CN102275958A - Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material - Google Patents
Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material Download PDFInfo
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- CN102275958A CN102275958A CN2011102156650A CN201110215665A CN102275958A CN 102275958 A CN102275958 A CN 102275958A CN 2011102156650 A CN2011102156650 A CN 2011102156650A CN 201110215665 A CN201110215665 A CN 201110215665A CN 102275958 A CN102275958 A CN 102275958A
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Abstract
The invention relates to a method for preparing magnesium hydroxide utilizing magnesium sulfate as a raw material, and the method comprises the following steps of: firstly preparing a 0.1- 4 mol/L solution from calcium nitrate or calcium chloride, then slowly adding magnesium sulfate used as the raw material to the solution, then filtering to obtain filter residue and filtrate, washing the filter residue to obtain gypsum, and introducing the filtrate into a circulation process. The method provided by the invention has the following advantages: 1) the cost is low, calcium oxide used as an alkalizer and an organic amine used as a precipitating agent can be recycled, thereby avoiding the defects of a calcium oxide method, simultaneously the amine circulation amount is low, the precipitation efficiency is high and the production raw material cost is reduced; 2) the energy consumption is low and environmental pollution caused by ammonia volatilization is avoided; and 3) the operation cost is low, the organic amine is used to precipitate magnesium hydroxide in the method, so that magnesium hydroxide adsorbs a certain amount of organic amine during generation and has hydrophobic property, the filtration speed is high and is more than 0.01 L/s.m<2> during filtering, washing is easy and the process operation cost is reduced.
Description
Technical field
The present invention relates to a kind of method of utilizing sal epsom feedstock production magnesium hydroxide, belong to field of inorganic chemical engineering.
Background technology
Magnesium hydroxide is a kind of white indissoluble powder, is widely used in PE, PP, PVC, ABS, PS, HIPS, PA, PBT, unsaturated polyester, Resins, epoxy, rubber, the flame retardant filler of paint; Aspect environmental protection,, can replace caustic soda and lime neutralizing agent as acid-bearing wastewater as the flue gas desulfurization (FGD) agent; As oil dope, play anticorrosion and desulfidation; Be used for the refining of electron trade, medicine, granulated sugar; Be used for lagging material and make other magnesium salts product.
At present, the preparation method of highly purified magnesium hydroxide mainly contains sodium hydroxide method, solvay soda process and calcium oxide method, sodium hydroxide method cost height, the filtration washing difficulty, solvay soda process ammonia internal circulating load is big, energy consumption height and ammonia loss amount are big, and equally also there is the problem of filtration washing difficulty in the calcium oxide method, can't prepare high purity magnesium hydrate.Especially as a kind of inorganic combustion inhibitor of excellent property, the market share that magnesium hydroxide occupied is very low always, and its basic reason is production cost height, complex process, so novel synthesis method and operational path are the active demand of market institute.
Organic amine as a kind of alkali when the precipitate metal ion and mineral alkalis such as sodium hydroxide, calcium hydroxide and ammoniacal liquor all be the effect that OH-is provided, but the organic amine price is more expensive, so industrial precipitate metal ion that generally seldom is used for, unless the method for rational recovery organic amine is arranged, the good grade of shaking about 1992 reported " the tertiary amine legal system is equipped with the thermodynamics of carbonate ", but mentioned the tertiary amine absorbing carbon dioxide, in addition, also have numerous documents and patent report organic amine such as diethanolamine, trolamine to be used for reclaiming the carbonic acid gas of industrial tail gas.The utilization of above organic amine is because the volatility of organic amine is littler than ammonia, during absorbing carbon dioxide the amine loss little, and organic amine is the bigger amine of water solubility, and can recycle in the aqueous solution.
Summary of the invention
Purpose of the present invention provides a kind of method of utilizing sal epsom feedstock production magnesium hydroxide, and it utilizes the water microsolubility of organic amine to realize the amine water sepn, makes the organic amine reusable edible, effectively reduces the use cost of organic amine.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the method for utilizing sal epsom feedstock production magnesium hydroxide, it is characterized in that at first nitrocalcite or calcium chloride are mixed with the solution of 0.1～4mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A and filtrate A, filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is:
1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stirring, is to react 0.5～2 hour under 10 ℃～100 ℃ conditions in temperature, filter then filter residue B and liquor B, filter residue B obtains magnesium hydrate powder through washing and drying, and the gained liquor B is standby;
2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reacted 0.5～2 hour under 10 ℃～100 ℃ conditions, leave standstill separatory, isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C;
3) separation of calcium: the liquor C adding is mixed with sal epsom, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A is inorganic soluble magnesium salts solution, can be recycled and reused for step 1).
Press such scheme, described sal epsom raw material is a solid.
Press such scheme, described inorganic soluble magnesium salts solution is that volumetric molar concentration is 0.1～4mol/L magnesium nitrate or magnesium chloride brine.
Press such scheme, described organic amine is a liquid under normal pressure, 10 ℃～100 ℃ conditions, under standard conditions, and acid dissociation constant pKa=10～11.5.
Press such scheme, described organic amine is a kind of or several mixing arbitrarily in Di-n-Butyl Amine, two n-amylamines, normal hexyl Amine and two normal hexyl Amines, and the mol ratio of contained magnesium elements amount is 2～2.4: 1 in the consumption of organic amine and the sal epsom raw material.
Press such scheme, the described mol ratio that contains the organic amine of its efficient oxidation calcium of calcium oxide raw material and adding is 1～1.5: 2.
Present method technology is simple, and is easy to operate, cheap, can prepare high purity, and easy filtering magnesium hydroxide.The magnesium hydroxide of present method preparation can be used for a plurality of fields such as chemical industry, environmental protection, food, medical treatment.
Chemical equation involved in the present invention is as follows:
CaO+2R
3NHX → CaX
2+ 2R
3N (but separatory)+H
2O
CaX
2+MgSO
4→CaSO
4↓+MgX
2
MgX
2+2R
3N+2H
2O→Mg(OH)
2↓+2R
3NHX
X=Cl wherein
-Or NO
3 -, R=H or alkyl, but R can not all be H or alkyl,
The gained magnesium hydroxide can prepare high-purity magnesium oxide through thermal degradation.
The preparation method of magnesium hydroxide provided by the present invention compares with traditional method, has the following advantages: 1) cost is low, and calcium oxide is as basifier, organic amine recycles as precipitation agent, has avoided the shortcoming of calcium oxide method, and the amine internal circulating load is little simultaneously, the deposition efficiency height has reduced the raw materials for production cost; 2) energy consumption is low, and this technology can be in normal-temperature operation, and amine can separate by the method for separatory with solution, has avoided the ammonia still process operation in the solvay soda process, has also avoided the pollution of ammonia volatilization to environment simultaneously; 3) process cost is low, and this method organic amine precipitated magnesium hydroxide makes magnesium hydroxide certain organic amine of absorption when generating, thereby has hydrophobic property, and when filtering, filtration velocity is very fast, greater than 0.01L/sm
2, and easily wash, reduced the process cost of technology.
Description of drawings
The process flow sheet of Fig. 1 preparation magnesium hydroxide of the present invention;
The thermogravimetric curve of the magnesium hydroxide that Fig. 2 the present invention is prepared;
The sem photograph of the magnesium hydroxide of Fig. 3 embodiment 1 gained, signify hydrogen magnesium oxide is sheet on the figure, size distribution is even, between 0.1-5 μ m.
Embodiment
The present invention will be further described in detail below in conjunction with drawings and Examples.
Embodiment 1
Raw material used in the present invention has 1 part in a. nitrocalcite, is 1mol; B. organic amine is 1 part, and organic amine is a Di-n-Butyl Amine, is 2mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with nitrocalcite the solution of 1mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium nitrate solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 0.5 hour under 20 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being nitric acid Di-n-Butyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 2 hours under 20 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being ca nitrate soln); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53.3 grams through above-mentioned steps, yield is 90%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Fig. 2 is the thermogravimetric curve of the prepared magnesium hydroxide of present method, and curve 1 is a thermogravimetric curve, and curve 2 is the thermogravimetric differential curve, shows that by heat analysis data the purity of prepared magnesium hydroxide is 99.1%.
Fig. 3 is the sem photograph of the magnesium hydroxide of embodiment 1 gained, and signify hydrogen magnesium oxide is sheet on the figure, and size distribution is even, between 0.1-5 μ m.
Embodiment 2
Raw material used in the present invention has 1 part in a. nitrocalcite, is 1mol; B. organic amine is 1 part, and organic amine is two n-amylamines, is 2.4mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.2mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with nitrocalcite the solution of 0.1mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium nitrate solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 2 hours under 80 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being nitric acid two n-amylamine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 0.5 hour under 80 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being ca nitrate soln); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 52.7 grams through above-mentioned steps, yield is 89%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 3
Raw material used in the present invention has 1 part in a. nitrocalcite, is 1mol; B. organic amine is 1 part, and organic amine is a normal hexyl Amine, is 2.2mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.5mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with nitrocalcite the solution of 1.5mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium nitrate solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 0.5 hour under 50 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being nitric acid normal hexyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 1.5 hours under 50 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being ca nitrate soln); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53.2 grams through above-mentioned steps, yield is 90%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 4
Raw material used in the present invention has 1 part in a. nitrocalcite, is 1mol; B. organic amine is 1 part, and organic amine is two normal hexyl Amines, is 2.4mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.3mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with nitrocalcite the solution of 3mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium nitrate solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 0.5 hour under 70 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being nitric acid two normal hexyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 2 hours under 40 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being ca nitrate soln); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 54.3 grams through above-mentioned steps, yield is 95%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 5
Raw material used in the present invention has 1 part in a. calcium chloride, is 1mol; B. organic amine is 1 part, and organic amine is a Di-n-Butyl Amine, is 2.1mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.1mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with calcium chloride the solution of 1mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium chloride solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 0.5 hour under 20 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being chlorination Di-n-Butyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 2 hours under 20 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being calcium chloride solution); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53.2 grams through above-mentioned steps, yield is 90%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 6
Raw material used in the present invention has 1 part in a. calcium chloride, is 1mol; B. organic amine is 1 part, and organic amine is two n-amylamines, is 2.4mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.2mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with calcium chloride the solution of 0.1mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium chloride solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 0.5 hour under 70 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being chlorination two n-amylamine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 2 hours under 60 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being calcium chloride solution); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53 grams through above-mentioned steps, yield is 89%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 7
Raw material used in the present invention has 1 part in a. calcium chloride, is 1mol; B. organic amine is 1 part, and organic amine is a normal hexyl Amine, is 2.0mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.3mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with calcium chloride the solution of 4mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium chloride solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 1 hour under 30 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being chlorination normal hexyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 0.5 hour under 40 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being calcium chloride solution); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 54.1 grams through above-mentioned steps, yield is 94%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 8
Raw material used in the present invention has 1 part in a. calcium chloride, is 1mol; B. organic amine is 1 part, and organic amine is two normal hexyl Amines, is 2.3mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.4mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with calcium chloride the solution of 3mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium chloride solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 1 hour under 70 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being chlorination two normal hexyl Amine solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 2 hours under 40 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being calcium chloride solution); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53 grams through above-mentioned steps, yield is 89%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Embodiment 9
Raw material used in the present invention has 1 part in a. calcium chloride, is 1mol; B. organic amine is 1 part, and organic amine is the mixture of two normal hexyl Amines and Di-n-Butyl Amine, and ratio of mixture is any ratio, and the amine consumption is 2.2mol; C. contain 1 part of calcium oxide raw material, measure its content of free calcium oxide before using, be 1.4mol; D. the sal epsom raw material is 2 parts, measures wherein sal epsom content before the use, and every part respectively is 1mol.
The setting up procedure of technological cycle of the present invention is at first being mixed with calcium chloride the solution of 2mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A (being plaster stone) and filtrate A (being magnesium chloride solution), filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is: the 1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stir, in temperature is to react 1 hour under 10 ℃ of conditions, filter then filter residue B (being magnesium hydroxide) and liquor B (being ammonia chloride solution), filter residue B through the washing and drying obtain magnesium hydrate powder, the gained liquor B is standby; 2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reaction is 1.5 hours under 10 ℃ of conditions, leaves standstill separatory, and isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C (being calcium chloride solution); 3) separation of calcium: the liquor C adding is mixed with the sal epsom raw material, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A can be recycled and reused for step 1).
Get magnesium hydroxide 53.1 grams through above-mentioned steps, yield is 90%, and purity is 98%, and the heating dehydration can get high-purity magnesium oxide.
Claims (6)
1. utilize the method for sal epsom feedstock production magnesium hydroxide, it is characterized in that at first nitrocalcite or calcium chloride are mixed with the solution of 0.1～4mol/L, slowly join the sal epsom raw material in the solution then, filter again, get filter residue A and filtrate A, filter residue A through wash plaster stone, filtrate A enters working cycle, described working cycle step is:
1) preparation of magnesium hydroxide: organic amine is joined among the filtrate A, stirring, is to react 0.5～2 hour under 10 ℃～100 ℃ conditions in temperature, filter then filter residue B and liquor B, filter residue B obtains magnesium hydrate powder through washing and drying, and the gained liquor B is standby;
2) reduction of amine: with liquor B with contain the calcium oxide raw material and mix stirring, reacted 0.5～2 hour under 10 ℃～100 ℃ conditions, leave standstill separatory, isolating organic amine is recycled and reused for step 1) after purifying, remaining water solidliquid mixture after filtration, it is standby to obtain liquor C;
3) separation of calcium: the liquor C adding is mixed with sal epsom, stir, cooling, filter to get filtrate then A and filter residue A, filter residue A are plaster stone through washing, filtrate A is inorganic soluble magnesium salts solution, can be recycled and reused for step 1).
2. by the described method of utilizing sal epsom feedstock production magnesium hydroxide of claim 1, it is characterized in that described sal epsom raw material is a solid.
3. by claim 1 or the 2 described methods of utilizing sal epsom feedstock production magnesium hydroxide, it is characterized in that described inorganic soluble magnesium salts solution is that volumetric molar concentration is 0.1～4mol/L magnesium nitrate or magnesium chloride brine.
4. by claim 1 or the 2 described methods of utilizing sal epsom feedstock production magnesium hydroxide, it is characterized in that described organic amine is liquid under normal pressure, 10 ℃～100 ℃ conditions, under standard conditions, acid dissociation constant pKa=10～11.5.
5. by claim 1 or the 2 described methods of utilizing sal epsom feedstock production magnesium hydroxide, it is characterized in that described organic amine is a kind of or several mixing arbitrarily in Di-n-Butyl Amine, two n-amylamines, normal hexyl Amine and two normal hexyl Amines, the mol ratio of contained magnesium elements amount is 2～2.4: 1 in the consumption of organic amine and the sal epsom raw material.
6. by claim 1 or the 2 described methods of utilizing sal epsom feedstock production magnesium hydroxide, it is characterized in that the described mol ratio that contains the organic amine of its efficient oxidation calcium of calcium oxide raw material and adding is 1～1.5: 2.
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| CN103896314A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-purity magnesium oxide by using boron-removed salt lake old brine as raw material |
| CN103896312A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-purity magnesium oxide by adopting seawater and salt lake brine as raw materials |
| CN103896313A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-activity magnesium oxide by adopting old brine in salt lake as material |
| CN105274622A (en) * | 2015-11-16 | 2016-01-27 | 武汉工程大学 | Method for preparing magnesium hydrate crystal whiskers and calcium sulfate with phosphate tailings as raw material |
| CN106986360A (en) * | 2017-04-01 | 2017-07-28 | 龙岩紫云化学科技有限公司 | The method that calcic magnesium carbonate thing ore deposit prepares magnesium hydroxide |
| CN108529654A (en) * | 2018-05-07 | 2018-09-14 | 天津君瑞和科技有限公司 | A method of with making from brine for micro/nano level magnesium hydroxide |
| CN116282092A (en) * | 2023-03-29 | 2023-06-23 | 中国恩菲工程技术有限公司 | Preparation method of magnesium oxide |
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| CN1332116A (en) * | 2001-08-20 | 2002-01-23 | 杜以波 | Homogeneous fluid process of preparing nanometer magnesium hydroxide |
| JP2010505722A (en) * | 2006-10-03 | 2010-02-25 | セルヴィシオス インダストリアレス ペニョーレス，ソシエダッド アノニマ デ キャピタル ヴァリアブル | Process for producing monodisperse and stable nanometer magnesium hydroxide and product thereof |
| CN101723431A (en) * | 2008-10-07 | 2010-06-09 | 中国恩菲工程技术有限公司 | Method for recovering magnesium from magnesium sulfate solution |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332116A (en) * | 2001-08-20 | 2002-01-23 | 杜以波 | Homogeneous fluid process of preparing nanometer magnesium hydroxide |
| JP2010505722A (en) * | 2006-10-03 | 2010-02-25 | セルヴィシオス インダストリアレス ペニョーレス，ソシエダッド アノニマ デ キャピタル ヴァリアブル | Process for producing monodisperse and stable nanometer magnesium hydroxide and product thereof |
| CN101723431A (en) * | 2008-10-07 | 2010-06-09 | 中国恩菲工程技术有限公司 | Method for recovering magnesium from magnesium sulfate solution |
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| 胡章文 等: "硫酸镁一步法制备氢氧化镁阻燃剂", 《过程工程学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896314A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-purity magnesium oxide by using boron-removed salt lake old brine as raw material |
| CN103896312A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-purity magnesium oxide by adopting seawater and salt lake brine as raw materials |
| CN103896313A (en) * | 2012-12-31 | 2014-07-02 | 江西江锂科技有限公司 | Method for preparing high-activity magnesium oxide by adopting old brine in salt lake as material |
| CN105274622A (en) * | 2015-11-16 | 2016-01-27 | 武汉工程大学 | Method for preparing magnesium hydrate crystal whiskers and calcium sulfate with phosphate tailings as raw material |
| CN106986360A (en) * | 2017-04-01 | 2017-07-28 | 龙岩紫云化学科技有限公司 | The method that calcic magnesium carbonate thing ore deposit prepares magnesium hydroxide |
| CN108529654A (en) * | 2018-05-07 | 2018-09-14 | 天津君瑞和科技有限公司 | A method of with making from brine for micro/nano level magnesium hydroxide |
| CN116282092A (en) * | 2023-03-29 | 2023-06-23 | 中国恩菲工程技术有限公司 | Preparation method of magnesium oxide |
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| CN102275958B (en) | 2013-02-06 |
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