CN109775734A - A kind of preparation method of low specific surface area basic magnesium carbonate - Google Patents
A kind of preparation method of low specific surface area basic magnesium carbonate Download PDFInfo
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- CN109775734A CN109775734A CN201910156123.7A CN201910156123A CN109775734A CN 109775734 A CN109775734 A CN 109775734A CN 201910156123 A CN201910156123 A CN 201910156123A CN 109775734 A CN109775734 A CN 109775734A
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Abstract
The invention discloses a kind of preparation methods of low specific surface area basic magnesium carbonate, are related to technical field of inorganic material.The present invention is reacted by urea with magnesium ion or magnesium hydroxide, and specific surface area is made and is less than 5m2The basic magnesium carbonate of/g solves basic magnesium carbonate because specific surface area is excessive and is difficult to the technical issues of adding in the polymer, while overcoming the deficiencies of blanking of the basic magnesium carbonate powder in adding procedure is difficult；Product of the present invention purity is high, preparation process is simple and environmentally-friendly, at low cost easy to industrialized production.
Description
Technical field:
The present invention relates to technical field of inorganic material, and in particular to a kind of preparation side of low specific surface area basic magnesium carbonate
Method.
Background technique:
Basic magnesium carbonate is a kind of efficient inorganic fire-retarded filler.It can be released during polymer combustion is decomposed
Vapor and carbon dioxide are released, the concentration of fuel gas on the one hand can be diluted, on the other hand can reduce the temperature of comburant
Degree, to play fire-retardant effect.Compared with common inorganic fire-retarded filler, the biggest advantage of basic magnesium carbonate is that it is total
Thermal weight loss can achieve 56%, and total thermal weight loss of aluminium hydroxide is 33.4%, and total thermal weight loss of magnesium hydroxide is then 30%.
In the case of identical adding proportion, the fire-retardant gas that basic magnesium carbonate can release is more, therefore has better fire-retardant effect
Fruit.
The synthetic method of common basic magnesium carbonate: with the side of the alkali solution precipitates magnesium chloride such as sodium carbonate or sodium bicarbonate
Method.However, the basic magnesium carbonate for the method synthesis being somebody's turn to do, has the shortcomings that large specific surface area, the specific surface area of product obtained
It puts down in 40~70m2/g。
In the polymer, the specific surface area of inorganic particle crosses conference and limits its additive amount in the polymer significantly.And
And the excessive specific surface area of inorganic particle can bring too low bulk specific weight, so that inorganic particle brings blanking in adding procedure
The inconvenience such as difficulty.
Summary of the invention:
Technical problem to be solved by the present invention lies in a kind of preparation method for the basic magnesium carbonate for providing low specific surface area,
Specifically, specific surface area is less than 5m2The preparation method of the basic magnesium carbonate of/g.
The following technical solution is employed for the technical problems to be solved by the invention to realize:
A kind of preparation method of basic magnesium carbonate, the specific method is as follows: in the magnesium that magnesium ion concentration is 0.5~2mol/L
Salting liquid is dispersed in water addition urea in the magnesium hydroxide slurry that concentration is 0.5~2mol/L and dissolves, then will dissolution
Solution afterwards is added in the hydrothermal reaction kettle of teflon lined, hydro-thermal insulation reaction, the slurry after reaction through over cleaning,
It filters, be dried to obtain specific surface area less than 5m2The molar ratio of the basic magnesium carbonate powder of/g, urea and magnesium ion is 1:1~1:
2。
The magnesium salts is selected from one or more of soluble magnesium salts such as magnesium chloride, magnesium nitrate, magnesium sulfate.
In the magnesium hydroxide slurry, the median of magnesium hydroxide is 0.1~10um.
Preferably 120~150 DEG C of the hydrothermal temperature.
The hydro-thermal insulation reaction time preferably 6~10h.
Sodium carbonate or sodium bicarbonate alkali is added in the synthetic method of common basic magnesium carbonate such as in magnesium chloride solution
Property solution makes magnesium ion and carbonate and the hydroxyl in conjunction with preparing.In the preparation process, the precipitating of magnesium ion is rapid
, therefore the crystal grain of reaction product has little time to grow, product is the aggregation of tiny laminar basic magnesium carbonate, such as Fig. 1 institute
Show, therefore there is big specific surface area.
Principle according to the present invention are as follows: urea can split the carbon dioxide off at 80 degrees Celsius or more and ammonia, ammonia are molten
A large amount of hydroxyl is separated out in water power, carbon dioxide can also be dissolved in this alkaline solution.Magnesium ion or magnesium hydroxide are in this alkali
Property in the environment of meeting and dissolution carbon dioxide and hydroxyl combine generate basic magnesium carbonate.Present inventor has found in an experiment,
Ratio can be made by the suitable magnesium salts of control or the concentration ratio of magnesium hydroxide and urea, and suitable hydrothermal temperature and time
Surface area is less than 5m2The basic magnesium carbonate of/g.
The beneficial effects of the present invention are: the present invention is reacted by urea with magnesium ion or magnesium hydroxide, specific surface is made
Product is less than 5m2The basic magnesium carbonate of/g solves basic magnesium carbonate and is difficult to add in the polymer because specific surface area is excessive
Technical problem, while overcoming the deficiencies of blanking of the basic magnesium carbonate powder in adding procedure is difficult；Product of the present invention purity
Height, preparation process is simple and environmentally-friendly, at low cost easy to industrialized production.
Detailed description of the invention:
Fig. 1 is that the SEM of 1 gained powder body material of embodiment schemes；
Fig. 2 for embodiment 2 powder body material SEM figure；
Fig. 3 for embodiment 3 powder body material X-RD figure；
Fig. 4 for embodiment 4 powder body material TG figure.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
Magnesium chloride 9.5g is added in tri- mouthfuls of beakers of the 250ml being placed in 60 degrees Celsius of bath temperature, distilled water is added
95g, stirring dissolve it all.The sodium carbonate liquor that 100ml concentration is 1mol/l is added, continues stirring 2 hours, is pasted
Shape product.Product is cleaned with deionized water to conductivity and is less than 30us/cm, then product is filtered, drying, finished product is obtained
6.8g, reaction yield 94.3%, test specific surface area are 45m2/g.Fig. 1 is the product that embodiment 1 obtains, and is tiny thin slice
Condensate.
Embodiment 2
Magnesium chloride 9.5g, urea 6g, it is 100 milliliters that distilled water to liquor capacity, which is added, and stirring dissolves solute all.It takes
Solution 80g is poured into the hydrothermal reaction kettle of the teflon lined of 100ml, and reaction kettle is placed in baking oven, and reaction temperature is set
It is 120 degrees Celsius, soaking time 6 hours fixed.After reaction, reactant is poured out, is cleaned with deionized water to conductivity and is less than
30us/cm, then by product suction filtration, drying, finished product 6.8g, reaction yield 92.3% are obtained, test specific surface area is 4.5m2/
g.Fig. 2 is the product that embodiment 2 obtains, to crystallize perfect plate body.
Embodiment 3
Magnesium nitrate 7.4g, urea 4.5g, it is 100 milliliters that distilled water to liquor capacity, which is added, and stirring dissolves solute all.
It takes solution 80g to pour into the hydrothermal reaction kettle of the teflon lined of 100ml, reaction kettle is placed in baking oven, reaction temperature
130 degrees Celsius, soaking time 8 hours of setting.After reaction, reactant is poured out, is cleaned with deionized water small to conductivity
In 30us/cm, then by product suction filtration, drying, finished product 6.9g, reaction yield 93.8% are obtained, test specific surface area is
3.9m2/g.Fig. 3 is the X diffraction pattern for the product that embodiment 3 obtains.
Embodiment 4
Magnesium sulfate 24g, urea 24g, it is 100 milliliters that distilled water to liquor capacity, which is added, and stirring dissolves solute all.It takes
Solution 80g is poured into the hydrothermal reaction kettle of the teflon lined of 100ml, and reaction kettle is placed in baking oven, and reaction temperature is set
It is 150 degrees Celsius, soaking time 10 hours fixed.After reaction, reactant is poured out, is cleaned with deionized water to conductivity and is less than
30us/cm, then by product suction filtration, drying, finished product 7.1g, reaction yield 96% are obtained, test specific surface area is 3.5m2/g。
Fig. 4 is the TG figure for the product that embodiment 4 obtains.
Embodiment 5
Median is magnesium hydroxide 5.8, the urea 12g of 3um, and it is 100 milliliters that distilled water to liquor capacity, which is added, is stirred
Mixing dissolves solute all.It takes solution 80g to pour into the hydrothermal reaction kettle of the teflon lined of 100ml, reaction kettle is set
In baking oven, reaction temperature sets 130 degrees Celsius, soaking time 10 hours.After reaction, reactant is poured out, spend from
Sub- water, which is cleaned to conductivity, is less than 30us/cm, then product is filtered, drying, obtains finished product 7.1g, reaction yield 96% is surveyed
Examination specific surface area is 1.6 m2/g。
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (5)
1. a kind of preparation method of low specific surface area basic magnesium carbonate, which is characterized in that the specific method is as follows: in magnesium ion concentration
For 0.5~2mol/L magnesium salt solution or to be dispersed in water concentration be that urea is added in the magnesium hydroxide slurry of 0.5~2mol/L
And dissolve, then dissolved solution is added in the hydrothermal reaction kettle of teflon lined, hydro-thermal insulation reaction, is reacted
Slurry afterwards is through over cleaning, the basic magnesium carbonate powder for filtering, being dried to obtain specific surface area less than 5m2/g, urea and magnesium ion
Molar ratio be 1:1~1:2.
2. the preparation method of low specific surface area basic magnesium carbonate according to claim 1, it is characterised in that: the magnesium salts
Selected from one or more of soluble magnesium salts such as magnesium chloride, magnesium nitrate, magnesium sulfate.
3. the preparation method of low specific surface area basic magnesium carbonate according to claim 1, it is characterised in that: the hydrogen-oxygen
The median for changing magnesium hydroxide in magnesium slurry is 0.1~10um.
4. the preparation method of low specific surface area basic magnesium carbonate according to claim 1, it is characterised in that: the hydro-thermal temperature
Preferably 120~150 DEG C of degree.
5. the preparation method of low specific surface area basic magnesium carbonate according to claim 1, it is characterised in that: the hydro-thermal is protected
Preferably 6~10h of warm reaction time.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110937615A (en) * | 2019-12-13 | 2020-03-31 | 江苏师范大学 | Synthesis method of basic magnesium carbonate ultrathin nanosheets |
| CN112479237A (en) * | 2020-12-08 | 2021-03-12 | 华东理工大学 | Method for preparing anhydrous magnesium carbonate by directly utilizing salt lake brine |
| CN112794349A (en) * | 2021-01-14 | 2021-05-14 | 江西理工大学 | Method for preparing anhydrous magnesium carbonate by hydrothermal method of large-particle-size magnesium oxide |
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| CN102897805A (en) * | 2012-09-17 | 2013-01-30 | 安徽中医学院 | Preparation method of one-dimensional basic magnesium carbonate nano wire and porous magnesium oxide nano wire |
| CN104495884A (en) * | 2014-11-21 | 2015-04-08 | 河北科技大学 | Basic magnesium carbonate and preparation method thereof |
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| CN102897805A (en) * | 2012-09-17 | 2013-01-30 | 安徽中医学院 | Preparation method of one-dimensional basic magnesium carbonate nano wire and porous magnesium oxide nano wire |
| CN104495884A (en) * | 2014-11-21 | 2015-04-08 | 河北科技大学 | Basic magnesium carbonate and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110937615A (en) * | 2019-12-13 | 2020-03-31 | 江苏师范大学 | Synthesis method of basic magnesium carbonate ultrathin nanosheets |
| CN112479237A (en) * | 2020-12-08 | 2021-03-12 | 华东理工大学 | Method for preparing anhydrous magnesium carbonate by directly utilizing salt lake brine |
| CN112794349A (en) * | 2021-01-14 | 2021-05-14 | 江西理工大学 | Method for preparing anhydrous magnesium carbonate by hydrothermal method of large-particle-size magnesium oxide |
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