CN105274622B - The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing - Google Patents
The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing Download PDFInfo
- Publication number
- CN105274622B CN105274622B CN201510785723.1A CN201510785723A CN105274622B CN 105274622 B CN105274622 B CN 105274622B CN 201510785723 A CN201510785723 A CN 201510785723A CN 105274622 B CN105274622 B CN 105274622B
- Authority
- CN
- China
- Prior art keywords
- solution
- phosphorus tailing
- calcium sulfate
- crystal whisker
- magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of methods preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing.By phosphorus tailing obtained by flotation and mixed in hydrochloric acid, react, clean, filter after obtain the mixed solution containing magnesium chloride and calcium chloride；Phosphorus tailing is mixed with sulfuric acid, is reacted, Adlerika is obtained after removal of impurities, filtering；Above two solution is mixed, react, filter after obtain calcium sulfate precipitation and magnesium chloride filtrate；Lye is added in magnesium chloride filtrate, reacts and obtains the liquid-solid mixture containing basic magnesium chloride whisker after being aged；Alkaline solution is then added, reacts and obtains magnesium hydroxide crystal whisker after being aged.The present invention prepares nanometer or micron magnesium hydroxide crystal whisker by raw material of phosphorus tailing, and the calcium sulfate of by-product high-quality realizes phosphorous chemical industry solid waste higher value application.
Description
Technical field
The invention belongs to utilizations of waste as resource and function nano Material Field, and in particular to be with phosphorus tailing with one kind
The method that raw material prepares magnesium hydroxide crystal whisker and calcium sulfate.
Background technology
Phosphorus ore is main fertilizer --- the raw material of phosphate fertilizer needed for Global Agriculture production, is the important guarantor of world food production
Card；It is also the raw material of fine chemical product production.The phosphorus ore grade in 90% or more China is less than 26%, average grade about 17%.
It is utilized with the continuous exploitation of phosphate rock resource, middle-low grade and hardly possible select the utilization of phosphate rock resource to be closed by many scientific research persons
Note.The content of magnesium, iron, aluminum oxide in the most of middle-low grade ores in China is high, needs to process by more complex ore dressing
Flow can just obtain the phosphorus concentrate for meeting production requirement.Magnesium in phosphorus ore is generally with dolomite (CaCO3·MgCO3) form deposit
The mass content of part phosphorus ore MgO reaches 10%.The country mostly uses reverse flotation to remove dolomite to obtain low magnesium essence at present
Mine carries out wet processing again, and MgO mass contents are higher in phosphorus tailing after flotation for most of phosphorus ores, and about 14~18%.With phosphorus
The increase year by year of tailing accumulating amount, not only results in waste of resources, but also brings serious environmental pollution.How by phosphorus mining tailing
It utilizes, turns waste into wealth, become sulphur dioxide of phosphor chemical industry problem in the urgent need to address.
About the research on utilization to association magnesium in phosphorus tailing, the achievement in research of Chinese researcher is gone on along in the world
Forefront.
Jin Shaoxiang etc. compares systematic research to the mineralogy important feature of calcium in phosphate ore flotation tailings, magnesium, phosphorus,
Some important conclusions are obtained, to be carried for the separation etc. of the comprehensive utilization of High-Mg phosphate tailings, dolomite and collophane
For theoretical foundation, to the secondary use of phosphorus tailing, instruct developer reasonably to carry out experimental design to have a very important significance.
Yang Shuhuai uses the method for hydrochloric acid and sulfuric acid mixed acid acidleach to decompose the technique of phosphorus tailing, and leachate is carried out
Comprehensive purifying has been finally reached ideal effect, to realizing that cycle production has practice guiding action.
Huang Fang et al. have studied phosphorus tailing and sulfuric acid dissolution during particle surface situation of change, liquid-solid phase substance
The situation of change of situation of change and solid particles surface product, for phosphorus tailing recycling provide it is very valuable
Theoretical reference.
Zhou Junhong etc. is with hydrochloric acidolysis phosphorus tailing preparing magnesium hydroxide, by strictly controlling the pH of solution, effectively by magnesium
Ion exchange comes out, and obtains magnesium hydroxide solution and the calcium carbonate of very high purity.
About the comprehensive utilization of phosphorus tailing, typically realized according to the characteristics of phosphorus tailing itself.The identical research of gold
The fillibility of phosphorus tailing finds that the phosphorus tailing of suitable grade has preferable feasibility as cemented filling material.Li Jie's system
Ground has studied the physical property of phosphorus tailing, and combines other raw materials in tailing location, obtains the real compact close, body of hole wall structure
It is excellent air entrained concrete.Its forest rent of king uses phosphorus tailing to be prepared as inert filler, and construction material prepares planting brick, foaming mixes
Solidifying soil, lightweight wall plate；In the case where being not incorporated into cement, the compression strength of planting brick has reached 50MPa.Guan Zongfu, Chen Yi
It is ripe to have prepared cement using phosphorus slag, phosphorus ore and phosphorus tailing and compound suitable waste residue or inorganic non-metallic mine by the people, Guo Suihua et al.
Expect adjuvant for combustion, using these auxiliary agents and suitably adjustment proportion scheme has been burnt into high strength clinker under normal operation.Lead to emerging wait
Ratio, the ratio of mud, phosphorus tailing volume, the cement consumption etc. for crossing research phosphorus slag and quick lime have obtained the guarantor more than national regulation index
Warm plate.
Without solving China's phosphorus tailing environmental problem that pile up like a mountain, it is solid to be also both not carried out phosphorous chemical industry for above-mentioned various methods
The comprehensive utilization of associated resources in body waste.
Magnesium hydroxide is a kind of important inorganic chemical product, usually with natural minerals shepardite, contain the halogen of magnesium chloride
Water halogen mine or magnesite are raw material, are made by physically or chemically converting.Magnesium hydroxide is a kind of with extremely strong resiliency
Can, the alkaline agent of efficient chemical absorption property and the inorganic combustion inhibitor with flame retardant property, be widely used in environmental protection, ceramic material,
The fields such as medicine, high molecular material, market demand are larger.Magnesium hydroxide crystal whisker is as a kind of inorganic Green Flammability strengthening material
Material has the characteristics such as low surface energy, good mechanical strength, high elastic modulus, is greatly improved filled polymer composite wood
Rigidity, intensity, dimensional stability and the heat distortion temperature of material.
Currently, only resting on laboratory stage to the comprehensive utilization of phosphorus ore association magnesium resource, low cost is comprehensive with greenization
Conjunction need further to develop using technology, equipment and technology.
Invention content
Present invention aims at a kind of method preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing is provided, have
Effect solves the global questions such as the accumulation of phosphorus tailing, pollution environment, improves the comprehensive utilization ratio of phosphorus ore association magnesium resource；The sulphur of by-product
Sour calcium can be used for plaster bandage, making plaster cast, chalk, craftwork etc.；The solid filtered out in acid hemolysis process simultaneously
Waste residue can be used for construction material.
To achieve the above objectives, as follows using technical solution：
A method of magnesium hydroxide crystal whisker and calcium sulfate being prepared by raw material of phosphorus tailing, process is as follows：
1) it by phosphorus tailing and mixed in hydrochloric acid obtained by flotation, reacts 1~4 hour, filters under conditions of 25~80 DEG C；Gained
Oxidant and alkaline solution are added in filtrate, control ph is 6.5~8, is obtained containing magnesium chloride and chlorination after precipitating, filtering
The mixed solution of calcium；
2) phosphorus tailing and sulfuric acid are mixed, is reacted 2~4 hours under the conditions of 25~80 DEG C, filtered；Oxygen is added in gained filtrate
Agent and alkaline solution, control ph are 6.5~8, and refined sulfuric acid magnesium solution is obtained after precipitating, filtering；
3) it is 1 by the molar ratio of calcium chloride and magnesium sulfate by step 1) and step 2) acquired solution:1 ratio mixing,
Under the conditions of 25~85 DEG C, stirring, reaction 0.5~1 hour obtain purified magnesium chloride solution, gained precipitation warp after precipitating, filtering
After washing, drying, calcium sulfate is obtained；
4) it by the purified magnesium chloride solution obtained by step 3), is placed in ultrasound environments, alkaline solution is added dropwise under stirring condition,
Control OH-/Mg2+Than 1：3~1：Between 7, reacted 1~2 hour under the conditions of 25~80 DEG C；It obtains preparing hydroxide after ageing
The liquid-solid mixture of the presoma basic magnesium chloride whisker of magnesium whisker；
5) liquid-solid mixture obtained by step 4) is placed in ultrasound environments, alkaline solution, control ph is added dropwise under stirring condition
It is 10~11, is reacted 0.5~1.5 hour under the conditions of 25~80 DEG C；It is aged, be filtered, washed, be dried to obtain magnesium hydroxide crystalline substance
Palpus；
By said program, the phosphorus tailing is phosphate ore flotation tailings, wherein containing P2O5% is 1.7~7.0wt%, white clouds
Stone [CaOMgO (CO2)2] it is 55~80wt%.
By said program, the hydrochloric acid is 20~38wt%；The sulfuric acid is 10wt%~30wt%.
By said program, the oxidant is hydrogen peroxide；Alkaline solution is that ammonium hydroxide, sodium hydroxide solution or potassium hydroxide are molten
Liquid.
By said program, step 4) Aging Temperature is 40~60 DEG C, and the digestion time time is 36~60 hours.
By said program, step 5) Aging Temperature is 40~60 DEG C, and digestion time is 0.5~1.5 hour, using water and second
Alcohol washs magnesium hydroxide crystal whisker successively, and drying temperature is 60~100 DEG C, dry to constant weight.
In step 4), if the alkaline solution being added dropwise is ammonium hydroxide, obtained presoma is nanometer basic magnesium chloride whisker；If
When the alkaline solution being added dropwise in step 4) is sodium hydroxide solution or potassium hydroxide solution, obtained presoma is micron alkali formula
Magnesium chloride whisker.In step 5), reacts, then obtained with ammonium hydroxide according to the solidliquid mixture containing nanometer basic magnesium chloride whisker
Be nano-sized magnesium hydroxide whisker；It is finally obtained to be if using sodium hydroxide solution or potassium hydroxide solution in step 5)
Micron sodium hydroxide whisker.
The present invention has the beneficial effect that：
The present invention prepares nanometer or micron magnesium hydroxide crystal whisker and calcium sulfate by raw material of phosphorus tailing, and phosphorous chemical industry may be implemented
Solid waste higher value application.
Compared with sulfuric acid solution phosphorus tailing prepares the method for magnesium hydroxide, the present invention is to the utilization rate higher of phosphorus tailing, life
Produce original pattern at low cost, and that magnesium hydroxide crystal whisker can be kept, the size tunable of magnesium hydroxide crystal whisker；Magnesium chloride will be contained
After being mixed with refined sulfuric acid magnesium solution with the mixed solution of calcium chloride, magnesium chloride can not only be enriched with, moreover it is possible to generate quality compared with
Good calcium sulfate.
Specific implementation mode
A method of preparing nanometer or micron magnesium hydroxide crystal whisker and calcium sulfate, including following step by raw material of phosphorus tailing
Suddenly：
1) it by phosphorus tailing and mixed in hydrochloric acid obtained by flotation, reacts 1~4 hour, filters under conditions of 25~80 DEG C；Gained
Oxidant and alkaline solution are added in filtrate, control ph is 6.5~8, is obtained containing magnesium chloride and chlorination after precipitating, filtering
The mixed solution of calcium；
2) phosphorus tailing and sulfuric acid are mixed, is reacted 2~4 hours under the conditions of 25~80 DEG C, filtered；Oxygen is added in gained filtrate
Agent and alkaline solution, control ph are 6.5~8, and refined sulfuric acid magnesium solution is obtained after precipitating, filtering；
3) it is 1 by the molar ratio of calcium chloride and magnesium sulfate by step 1) and step 2) acquired solution:1 ratio mixing,
Under the conditions of 25~85 DEG C, stirring, reaction 0.5~1 hour obtain purified magnesium chloride solution, gained precipitation warp after precipitating, filtering
After washing, drying, calcium sulfate is obtained；
4) it by the purified magnesium chloride solution obtained by step 3), is placed in ultrasound environments, alkaline solution is added dropwise under stirring condition,
Control OH-/Mg2+Than 1：3~1：Between 7, reacted 1~2 hour under the conditions of 25~80 DEG C；It obtains preparing hydroxide after ageing
The liquid-solid mixture of the presoma basic magnesium chloride whisker of magnesium whisker；
5) liquid-solid mixture obtained by step 4) is placed in ultrasound environments, alkaline solution is added dropwise under stirring condition, control pH
Value is 10~11, is reacted 0.5~1.5 hour under the conditions of 25~80 DEG C；It is aged, be filtered, washed, dry obtained magnesium hydroxide
Whisker.
By said program, the phosphorus tailing is phosphate ore flotation tailings, wherein containing P2O5% is 1.7~7.0wt%, white clouds
Stone [CaOMgO (CO2)2] it is 55~80wt%.
Optimally, the hydrochloric acid is 10~38wt%；The sulfuric acid is 10wt%~98wt%.
Optimally, the oxidant is hydrogen peroxide；Alkaline solution is ammonium hydroxide, sodium hydroxide solution or potassium hydroxide solution.
Optimally, in step 4), if the alkaline solution being added dropwise is ammonium hydroxide, obtained presoma is nanometer basic magnesium chloride
Whisker；If the alkaline solution being added dropwise in step 4) is sodium hydroxide solution or potassium hydroxide solution, obtained presoma is
Micron basic magnesium chloride whisker.
Optimally, it in step 5), according to solidliquid mixture and ammonium hydroxide containing nanometer basic magnesium chloride whisker, then obtains
Be nano-sized magnesium hydroxide whisker；It is finally obtained to be if using sodium hydroxide solution or potassium hydroxide solution in step 5)
Micron sodium hydroxide whisker.
Optimally, step 4) Aging Temperature is 40~60 DEG C, and the digestion time time is 12~72 hours.
Optimally, step 5) Aging Temperature is 40~60 DEG C, and digestion time is 0.5~1.5 hour, using water and ethyl alcohol according to
Secondary washing magnesium hydroxide crystal whisker, drying temperature are 60~100 DEG C, dry to constant weight.
Embodiment 1
By in 200 grams of input three-necked flasks of phosphorus tailing obtained by flotation, 49.14 milliliters of water are added, reach 70 DEG C of preset temperature
Afterwards, under agitation, it is slowly added to 351.11 milliliter 38% of hydrochloric acid, after reacting 3.5 hours, is filtered, washed carry out solid-liquid
Separation；1.08 milliliter of 30% hydrogen peroxide is added, ammonium hydroxide is added dropwise under agitation, control filtrate pH value is 6.7, is reacted 1 hour,
Filtering, obtains magnesium chloride and calcium chloride mixed solution, is labeled as solution A；Phosphorus 220.76 grams of inputs of tailing obtained by flotation are another
In three-necked flask, add 825.41 milliliters of water, after reaching 50 DEG C of preset temperature, the sulfuric acid for being slowly added to 129 milliliters of 98wt% carries out
Reaction is filtered, washed and is separated by solid-liquid separation after reacting 2 hours；1.08 milliliter of 30% hydrogen peroxide is added, under agitation, drop
It is 6.7 to ammoniate water management filtrate pH value, is reacted 1 hour, and filtering obtains refined Adlerika, is denoted as solution B；By molten A and
Solution B is 1 by the molar ratio of calcium chloride and magnesium sulfate:1 ratio mixing, is sufficiently stirred, reaction 0.5 hour, so at 45 DEG C
After be filtered, washed and be separated by solid-liquid separation, control a concentration of 3mol/l of magnesium chloride solution, be labeled as solution C, filtered white is solid
Body obtains calcium sulphate powders after dry.
Ultrasonic device and blender are opened, control system temperature is 30 DEG C, is slowly dripped in the three-necked flask equipped with solution C
Add 2.83 milliliters of ammonium hydroxide, after reacting 1 hour, is aged 36 hours under the conditions of 40 DEG C；After the completion of ageing, it is again turned on ultrasonic device
And blender, and into liquid-solid mixture, ammonium hydroxide to the pH value of dropwise addition 20% is 10, is reacted 0.5 hour under the conditions of 50 DEG C；Instead
It after answering, is aged 0.5 hour, filters under the conditions of 40 DEG C, white solid phase is washed using water and ethyl alcohol successively, finally at 60 DEG C
Lower drying obtains nano-sized magnesium hydroxide whisker after drying to constant weight.
Embodiment 2
By in 200 grams of input three-necked flasks of phosphorus tailing obtained by flotation, add 14.72 milliliters of water, after reaching 50 DEG C of preset temperature,
Under agitation, it is slowly added to the hydrochloric acid of 380.29 milliliters of 38wt%, after reacting 3.5 hours, is filtered, washed and carries out solid-liquid point
From；1.08 milliliters of 30wt% hydrogen peroxide are added, under agitation, it is 6.7 that ammonium hydroxide control filtrate pH, which is added dropwise, is reacted 1 hour, mistake
Filter, obtains magnesium chloride and calcium chloride mixed solution, is labeled as solution A；By 220.76 grams of inputs another three of phosphorus tailing obtained by flotation
In mouth flask, add 825.41 milliliters of water, after reaching 50 DEG C of preset temperature, is slowly added to the sulfuric acid of 129 milliliters of 98wt%, reaction 2
After hour, it is filtered, washed and is separated by solid-liquid separation；2.83 milliliters of 30wt% hydrogen peroxide are added, under agitation, ammonium hydroxide control are added dropwise
PH value processed is 6.7, is reacted 1 hour, and filtering obtains refined Adlerika, is denoted as solution B；Molten A and solution B are pressed into chlorination
The molar ratio of calcium and magnesium sulfate is 1:1 ratio mixing, is sufficiently stirred at 45 DEG C, reacts 0.5 hour, be filtered, washed, carry out
It is separated by solid-liquid separation, controls a concentration of 3.5mol/l of magnesium chloride solution, be labeled as solution C, filtered white solid obtains after dry
To calcium sulphate powders.
Ultrasonic device and blender are opened, control system temperature is 30 DEG C, is slowly dripped in the three-necked flask equipped with solution C
Add 2.83 milliliters of 28wt% ammonium hydroxide, after reacting 1 hour, is aged 36 hours under the conditions of 40 DEG C；After the completion of ageing, it is again turned on super
Acoustic equipment and blender, and it is 10 to be passed through ammonia to pH value into liquid-solid mixture, under the conditions of 50 DEG C, is reacted 0.5 hour；Instead
It after answering, is aged 1 hour under the conditions of 40 DEG C, then filters, white solid phase is washed using water and ethyl alcohol successively, finally 60
It is dry at DEG C, obtain nano-sized magnesium hydroxide whisker after drying to constant weight.
Embodiment 3
By in 200 grams of input three-necked flasks of phosphorus tailing obtained by flotation, 49.14 milliliters of water are added, reach 30 DEG C of preset temperature
Afterwards, under agitation, it is slowly added to the hydrochloric acid of 351.11 milliliters of 38wt%, after reacting 3.5 hours, is filtered, washed and is consolidated
Liquid detaches；1.08 milliliters of 30wt% hydrogen peroxide are added, ammonium hydroxide is added dropwise under agitation, control filtrate pH value is 6.7, and reaction 1 is small
When, filtering obtains magnesium chloride and calcium chloride mixed solution, is labeled as solution A；220.76 grams of inputs of phosphorus tailing obtained by flotation are another
In one three-necked flask, add 596.87 milliliters of water, after reaching 50 DEG C of preset temperature, is slowly added to the sulphur of 335.68 milliliters of 50wt%
Acid is filtered, washed, is separated by solid-liquid separation after reacting 2 hours；1.08 milliliters of 30wt% hydrogen peroxide are added, under agitation,
It is 7 that ammonium hydroxide control filtrate pH value, which is added dropwise, is reacted 1 hour, and filtering obtains refined Adlerika, is denoted as solution B；By molten A and
Solution B is 1 by the molar ratio of calcium chloride and magnesium sulfate:1 ratio mixing, is sufficiently stirred, reaction 0.5 is small under the conditions of 45 DEG C
When, it is filtered, washed, is separated by solid-liquid separation, control a concentration of 4.0mol/l of magnesium chloride solution, be labeled as solution C, it is filtered white
Color solid obtains calcium sulphate powders after dry.
Ultrasonic device and blender are opened, control system temperature is 30 DEG C, is slowly dripped in the three-necked flask equipped with solution C
Add 2.10 milliliters of ammonium hydroxide, after reacting 1 hour, is aged 36 hours under the conditions of 40 DEG C；After the completion of ageing, it is again turned on ultrasonic device
And blender, and it is 10 that potassium hydroxide solution to the pH value of 50wt%, which is added dropwise, into liquid-solid mixture, is reacted under the conditions of 50 DEG C
0.5h；After reaction, it is aged 0.5 hour, filters at 40 DEG C, white solid phase is washed using water and ethyl alcohol successively, is finally existed
It is dry at 60 DEG C, obtain a micron magnesium hydroxide crystal whisker after drying to constant weight.
Embodiment 4
By in 100 grams of input three-necked flasks of phosphorus tailing obtained by flotation, 24.57 milliliters of water are added, reach 80 DEG C of preset temperature
Afterwards, it is slowly added to the hydrochloric acid of 175.56 milliliters of 38wt%, after reacting 3.5 hours, is filtered, washed and is separated by solid-liquid separation；It is added
Ammonium hydroxide is added dropwise in 0.54 milliliter of 30wt% hydrogen peroxide under agitation, and control filtrate pH value is 6.7, is reacted 1 hour, and filtering obtains
To magnesium chloride and calcium chloride mixed solution, it is labeled as solution A；By 110.38 grams of another three-necked flasks of input of phosphorus tailing obtained by flotation
In, 412.7 milliliters of water are added, after reaching 80 DEG C of preset temperature, the sulfuric acid for being slowly added to 64.69 milliliters of 98wt% is reacted,
After reaction 2 hours, it is filtered, washed and is separated by solid-liquid separation；1.08 milliliters of 30wt% hydrogen peroxide are added, ammonia is added dropwise under agitation
Water, control filtrate pH value are 6.7, are reacted 1 hour, and filtering obtains refined Adlerika, is denoted as solution B；By molten A and molten
Liquid B is 1 by the molar ratio of calcium chloride and magnesium sulfate:1 ratio mixing, is sufficiently stirred, reaction 0.5 hour, then at 45 DEG C
It is filtered, washed and is separated by solid-liquid separation, control a concentration of 4.5mol/l of magnesium chloride solution, be labeled as solution C, filtered white is solid
Body obtains calcium sulphate powders after dry.
Ultrasonic device and blender are opened, control system temperature is 40 DEG C, is slowly dripped in the three-necked flask equipped with solution C
Add 1.40 milliliters of ammonium hydroxide, after reacting 1 hour, is aged 48 hours under the conditions of 40 DEG C；After the completion of ageing, it is again turned on ultrasonic device
And blender, and it is 10 that sodium hydroxide solution to the pH value of 30wt%, which is added dropwise, into liquid-solid mixture, reacts 1 under the conditions of 50 DEG C
Hour；Then it is aged 0.5 hour, filters under the conditions of 40 DEG C, white solid phase is washed using water and ethyl alcohol successively, finally at 60 DEG C
Lower drying obtains a micron magnesium hydroxide crystal whisker after drying to constant weight.
Claims (7)
1. a kind of method preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing, it is characterised in that including following step
Suddenly：
1) it by phosphorus tailing and mixed in hydrochloric acid obtained by flotation, reacts 1~4 hour, filters under conditions of 25~80 DEG C；Gained filtrate
Middle addition oxidant and alkaline solution, control ph are 6.5~8, are obtained after precipitating, filtering containing magnesium chloride and calcium chloride
Mixed solution；
2) phosphorus tailing and sulfuric acid are mixed, is reacted 2~4 hours under the conditions of 25~80 DEG C, filtered；Oxidant is added in gained filtrate
And alkaline solution, control ph 6.5~8 obtain refined sulfuric acid magnesium solution after precipitating, filtering；
3) it is 1 by the molar ratio of calcium chloride and magnesium sulfate by step 1) and step 2) acquired solution:1 ratio mixing, 25~
Under the conditions of 85 DEG C, stirring, reaction 0.5~1 hour obtain purified magnesium chloride solution after precipitating, filtering, and gained is precipitated through washing
After washing, drying, calcium sulfate is obtained；
4) it by the purified magnesium chloride solution obtained by step 3), is placed in ultrasound environments, alkaline solution is added dropwise under agitation, control
OH processed-/Mg2+Than 1：3~1：Between 7, reacted 1~2 hour under the conditions of 25~80 DEG C；Basic magnesium chloride crystalline substance is obtained after ageing
The liquid-solid mixture of palpus；
5) liquid-solid mixture obtained by step 4) is placed in ultrasound environments, alkaline solution, control ph 10 is added dropwise under stirring condition
~11, it is reacted 0.5~1.5 hour under the conditions of 25~80 DEG C；It is aged, be filtered, washed, dry obtained magnesium hydroxide crystal whisker.
2. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
The phosphorus tailing is phosphate ore flotation tailings, wherein containing P2O5% is 1.7~7.0wt%, dolomite [CaOMgO (CO2)2]
For 55~80wt%.
3. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
The hydrochloric acid is 10wt%~38wt%；The sulfuric acid is 10wt%~98wt%.
4. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
The oxidant is hydrogen peroxide；Alkaline solution is ammonium hydroxide, sodium hydroxide solution or potassium hydroxide solution.
5. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
Aging Temperature is 40~60 DEG C in step 4), and digestion time is 12~72 hours.
6. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
Step 5) Aging Temperature is 40~60 DEG C, and digestion time is 0.5~1.5 hour, using the washing hydroxide respectively of water and ethyl alcohol
Magnesium whisker, drying temperature are 60~100 DEG C, dry to constant weight.
7. the method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing as described in claim 1, it is characterised in that
Step 4) with 5) in alkaline solution used be ammonium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510785723.1A CN105274622B (en) | 2015-11-16 | 2015-11-16 | The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510785723.1A CN105274622B (en) | 2015-11-16 | 2015-11-16 | The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105274622A CN105274622A (en) | 2016-01-27 |
| CN105274622B true CN105274622B (en) | 2018-08-03 |
Family
ID=55144423
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510785723.1A Expired - Fee Related CN105274622B (en) | 2015-11-16 | 2015-11-16 | The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105274622B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105879889B (en) * | 2016-06-03 | 2018-07-17 | 武汉工程大学 | A method of preparing catalyst using phosphorus tailing or low grade collophanite |
| CN106495191B (en) * | 2016-10-09 | 2019-03-29 | 湖北三宁化工股份有限公司 | A kind of method that hydrochloric acid decomposes phosphorus tailing preparing magnesium hydroxide and calcium sulfate |
| CN108179474A (en) * | 2017-12-25 | 2018-06-19 | 岭南师范学院 | A kind of method for the magnesium hydroxide crystal whisker for preparing high dispersive from bittern in salt lake using wind energy |
| CN108441967A (en) * | 2018-04-10 | 2018-08-24 | 武汉工程大学 | The method that hydrochloric acid resolving high magnesium phosphorus tailing prepares calcium sulfate crystal whiskers |
| CN110436435A (en) * | 2019-09-11 | 2019-11-12 | 武汉工程大学 | The method that circulation acidleach High-Mg phosphate tailings prepare calcium chlorophosphate and magnesium chloride whisker |
| CN110484970B (en) * | 2019-09-11 | 2021-11-12 | 武汉工程大学 | Resourceful treatment method for high-magnesium phosphate tailings |
| CN110424055B (en) * | 2019-09-11 | 2021-11-12 | 武汉工程大学 | Resource utilization method of high-magnesium phosphate tailings |
| CN111217385A (en) * | 2020-02-23 | 2020-06-02 | 武汉工程大学 | Method for preparing calcium-magnesium-aluminum hydrotalcite by using phosphate tailings |
| CN111285407A (en) * | 2020-02-23 | 2020-06-16 | 武汉工程大学 | Method for preparing calcium-magnesium-aluminum-iron hydrotalcite by using high-magnesium-phosphorus tailings as raw materials |
| CN111218033A (en) * | 2020-02-27 | 2020-06-02 | 武汉工程大学 | Method for preparing composite flame retardant by using phosphate tailings |
| CN111302376A (en) * | 2020-02-27 | 2020-06-19 | 武汉工程大学 | Method for preparing flame retardant by utilizing hydrochloric acid to carry out acidolysis on high-magnesium phosphate tailings |
| CN111302379B (en) * | 2020-04-20 | 2022-09-27 | 武汉工程大学 | Method for producing alpha-gypsum powder and light calcium carbonate by combining phosphorus tailings and phosphogypsum |
| CN111333050B (en) * | 2020-04-20 | 2023-03-07 | 武汉工程大学 | Combined production of magnesium ammonium phosphate and MgCO from phosphorus tailings and phosphogypsum 3 And by-product NH 4 Cl process |
| CN111410223B (en) * | 2020-04-20 | 2022-09-27 | 武汉工程大学 | Method for recycling carbon resources in phosphorus tailings |
| CN111484063A (en) * | 2020-04-20 | 2020-08-04 | 武汉工程大学 | Method for preparing ammonium chloride and light magnesium carbonate by utilizing phosphate tailings and recycling ammonium chloride and light magnesium carbonate |
| CN114275802B (en) * | 2021-12-29 | 2022-08-26 | 中国地质科学院矿产综合利用研究所 | Method for large-scale absorption and high-value utilization of phosphate rock tailings |
| CN115418720B (en) * | 2022-08-03 | 2024-02-27 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing magnesium hydroxide whisker and calcium sulfate by taking salt lake brine as raw material |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172627B (en) * | 2007-10-11 | 2011-02-02 | 河北科技大学 | Method of producing magnesium hydroxide |
| CN101323974A (en) * | 2008-07-08 | 2008-12-17 | 浙江大学 | Method for preparing calcium sulphate crystal whisker from dolomite |
| CN102275958B (en) * | 2011-07-29 | 2013-02-06 | 武汉工程大学 | Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material |
| CN102618931B (en) * | 2012-04-06 | 2015-04-22 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN102874851A (en) * | 2012-09-28 | 2013-01-16 | 沈阳化工大学 | Method of utilizing brine to coproduce magnesium hydroxide and calcium sulfate whisker |
| CN103950957A (en) * | 2014-04-22 | 2014-07-30 | 彭振超 | Process method for preparing magnesium hydroxide from magnesium sulfate |
| CN104261443A (en) * | 2014-09-25 | 2015-01-07 | 池州西恩新材料科技有限公司 | Process for calcium-method production of magnesium hydrate by using nanofiltration membrane |
| CN104593867A (en) * | 2014-12-25 | 2015-05-06 | 武汉工程大学 | Method for preparing in-situ modified nano-magnesium hydroxide whiskers by taking phosphate tailings as raw materials |
| CN104528778A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials |
| CN104611763A (en) * | 2014-12-25 | 2015-05-13 | 武汉工程大学 | Technology of using phosphate tailing as raw material to produce in-situ modified nano-magnesium hydroxide whisker |
-
2015
- 2015-11-16 CN CN201510785723.1A patent/CN105274622B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105274622A (en) | 2016-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105274622B (en) | The method for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing | |
| CN105442048B (en) | The technique for preparing magnesium hydroxide crystal whisker and calcium sulfate as raw material using phosphorus tailing | |
| CN101293663B (en) | Novel technique for preparing fine calcium carbonate | |
| CN108273826B (en) | A kind of complete mutually high-valued recoverying and utilizing method of lithium slag | |
| CN101235440A (en) | Method of comprehensively utilizing serpentine | |
| CN103508689A (en) | Method for preparing alpha semi-hydrated gypsum at low cost and prepared alpha semi-hydrated gypsum and gypsum block | |
| CN109250736A (en) | The method for preparing activated magnesia using reverse flotation phosphorus tailing | |
| CN110358937A (en) | A method of the selective enrichment scandium from titanium white waste acid and red mud | |
| CN102502722A (en) | Preparation method of high-purity magnesium oxide | |
| CN110055365A (en) | A kind of method that calcification-carbonization iron red mud recycles iron and tailings cement | |
| CN101823745B (en) | Method for producing super-fine light-weighted calcium carbonate, ammonium chloride and carbon powder with waste associated alkali solution and acetylene sludge | |
| CN106629806A (en) | Method for producing dihydrate gypsum from waste liquid in laterite nickel ore wet process | |
| CN103408050B (en) | Method of efficient extraction of aluminum, iron, and titanium in coal gangue | |
| CN106044784A (en) | Method for producing high-purity silicon dioxide by utilizing flyash | |
| CN109133775A (en) | Lithium slag mixture gravel type cement concrete and preparation method thereof | |
| CN115196843B (en) | Red mud dealkalization stabilization method | |
| CN110467171A (en) | A kind of recycling processing method recycling acidleach High-Mg phosphate tailings | |
| CN102115143A (en) | Method for producing calcium sulfate from carbide slag | |
| CN109695059A (en) | A kind of preparation method of crystal whisker of gypsum | |
| CN102432072A (en) | Method for preparing magnesium oxide, ferric oxide, silicon dioxide and boric acid from ludwigite | |
| CN105271290A (en) | Method for preparing analcite through high-alumina fly ash | |
| CN102115813B (en) | Comprehensive utilization method for low-grade magnesite | |
| CN106238223B (en) | Melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor and its preparation, application method | |
| CN101760630A (en) | Method for recovering copper from copper sulfate solution | |
| CN109319896A (en) | The method for preparing flocculant with flyash and vanadium titano-magnetite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180803 Termination date: 20211116 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |