present invention 1.
Fig. 3 is the magnesian transmission electron microscope local pictures of ultralow bulk density prepared by the embodiment of the present invention 1.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
Embodiment 1
The magnesium nitrate aqueous solution of preparation 0.5mol/L, the sodium hydroxide solution of 1mol/L, under room temperature, with 50ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is that the white precipitate deionized water obtained is cleaned by 500r/min., centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then passes into supercritical co, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 15L/h, runs 1h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0327g/ml.By the roasting of gained white powder, obtaining its bulk density of magnesium oxide powder is 0.0342g/ml.
Embodiment 2
The magnesium nitrate aqueous solution of preparation 0.5mol/L, the sodium hydroxide solution of 1mol/L, get 50ml sodium hydroxide solution heating in water bath to 100 DEG C, with 200ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is 500r/min, the white precipitate deionized water obtained is cleaned, centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then supercritical co is passed into, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 30L/h, runs 1h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0244g/ml.By the roasting of gained white powder, obtain magnesium oxide, its bulk density is 0.0284g/ml.
Embodiment 3
The magnesium chloride brine of preparation 1.0mol/L, the sodium hydroxide solution of 2.0mol/L, get 25ml sodium hydroxide solution heating in water bath to 100 DEG C, with 400ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is 500r/min, the white precipitate deionized water obtained is cleaned, centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then supercritical co is passed into, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 30L/h, runs 1.5h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0335g/ml.By the roasting of gained white powder, obtain magnesium oxide, its bulk density is 0.0363g/ml.
Embodiment 4
The magnesium nitrate aqueous solution of preparation 0.5mol/L, the sodium hydroxide solution of 1mol/L, get 50ml sodium hydroxide solution heating in water bath to 100 DEG C, with 200ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is 500r/min, the white precipitate deionized water obtained is cleaned, centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then supercritical co is passed into, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 40L/h, runs 1.5h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0314g/ml.By the roasting of gained white powder, obtain magnesium oxide, its bulk density is 0.0336g/ml.
Embodiment 5
The magnesium nitrate aqueous solution of preparation 0.5mol/L, the sodium hydroxide solution of 1mol/L, get 50ml sodium hydroxide solution heating in water bath to 100 DEG C, with 200ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is 500r/min, the white precipitate deionized water obtained is cleaned, centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then supercritical co is passed into, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 60L/h, runs 2h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0164g/ml.By the roasting of gained white powder, obtain magnesium oxide, its bulk density is 0.0171g/ml.
Embodiment 6
The magnesium nitrate aqueous solution of preparation 0.5mol/L, the sodium hydroxide solution of 1mol/L, get 50ml sodium hydroxide solution heating in water bath to 75 DEG C, with 400ml/h speed, magnesium nitrate solution is added drop-wise in sodium hydroxide solution with syringe pump, stirring velocity is 500r/min, the white precipitate deionized water obtained is cleaned, centrifugal, centrifugal gained white precipitate ethanol is washed twice, then the ethanol homogenate that gained precipitates is added in supercritical drying still, still is heated to 60 DEG C, then supercritical co is passed into, maintaining still internal pressure is 15MPa, open purging valve, regulate CO
2flow is 60L/h, runs 1.5h, and take out gained magnesium hydroxide white powder, its bulk density is 0.0235g/ml.By the roasting of gained white powder, obtain magnesium oxide, its bulk density is 0.0262g/ml.
Claims (11)
1. the magnesian preparation method of ultralow bulk density, is characterized in that comprising the steps:
1) soluble magnesium salt brine solution and aqueous sodium hydroxide solution is prepared; The concentration of described soluble magnesium salt brine solution is 0.1 ~ 2.0mol/L, and the temperature of described aqueous sodium hydroxide solution is between 25 ~ 100 DEG C, and the concentration of aqueous sodium hydroxide solution is 0.2 ~ 4.0mol/L;
2) soluble magnesium salt brine solution is under agitation added in aqueous sodium hydroxide solution with constant speed; The speed of described stirring is 100 ~ 600r/min; The described equipment added in aqueous sodium hydroxide solution adopts syringe pump; The injection needles diameter of described syringe pump is 0.45 ~ 4mm, described in the speed added in aqueous sodium hydroxide solution be 50 ~ 400mL/h; The pH of reaction system is 11 ~ 12;
3) after reaction terminates, by the white precipitate washing obtained, centrifugal or filter, organic solvent soaks, guard aperture is dry; Described organic solvent is selected from the one in methyl alcohol, ethanol, Virahol; Described guard aperture drying adopts vacuum-drying, lyophilize, spraying dry or supercritical drying;
4) by the roasting of dried ultralow bulk density magnesium hydroxide white powder, obtain extremely-low density magnesium oxide, described dried ultralow bulk density magnesium hydroxide white powder, its bulk density is less than 0.1g/mL.
2. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 1) in, described solubility magnesium salts be selected from magnesium nitrate, magnesium chloride, magnesium sulfate any one.
3. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 1) in, the concentration of described soluble magnesium salt brine solution is 0.5mol/L; The temperature of described aqueous sodium hydroxide solution is between 25 ~ 100 DEG C, and the concentration of aqueous sodium hydroxide solution is 1.0mol/L.
4. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 2) in, the speed of described stirring is 400r/min.
5. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 2) in, the injection needles diameter of described syringe pump is 1.2mm; The described speed added in aqueous sodium hydroxide solution is 200mL/h.
6. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 3) in, described organic solvent is ethanol.
7. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, it is characterized in that in step 3) in, described supercritical drying adopts supercritical co dry, temperature in described supercritical co drying process is 35 ~ 80 DEG C, pressure is 8 ~ 30MPa, and time of drying is 0.5 ~ 3h.
8. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 7, it is characterized in that the temperature in described supercritical co drying process is 60 DEG C, pressure is 15MPa, and time of drying is 1h.
9. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, is characterized in that in step 4) in, described bulk density is less than 0.04g/mL.
10. the magnesian preparation method of a kind of ultralow bulk density as claimed in claim 1, it is characterized in that in step 4) in, described roasting, be that the roasting in retort furnace of magnesium hydroxide white powder is obtained ultralow bulk density magnesium hydroxide, the temperature of roasting is 500 ~ 900 DEG C.
11. magnesian preparation methods of a kind of ultralow bulk density as claimed in claim 10, is characterized in that the temperature of described roasting is 600 DEG C.
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| CN110745926A (en) * | 2019-11-14 | 2020-02-04 | 北京环球中科水务科技有限公司 | Preparation method of coagulant for removing phosphorus in water body |
| CN113184883A (en) * | 2021-05-11 | 2021-07-30 | 青海施丹弗化工有限责任公司 | Method for continuously producing nano magnesium oxide |
| CN114291832B (en) * | 2021-12-31 | 2024-01-30 | 青海创信电子材料有限公司 | Preparation method of magnesium hydroxide |
| CN115353130A (en) * | 2022-08-26 | 2022-11-18 | 广西博世科环保科技股份有限公司 | Preparation method of defluorination nano magnesium oxide |
Citations (2)
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|---|---|---|---|---|
| CN1037690A (en) * | 1988-05-16 | 1989-12-06 | 上海敦煌化工厂 | Method of fabricating magnesium oxide |
| CN101348937A (en) * | 2008-09-05 | 2009-01-21 | 清华大学 | Preparation of high length-diameter ratio magnesium hydroxide sulfate hydrate whisker |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037690A (en) * | 1988-05-16 | 1989-12-06 | 上海敦煌化工厂 | Method of fabricating magnesium oxide |
| CN101348937A (en) * | 2008-09-05 | 2009-01-21 | 清华大学 | Preparation of high length-diameter ratio magnesium hydroxide sulfate hydrate whisker |
Non-Patent Citations (1)
| Title |
|---|
| 纳米氧化镁的制备;郭英凯 等;《化学工程》;20070630;第35卷(第6期);第70-73页 * |
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