Method for directly synthesizing basic magnesium sulfate whiskers by brine

A magnesium sulfate whisker and bittern technology, which is applied in the field of inorganic material preparation, can solve the problems of high raw material cost, unsuitability for industrial production, complex process, etc., and achieve low raw material price, high product purity and yield, and simple process steps Effect

Active Publication Date: 2011-04-06
TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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  • Abstract
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Problems solved by technology

[0010] Aiming at problems such as complex process, high raw material cost and unsuitability for industrialized production in the preparation of basic magnesium sulfate whiskers in the prior art, the present invention introduces the direct synthesis of alkali by using bittern after salt production, ammonia water and magnesium sulfate heptahydrate. A new method for formulating magnesium sulfate whiskers, which is convenient for industrial production

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  • Method for directly synthesizing basic magnesium sulfate whiskers by brine
  • Method for directly synthesizing basic magnesium sulfate whiskers by brine

Examples

Experimental program
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Embodiment 1

[0028] Take 2 liters of bittern, analyze to get SO 4 2- It is 58.06g / L, that is, a total of 1.21 moles of SO 4 2- , add 2.42L of 0.5mol / L calcium chloride solution, add 1.21 moles of calcium chloride in total, stir for 10 minutes, filter, and analyze to get Mg 2+ 18.23g / L, SO 4 2- It is 2.98g / L. Measure 1 liter of pretreated bittern and place it in a 3-liter high-pressure reactor, and use 2 times the magnesium ion (Mg) in the pretreated bittern 2+ ) Molar weight adds ammoniacal liquor (25%, m / m) namely 212.68g, with 2 times of magnesium ion (Mg 2+ ) molar amount of magnesium sulfate heptahydrate (98.13%, m / m) was added, namely 380.84g. Start stirring at 300 rpm, and raise the temperature to 160°C. Stop heating, continue stirring, constant temperature hydrothermal reaction for 8 hours, stop constant temperature. Then cool naturally to room temperature, move the basic magnesium sulfate whisker suspension prepared in the autoclave out of the autoclave, separate the solid...

Embodiment 2

[0030] Take 2 liters of bittern, analyze to get SO 4 2- It is 55.22g / L, that is, a total of 1.15 moles of SO 4 2- , add 2.3 L of 0.5mol / L calcium chloride solution, add 1.15 moles of calcium chloride in total, stir for 10 minutes, filter, and analyze to get Mg 2+ 17.28g / L, SO 4 2- It is 2.36g / L. Measure bittern after 1 liter of pretreatment and place it in 3 liters of high-pressure reactors, with 2.1 times of magnesium ion (Mg 2+ ) Molar weight adds ammoniacal liquor (25%, m / m) namely 211.68g, with 2.4 times of magnesium ion (Mg 2+ ) molar amount of magnesium sulfate heptahydrate (98.13%, m / m) that is 433.19g was added. Turn on stirring at 400 rpm, and raise the temperature to 150°C. Stop heating, continue stirring, constant temperature hydrothermal reaction for 6 hours, stop constant temperature. Then cool naturally to room temperature, move the basic magnesium sulfate whisker suspension prepared in the autoclave out of the autoclave, separate the solid from the liqu...

Embodiment 3

[0032] Take 2 liters of bittern, analyze to get SO 4 2- It is 57.21g / L, that is, 1.19 moles of SO 4 2- , add 2.38L of 0.5mol / L calcium chloride solution, add 1.19 moles of calcium chloride in total, stir for 10 minutes, filter, and analyze, Mg 2+ 17.92g / L, SO 4 2- It is 3.02g / L. Measure 1 liter of pretreatment bittern and be placed in 3 liters of pressure reactors, with 2.15 times the magnesium ion (Mg in the pretreatment bittern) 2+ ) Molar weight adds ammoniacal liquor (25%, m / m) i.e. 224.75g, with 2.6 times the magnesium ion (Mg in the pretreatment bittern) 2+ ) molar amount of magnesium sulfate heptahydrate (98.13%, m / m) was added, namely 486.67g. Turn on stirring at 450 rpm, and raise the temperature to 170°C. Stop heating, continue stirring, constant temperature hydrothermal reaction for 5 hours, stop constant temperature. Then cool naturally to room temperature, move the basic magnesium sulfate whisker suspension prepared in the autoclave out of the autoclave, ...

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Abstract

The invention discloses a method for directly synthesizing basic magnesium sulfate whiskers by brine. The brine after salt manufacturing, ammonia water and magnesium sulfate heptahydrate are taken as raw materials to synthesize the basic magnesium sulfate whiskers. The method comprises the following steps of: performing thermostatic hydrothermal reaction on the pretreated brine, ammonia water and magnesium sulfate heptahydrate in a high-pressure reaction kettle to prepare basic magnesium sulfate whisker suspension, wherein the molar ratio of magnesium ions (Mg2+) of the brine to the ammonia water (NH3.H2O) to magnesium sulfate (MgSO4.7H2O) in the reaction kettle is 1.0:2.0-2.2:2.0-3.0, the stirring speed is 300 to 500rpm, the temperature is raised to 120-200DEG C, and the reaction time is 4 to 8 hours; and performing solid-liquid separation on the basic magnesium sulfate whisker suspension, washing the solid with running water, and drying a filter cake obtained after washing to obtain the basic magnesium sulfate whisker product. The technological process is simple, the cost of raw materials is low, the energy consumption is low, the product purity and quality are high, and after the synthesized whiskers are added into a composite material taking rubber and plastics as a matrix, the composite material has good reinforced property and flame retardancy.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to a method for directly synthesizing basic magnesium sulfate whiskers by using bittern. Background technique [0002] Basic magnesium sulfate whiskers [5Mg(OH) 2 · MgSO 4 ·3H 2 O] is a needle-like single crystal material with high strength, low density and high elastic modulus, which can be used as a reinforcing and toughening agent for composite materials such as plastics, rubber and resins. The good electrical insulation properties of basic magnesium sulfate whiskers also make it play an important role in the field of cables. At the same time, since the basic magnesium sulfate whiskers lose the crystal water contained in them at 260°C and the hydroxyl water contained in them at 300°C, hydrolysis and dehydration will not occur under rubber and plastic processing conditions (<200°C). , Therefore, basic magnesium sulfate whiskers can not only be use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/46C30B29/62
Inventor 郭淑元张雨山黄西平张家凯董泽亮
Owner TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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