CN103936039B - A kind of method adopting dry powder sodium carbonate directly to prepare Stan-Mag Magnesium Carbonate - Google Patents
A kind of method adopting dry powder sodium carbonate directly to prepare Stan-Mag Magnesium Carbonate Download PDFInfo
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- CN103936039B CN103936039B CN201410185301.6A CN201410185301A CN103936039B CN 103936039 B CN103936039 B CN 103936039B CN 201410185301 A CN201410185301 A CN 201410185301A CN 103936039 B CN103936039 B CN 103936039B
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Abstract
The invention discloses a kind of method adopting dry powder sodium carbonate directly to prepare Stan-Mag Magnesium Carbonate, it is the bittern (MgCl of 15%-30% (W/V) by concentration
2), be heated to 90-98 DEG C, with 60-80 rev/min, stir lower gradation and add solid sodium carbonate gradually, feed time continues 1.5-3 hour, continues reacting by heating 30-60 minute, filtered while hot, the crystallization obtained after washing dries 2-3 hour at 100 DEG C, obtains content of magnesia 40.3%, the Stan-Mag Magnesium Carbonate of tap density 0.48-0.56g/mL.In 15%-30% (W/V) bittern, the mol ratio of magnesium dichloride and solid sodium carbonate is 1:0.7-0.9.Aqueous sodium carbonate changes into and directly uses dry powder sodium carbonate by the present invention, so just can omit the operation and equipment of dissolving sodium carbonate, makes reaction become more simple, and tap density can be made to improve; Make conversion unit be simplified to greatest extent, quality product improves simultaneously.
Description
Technical field
The invention belongs to technical field of medicine synthesis, relate to the preparation method of Stan-Mag Magnesium Carbonate, is a kind of method that novel employing dry powder sodium carbonate directly prepares Stan-Mag Magnesium Carbonate in particular.
Background technology
At present, domestic every profession and trade is to the aggregate demand of various magnesium salts at about 400,000 tons, and wherein the industry such as plastics, rubber, papermaking needs Magnesium Carbonate Light 41-45 8-15 ten thousand tons, and at the consumption of Ceramics Enterprises more than 30,000 tons, other industry needs various magnesium salts 15-25 ten thousand tons.Country is annual simultaneously also will to external exit portion magnesium salts product.The import price of magnesiumcarbonate is about 1700 dollars, and export price is only more than 600 dollar, and this illustrates that the magnesium products class that China produces is lower, and high-grade product still needs import.Magnesium Carbonate Light 41-45 is mainly used in plastics, rubber, building, the fields such as food-processing; Stan-Mag Magnesium Carbonate is then mainly used in medicine industry and foodstuffs industry, is used for the treatment of the treatment of the illnesss such as gastric and duodenal ulcer, is one of important component of foodstuff additive.
The most direct method of production of magnesiumcarbonate has two kinds, and one utilizes solid magnesium ore deposit (as rhombspar, the U.S. stone of water chestnut, magnesia etc.) to be sintered into light calcined magnesia, and the latter is through aquation purification processes, and then magnesiumcarbonate is prepared in charing; Another kind method is raw material with bittern, magnesiumcarbonate is prepared by ammonium carbonate method, Method of Soda, ammonia process-charring. a kind of front method utilizes land magnesium ore resources, a kind of rear method is then utilize seawater resources, manufacturing enterprise produces according to residing geographical position or any method of source resource situation Selection utilization, and the magnesiumcarbonate as West Europe 70% is raw material production by rhombspar; The largest production state of magnesiumcarbonate is produced for Russia with magnisite.The shortcoming of above-mentioned two kinds of methods is that technique is relatively loaded down with trivial details, and required equipment is more, and in production, corresponding cost of labor also can increase.
Bittern-Method of Soda prepares Stan-Mag Magnesium Carbonate, is to carry out precipitin reaction, filtration washing after first bittern and aqueous sodium carbonate being carried out pre-treatment, dehydration, the operation such as to dry, pulverize and produces Stan-Mag Magnesium Carbonate.Peng Juhua, Feng Baihu. the preparation of food grade Stan-Mag Magnesium Carbonate. Huaihai Institute of Technology journal, 2004,13(3): 54-56.Its shortcoming is that technique is relatively loaded down with trivial details, and required equipment is more, and in production, corresponding cost of labor also can increase.
Summary of the invention
The invention discloses a kind of method adopting dry powder sodium carbonate directly to prepare Stan-Mag Magnesium Carbonate, it is that (bittern is the by product after seawater produces sodium-chlor to 15%-30% (W/V) bittern, containing magnesium dichloride MgCl by concentration
2reaction of the present invention is in fact the replacement(metathesis)reaction of magnesium dichloride in bittern and sodium carbonate), be heated to 90-98 DEG C, stir lower gradation and add solid sodium carbonate gradually, feed time continues 1.5-3 hour, continue reacting by heating 30-60 minute, filtered while hot, the crystallization obtained after washing dries 2-3 hour at 100 DEG C, obtain content of magnesia 40.3%, the Stan-Mag Magnesium Carbonate of tap density 0.48-0.56g/mL; Wherein in 15%-30% (W/V) bittern, the mol ratio of magnesium dichloride and solid sodium carbonate is 1:0.7-0.9.
The concentration of bittern of the present invention is at 15%-30% (W/V), and preferred bittern concentration is 20%-25% (W/V), and most preferred bittern concentration is 22.5%.
MgCl in 2.5% bittern (W/V)
2be 1:0.8 with the mol ratio of solid sodium carbonate; Preferred temperature of reaction is 90-95 DEG C.
Gradation of the present invention is reinforced to be referred to: add a defective material after certain interval of time, as added once for 10-15 minute.Also can add once for 15 minutes
The tap density of Magnesium Carbonate Light 41-45 is generally about 0.15g/ml, and the tap density of Stan-Mag Magnesium Carbonate is generally about 0.6g/mL.No matter be Magnesium Carbonate Light 41-45 or Stan-Mag Magnesium Carbonate, stable tap density is all a very important product index.Stan-Mag Magnesium Carbonate production difficulty is larger, and quality product requires higher, and price is also more expensive.Due to Magnesium Carbonate Light 41-45 and Stan-Mag Magnesium Carbonate can not be distinguished from molecular formula and assay aspect, so product tap density just becomes the important evidence which kind of magnesiumcarbonate differentiation is. utilize reaction conditions to become to the tap density affecting magnesiumcarbonate the common method that scientific worker studies lightweight or Stan-Mag Magnesium Carbonate.
Bittern reacts from sodium carbonate also can produce Magnesium Carbonate Light 41-45 when condition is different, and this just controls relevant with reaction conditions.Temperature controls, concentration controls, order of addition(of ingredients), reaction times etc. all produces great effect to producing any magnesiumcarbonate. and Peng Juhua etc. have studied the processing condition that bittern and aqueous sodium carbonate method produce Stan-Mag Magnesium Carbonate, find that the tap density impact of material concentration (comprising bittern concentration and concentration of sodium carbonate) on product is very large: when MgCl2 concentration is at 0.8mol/L, aqueous sodium carbonate concentration is when 0.9mol/L, and product tap density is the highest; Temperature of reaction also has impact to tap density, and when 90 DEG C, the tap density of product is the highest; When the impact in reaction times is then reaction aging 3h, tap density is the highest.
Method of the present invention and aforesaid method distinguish to be it is not use aqueous sodium carbonate, but directly use carbon element sodium solid particulate.Due to the difference of solid particulate and the aqueous solution, so the factor affecting product tap density is also not quite similar.
High spot reviews of the present invention reactant concn, stirring velocity, feed way pile up close impact to product, and to affect result please see the following form:
The impact of processing condition change on Stan-Mag Magnesium Carbonate tap density
Conclusion:
(1) when bittern concentration is large, magnesiumcarbonate tap density increases, and tend to Stan-Mag Magnesium Carbonate future development, but the sodium carbonate comprised in product increases, and causes washing lotion alkalescence to cross and washs by force and not easily.
(2) when rotating speed is fast, tap density is low, tends to Magnesium Carbonate Light 41-45 future development; When rotating speed is slow, tap density is high; Tend to Stan-Mag Magnesium Carbonate future development.
(3) adopt gradation feed way that tap density can be made to increase by about 0.05 (gradation is reinforced can accomplish more than 0.48, only has about 0.4 before this), tend to Stan-Mag Magnesium Carbonate future development.
Aqueous sodium carbonate changes into and directly uses dry powder sodium carbonate by the present invention, so just can eliminate the operation and equipment of dissolving sodium carbonate, makes reaction become more simple, and tap density can be made to improve.
The content of the present invention to prepared Stan-Mag Magnesium Carbonate measures, and its method is as follows:
Get these product and be about 1g, accurately weighed, the 5ml that adds water makes moistening, and after precision adds sulfuric acid titrating solution (0.5mol/L) 30ml dissolving, methylate orange indicating liquid 1, with sodium hydroxide titration liquid (1mol/L) titration; From the volume (ml) consuming sulfuric acid titrating solution (0.5mol/L), deduct the volume (ml) that the calcium oxide that is mixed with should consume, calculate.Every 1ml sulfuric acid titrating solution (0.5mol/L) is equivalent to the CaO of MgO or 28.04mg of 20.15mg.
The measuring method of Stan-Mag Magnesium Carbonate tap density prepared by the present invention:
Get a clean 50mL graduated cylinder, precise is W1, at the uniform velocity adds testing sample to about 40mL, and again weighing graduated cylinder weight, is W2; The volume of tap density=W2-W1/ sample).
The positively effect that Stan-Mag Magnesium Carbonate preparation method disclosed in this invention is compared with prior art had is:
(1) operation of dissolved solids sodium carbonate and heating sodium carbonate liquid is saved
(2) save the equipment of dissolved solids sodium carbonate, conversion unit is simplified to greatest extent.
(3) the Stan-Mag Magnesium Carbonate tap density that the present invention produces can arrive 0.54g/mL, meets the needs of outlet.
Embodiment
In order to explain enforcement of the present invention more fully, provide following preparation method's embodiment.These embodiments are only explain instead of limit the scope of the invention.Wherein reacting the bittern used has commercially available.
Embodiment 1
In a 500mL there-necked flask, add the bittern 300mL that MgCl2 concentration is 15% (W/V), reacting by heating liquid to 90 DEG C, under slow stirring, (70 revs/min) add solid sodium carbonate by few gradation at the most, finally control pH is 7, solid sodium carbonate consumption is 35g, and feed time continues 1.5 hours.Continue reacting by heating 30 minutes, filtered while hot, a large amount of deionized water wash, the crystallization obtained is dried 2 hours at 100 DEG C.Stan-Mag Magnesium Carbonate must measure 24.2g, and yield 78.4%(is in sodium carbonate), content of magnesia 40.5%, tap density 0.42g/mL.MgCl2 wherein in 15% bittern (W/V) and the mol ratio of solid sodium carbonate are 1:0.7.
Embodiment 2
In a 500mL there-necked flask, adding MgCl2 concentration is 22.5% (W/V) bittern 200mL, reacting by heating liquid to 94 DEG C, under slow stirring, (60 revs/min) add solid sodium carbonate by few gradation at the most, finally control pH is 7.2, solid sodium carbonate consumption is 40g, feed time continues 2.5 hours, continues reacting by heating 60 minutes, filtered while hot, a large amount of deionized water wash, the crystallization obtained is dried 3 hours at 100 DEG C, and Stan-Mag Magnesium Carbonate must measure 26.8g, and yield 75.8%(is in sodium carbonate), content of magnesia 40.3%, tap density 0.56g/mL.MgCl2 wherein in 22.5% bittern (W/V) and the mol ratio of solid sodium carbonate are 1:0.8.
Embodiment 3
In a 500mL there-necked flask, adding MgCl2 concentration is 30% (W/V) bittern 150mL, reacting by heating liquid to 98 DEG C, with 80 revs/min, stir lower gradation and add solid sodium carbonate gradually, finally control pH is 7.5, and solid sodium carbonate consumption is 45g, and feed time continues 3 hours, continue reacting by heating 45 minutes, filtered while hot, a large amount of deionized water wash, the crystallization obtained is dried 3 hours at 100 DEG C, Stan-Mag Magnesium Carbonate must measure 37.3g, yield 94.0%(is in sodium carbonate), content of magnesia 35.5 %, tap density 0.51g/mL.MgCl2 wherein in 30% bittern (W/V) and the mol ratio of solid sodium carbonate are 1:0.9.
Claims (2)
1. the preparation method of a Stan-Mag Magnesium Carbonate, it is characterized in that it is is the bittern of 15%-30% (W/V) by concentration, be heated to 90-98 DEG C, with 60-80 rev/min, stir lower gradation and add solid sodium carbonate gradually, feed time continues 1.5-3 hour, continue reacting by heating 30-60 minute, filtered while hot, 2-3 hour is dried in the crystallization obtained after washing, obtain content of magnesia 40.3%, the Stan-Mag Magnesium Carbonate of tap density 0.48-0.56g/mL; Wherein in 15%-30% (W/V) bittern, the mol ratio of magnesium dichloride and solid sodium carbonate is 1:0.7-0.9.
2. preparation method according to claim 1, wherein said bittern concentration is 20%-25% (W/V); Temperature of reaction is 90-95 DEG C, reaction times 2-2.5 hour, the MgCl in 20% bittern (W/V)
2be 1:0.8 with the mol ratio of solid sodium carbonate.
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