CN106673025A - Technological method for producing magnesium hydroxide by utilization of magnesium-containing wastewater generated by laterite nickel ore wet-process - Google Patents
Technological method for producing magnesium hydroxide by utilization of magnesium-containing wastewater generated by laterite nickel ore wet-process Download PDFInfo
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- CN106673025A CN106673025A CN201611014237.0A CN201611014237A CN106673025A CN 106673025 A CN106673025 A CN 106673025A CN 201611014237 A CN201611014237 A CN 201611014237A CN 106673025 A CN106673025 A CN 106673025A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a technological method for producing magnesium hydroxide by the utilization of magnesium-containing wastewater generated by laterite nickel ore wet-process. Laterite nickel ore pickle liquor mainly contains elements such as nickel, iron, magnesium, manganese, etc. After separation and purification processes such as iron removal, nickel precipitation, manganese removal by oxidation, mixed liquor of magnesium chloride and calcium chloride with high purity is obtained. The clear mixed liquor and refined lime milk with a certain concentration are mixed according to a certain ratio under a certain condition to react so as to generate magnesium hydroxide precipitate. By the technological method, the magnesium resource in the laterite nickel ore is recovered at low cost, comprehensive utilization of magnesium is realized. Meanwhile, the problem that product quality doesn't reach the standard by a lime cream process for magnesium precipitation is solved. A new process route is opened up for a traditional magnesium hydroxide preparation method, and the national resource of magnesium is effectively protected.
Description
Technical field
The invention belongs to resource reclaim field of comprehensive utilization, and in particular to one kind is produced using lateritic nickel ore wet processing and contained
Magnesium waste liquid produces the process of magnesium hydroxide.
Background technology
Magnesium hydroxide is the excellent fire retardant of plastics, rubber, be have in generally acknowledged rubber and plastic industry fire-retardant, suppression cigarette,
The outstanding fire retardant of filling triple functions.It is widely used in rubber, chemical industry, building materials, plastics and electronics, unsaturated polyester (UP) and oil
In paint, coating Polymer material.Magnesium hydroxide can replace Caustic soda and Calx conduct as flue gas desulfurization agent in terms of environmental protection
The nertralizer of acid-bearing wastewater.
Lateritic nickel ore is the maximum mineral of global nickel resources reserves, with the increasingly depleted of nickel sulfide ore, lateritic nickel ore smelting
Refining is more and more.Lateritic nickel ore in addition to nickeliferous, also substantial amounts of ferrum and magnesium.Traditional smelting process has pyrometallurgical smelting and wet
Method is smelted, and wherein pyrometallurgical smelting can not reclaim magnesium.Recycling of the hydrometallurgy to magnesium is roughly divided into does Magnesium sulfate heptahydrate, oxidation
Magnesium.General technology is liquid after the heavy nickel of sulfuric acid process, and evaporative crystallization prepares Magnesium sulfate heptahydrate after purification.Hydrochloric acid method is typically chloride
Change magnesium solution spraying cracking production magnesium oxide, hydrochloric acid reuse.
And the raw material for producing industrial magnesium hydroxide is mainly natural brucite, magnesite, dolomite and salt.Production technology
Predominantly ammonia process and sodium hydroxide, wherein sodium-hydroxide method is expensive, is only applicable to some high-quality fields.Ammonia process produces hydrogen
The conversion ratio of magnesium oxide is low, and probably only 60% ~ 70%, the exceeded pollution environment of ammonia nitrogen in high cost and outer draining.
The content of the invention
It is an object of the invention to provide a kind of for solving lateritic nickel ore to overcome above the deficiencies in the prior art
The problem of the recycling of middle magnesium elements, reduces saving substantial amounts of magnesium mineral resources while production cost, significantly improves enterprise
And social benefit.The magnesium hydroxide of preparation can be back to use during wet processing and make nertralizer to improve the product of other products
Matter, it is also possible to be used as industrial products.
Technical scheme：The invention discloses a kind of produce magnesium-containing waste solution production magnesium hydroxide using lateritic nickel ore wet processing
Process, comprise the steps：
The first step, acidleach operation：Take lateritic nickel ore levigate, be configured to ore pulp, add hydrochloric acid to carry out heated and stirred, then carry out solid
Liquid is separated, and obtains filtrate A；
Second step, remove impurity operation：Above-mentioned filtrate A is carried out into impurity and purification process, described remove impurity refers to different according to each metal
Precipitation pH value, adjusting pH by way of, remove the impurity such as ferrum, nickel, cobalt, manganese in feed liquid.Carry out first except ferrum, except ferrum mistake
Process control PH generates ferrum by adding the alkaline matter such as sodium carbonate or other carbonate in 1.0-4.5, temperature 40-100 DEG C with ferrum
Compound precipitation, Jing solid-liquid separation remove, be purified liquid B.Then in the basic conditions, by adjusting different PH difference
Remove the nickel cobalt manganese in scavenging solution B.Control PH adds the material such as sodium hydroxide or calcium hydroxide in 6.0-8.0, temperature 0-60 DEG C
Hydroxide nickel cobalt precipitation, Jing solid-liquid separation are generated with nickel cobalt reaction to remove；Continuously add sodium hydroxide or calcium hydroxide adjusts PH
In 8.0-9.5, while adding H2O2Or blast air oxidation and generate MnO (OH) 2, Jing solid-liquid separation and remove manganese.Finally give colourless
Transparent Adlerika D.
The preparation of the 3rd step, refined lime breast：Raw material Calx through 30 ~ 1 the 3rd step, the preparation of refined lime breast：
Raw material Calx is carried out step by step after 30 ~ 120min digestion through means such as spiral slag extracting machine, vibrosieve, cyclone hydraulic separators
Prerefining obtains lime cream, i.e. ripening is further refined to lime cream and obtains refined lime breast.
4th step, the preparation of magnesium hydroxide：The lime cream for refining adds anti-simultaneously with magnesium chloride containing, calcium chloride solution C
Device is answered to carry out chemical reaction.
5th step, reaction terminate, and filtration, washing obtain magnesium hydroxide filter cake.
Lateritic nickel ore mog is 60 ~ 120 mesh wherein in the first step.
The ratio that hydrochloric acid is added wherein in the first step is 2 ~ 3 for sour mineral nitrogen amount score ratio.
Heated and stirred temperature is 20 DEG C ~ 90 DEG C wherein in the first step, and the response time is 2 ~ 5 hours.
The lime milk concentration refined in wherein the 4th step is 8% ~ 12%.
The lime cream refined in wherein the 4th step is chemical reaction with the reaction ratio of magnesium chloride containing, calcium chloride solution C
Metering-type mol ratio 0.6 ~ 1.1:1.
Reaction temperature is 25 ~ 60 DEG C in wherein the 4th step, 0.5 ~ 3 hour response time.
The magnesium hydroxide nucleus that early stage generates is placed in reactor as crystal seed in wherein the 4th step.
Beneficial effect：Largely solve low cost and reclaim magnesium resource in lateritic nickel ore, the comprehensive utilization for realizing magnesium is asked
Topic.Solve milk of lime process magnesium sinking, product quality problem not up to standard simultaneously.And the preparation method for traditional magnesium hydroxide is opened
A new process route has been sent out, national magnesium resource has been effectively protected.
Specific embodiment
Embodiment 1
The first step, acidleach operation：Lateritic nickel ore Jing ball mill wet grindings are taken, mog is 100 mesh, ore pulp is configured to, by sour ore deposit
Mass fraction ratio is that 2 ratio adds hydrochloric acid to be stirred, and 50 DEG C are heated to while stirring, and then reaction carries out solid-liquid in 3 hours
Separate, obtain filtrate A；
Second step, remove impurity operation：Above-mentioned filtrate A is carried out into impurity and purification process, described remove impurity refers to different according to each metal
Precipitation pH value, adjusting pH by way of, remove the impurity such as ferrum, nickel, cobalt, manganese in feed liquid.Carry out first except ferrum, except ferrum mistake
Process control PH generates the compound of ferrum by adding the alkaline matter such as sodium carbonate or other carbonate in 2.0, temperature 60 C with ferrum
Precipitation, Jing solid-liquid separation are removed, and are purified liquid B.Then in the basic conditions, purification is removed respectively by adjusting different PH
Nickel cobalt manganese in liquid B.Control PH adds the material such as sodium hydroxide or calcium hydroxide to generate with nickel cobalt reaction in 20 DEG C of 7.0, temperature
Hydroxide nickel cobalt precipitation, Jing solid-liquid separation are removed；Continuously add sodium hydroxide or calcium hydroxide adjusts PH 8.5, while adding
H2O2Or blast air oxidation and generate MnO (OH) 2, Jing solid-liquid separation and remove manganese.Finally give water white Adlerika D.
The preparation of the 3rd step, refined lime breast：Raw material Calx through 30 ~ 1 the 3rd step, the preparation of refined lime breast：
Raw material Calx carries out first time slag-liquid separation Jing after 90min digestion into spiral slag extracting machine, and rough lime cream is with being pumped into shaking
Dynamic sieve carries out second slag-liquid separation, then through cyclone hydraulic separators carries out third time slag-liquid separation again, through three slag liquid point
Prerefining lime cream after carries out again ageing 5 hours in ageing tank, obtains qualified refined lime breast.
4th step, the preparation of magnesium hydroxide：The lime cream for refining is with magnesium chloride containing, calcium chloride solution C stoichiometrically
0.8 times of formula is added in successive reaction kettle and carries out successive reaction simultaneously, and reaction temperature is 40 DEG C, and the response time is 2 hours.
5th step, reaction carry out three countercurrent washings and solid-liquid separation after terminating, the magnesium hydroxide filter cake for obtaining.
Note：Ore used in embodiment originates from Indonesia or Filipine lateritic nickel ore, and lateritic nickel ore used is just like table 1 below
Listed Main Ingredients and Appearance：The magnesium hydroxide composition of preparation is shown in Table 2；
Embodiment 2
The first step, acidleach operation：Lateritic nickel ore Jing ball mill wet grindings are taken, mog is 90 mesh, ore pulp is configured to, by sour mineral nitrogen
Amount score ratio is that 2 ratio adds hydrochloric acid to be stirred, and 45 DEG C are heated to while stirring, and then reaction carries out solid-liquid point in 3 hours
From obtaining filtrate A；
Second step, remove impurity operation：Above-mentioned filtrate A is carried out into impurity and purification process, described remove impurity refers to different according to each metal
Precipitation pH value, adjusting pH by way of, remove the impurity such as ferrum, nickel, cobalt, manganese in feed liquid.Carry out first except ferrum, except ferrum mistake
Process control PH generates the compound of ferrum by adding the alkaline matter such as sodium carbonate or other carbonate in 80 DEG C of 1.5, temperature with ferrum
Precipitation, Jing solid-liquid separation are removed, and are purified liquid B.Then in the basic conditions, purification is removed respectively by adjusting different PH
Nickel cobalt manganese in liquid B.Control PH adds the material such as sodium hydroxide or calcium hydroxide to generate with nickel cobalt reaction in 30 DEG C of 6.5, temperature
Hydroxide nickel cobalt precipitation, Jing solid-liquid separation are removed；Continuously add sodium hydroxide or calcium hydroxide adjusts PH 8.2, while adding
H2O2Or blast air oxidation and generate MnO (OH) 2, Jing solid-liquid separation and remove manganese.Finally give water white Adlerika D.
The preparation of the 3rd step, refined lime breast：Raw material Calx Jing after 90min digestion, into spiral slag extracting machine the is carried out
Slag-liquid separation, rough lime cream carries out second slag-liquid separation with vibrosieve is pumped into, then again through rotary filter press
Device carries out third time slag-liquid separation, and it is little that the prerefining lime cream after three slag-liquid separations carries out again ageing 3 in ageing tank
When, obtain qualified refined lime breast.
4th step, the preparation of magnesium hydroxide：The lime cream for refining is with magnesium chloride containing, calcium chloride solution C stoichiometrically
0.8 times of formula is added in successive reaction kettle and carries out successive reaction simultaneously, and reaction temperature is 40 DEG C, and the response time is 2 hours.
5th step, reaction carry out three countercurrent washings and solid-liquid separation after terminating, the magnesium hydroxide filter cake for obtaining.
Note：Ore used in embodiment originates from Indonesia or Filipine lateritic nickel ore, and lateritic nickel ore used is just like table 3 below
Listed Main Ingredients and Appearance：
Embodiment 3
The first step, acidleach operation：Lateritic nickel ore Jing ball mill wet grindings are taken, mog is 100 mesh, ore pulp is configured to, by sour ore deposit
Mass fraction ratio is that 2 ratio adds hydrochloric acid to be stirred, and 50 DEG C are heated to while stirring, and then reaction carries out solid-liquid in 3 hours
Separate, obtain filtrate A；
Second step, remove impurity operation：Above-mentioned filtrate A is carried out into impurity and purification process, described remove impurity refers to different according to each metal
Precipitation pH value, adjusting pH by way of, remove the impurity such as ferrum, nickel, cobalt, manganese in feed liquid.Carry out first except ferrum, except ferrum mistake
Process control PH generates the compound of ferrum by adding the alkaline matter such as sodium carbonate or other carbonate in 82 DEG C of 3.2, temperature with ferrum
Precipitation, Jing solid-liquid separation are removed, and are purified liquid B.Then in the basic conditions, purification is removed respectively by adjusting different PH
Nickel cobalt manganese in liquid B.Control PH adds the material such as sodium hydroxide or calcium hydroxide to generate with nickel cobalt reaction in 7.5, temperature 45 C
Hydroxide nickel cobalt precipitation, Jing solid-liquid separation are removed；Continuously add sodium hydroxide or calcium hydroxide adjusts PH 9.0, while adding
H2O2Or blast air oxidation and generate MnO (OH) 2, Jing solid-liquid separation and remove manganese.Finally give water white Adlerika D.
The preparation of the 3rd step, refined lime breast：Raw material Calx Jing after 120min digestion, into spiral slag extracting machine the is carried out
Slag-liquid separation, rough lime cream carries out second slag-liquid separation with vibrosieve is pumped into, then again through rotary filter press
Device carries out third time slag-liquid separation, and it is little that the prerefining lime cream after three slag-liquid separations carries out again ageing 4 in ageing tank
When, obtain qualified refined lime breast.
4th step, the preparation of magnesium hydroxide：The lime cream for refining is with magnesium chloride containing, calcium chloride solution C stoichiometrically
0.8 times of formula is added in successive reaction kettle and carries out successive reaction simultaneously, and reaction temperature is 40 DEG C, and the response time is 2 hours.
5th step, reaction carry out three countercurrent washings and solid-liquid separation after terminating, the magnesium hydroxide filter cake for obtaining.
Note：Ore used in embodiment originates from Indonesia or Filipine lateritic nickel ore, and lateritic nickel ore used is just like table 4 below
Listed Main Ingredients and Appearance：
The magnesium hydroxide filter cake product quality prepared in embodiment meets the filter cake shape hydrogen of industry standard HY/T111-2008
Magnesium oxide.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of utilization lateritic nickel ore wet processing produces the process that magnesium-containing waste solution produces magnesium hydroxide, it is characterised in that
Comprise the steps：
The first step, acidleach operation：Take lateritic nickel ore levigate, be configured to ore pulp, add hydrochloric acid to carry out heated and stirred, then carry out solid
Liquid is separated, and obtains filtrate A；
Second step, remove impurity operation：Above-mentioned filtrate A is carried out into impurity and purification process, described remove impurity refers to different according to each metal
Precipitation pH value, adjusting pH by way of, remove the impurity such as ferrum, nickel, cobalt, manganese in feed liquid；
Carry out first except ferrum, iron removal controls PH in 1.0-4.5, temperature 40-100 DEG C, by adding sodium carbonate or other carbon
The alkaline matters such as hydrochlorate generate the compound precipitation of ferrum, Jing solid-liquid separation with ferrum and remove, and are purified liquid B；
Then in the basic conditions, the nickel cobalt manganese in scavenging solution B is removed respectively by the different PH of regulation；
Control PH adds the material such as sodium hydroxide or calcium hydroxide to generate hydrogen-oxygen with nickel cobalt reaction in 6.0-8.0, temperature 0-60 DEG C
Change nickel cobalt precipitation, Jing solid-liquid separation to remove；Continuously add sodium hydroxide or calcium hydroxide adjusts PH in 8.0-9.5, while adding
H2O2Or blast air oxidation and generate MnO (OH) 2, Jing solid-liquid separation and remove manganese；Finally give water white Adlerika D；
The preparation of the 3rd step, refined lime breast：Raw material Calx after 30 ~ 120min digestion, through spiral slag extracting machine, vibration
The means such as screening, cyclone hydraulic separators carry out step by step prerefining and obtain lime cream, further refine i.e. ripening to lime cream and obtain
To refined lime breast；
4th step, the preparation of magnesium hydroxide：The lime cream for refining is with magnesium chloride containing, calcium chloride solution C while adding reactor
Carry out chemical reaction；
5th step, reaction terminate, and filtration, washing obtain magnesium hydroxide filter cake.
2. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that lateritic nickel ore mog is 60 ~ 120 mesh in the described first step first step.
3. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that the ratio that hydrochloric acid is added in the described first step is 2 ~ 3 for sour mineral nitrogen amount score ratio.
4. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that heated and stirred temperature is 20 DEG C ~ 90 DEG C in the described first step, the response time is 2 ~ 5 hours.
5. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that the lime milk concentration refined in the 4th described step is 8% ~ 12%.
6. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that the lime cream refined in the 4th described step and magnesium chloride containing, the reaction ratio of calcium chloride solution C
Example is stoichiometric equation of chemical reaction mol ratio 0.6 ~ 1.1:1.
7. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that reaction temperature is 25 ~ 60 DEG C in the 4th described step, 0.5 ~ 3 hour response time.
8. a kind of utilization lateritic nickel ore wet processing according to claim 1 produces the work that magnesium-containing waste solution produces magnesium hydroxide
Process, it is characterised in that the magnesium hydroxide nucleus that early stage generates is placed in reactor as crystal seed in the 4th described step.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611014237.0A CN106673025A (en) | 2016-11-18 | 2016-11-18 | Technological method for producing magnesium hydroxide by utilization of magnesium-containing wastewater generated by laterite nickel ore wet-process |
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| CN201611014237.0A CN106673025A (en) | 2016-11-18 | 2016-11-18 | Technological method for producing magnesium hydroxide by utilization of magnesium-containing wastewater generated by laterite nickel ore wet-process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328659A (en) * | 2018-02-23 | 2018-07-27 | 北京科技大学 | A kind of method that integrated treatment utilizes high magnesium ferronickel slag |
| WO2020019918A1 (en) * | 2018-07-24 | 2020-01-30 | 眉山顺应动力电池材料有限公司 | Method for homogeneous precipitation separation of nickel, cobalt and manganese from laterite nickel ore acid leaching solution |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050411A (en) * | 1989-09-20 | 1991-04-03 | 中国人民解放军信阳陆军学院训练部科研处 | The comprehensive utilization of serpentine tailing |
| CN103290213A (en) * | 2013-05-21 | 2013-09-11 | 胡雷 | Process for recycling valuable metal from nickel laterite ores and simultaneously by-producing anhydrous calcium chloride |
-
2016
- 2016-11-18 CN CN201611014237.0A patent/CN106673025A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050411A (en) * | 1989-09-20 | 1991-04-03 | 中国人民解放军信阳陆军学院训练部科研处 | The comprehensive utilization of serpentine tailing |
| CN103290213A (en) * | 2013-05-21 | 2013-09-11 | 胡雷 | Process for recycling valuable metal from nickel laterite ores and simultaneously by-producing anhydrous calcium chloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328659A (en) * | 2018-02-23 | 2018-07-27 | 北京科技大学 | A kind of method that integrated treatment utilizes high magnesium ferronickel slag |
| WO2020019918A1 (en) * | 2018-07-24 | 2020-01-30 | 眉山顺应动力电池材料有限公司 | Method for homogeneous precipitation separation of nickel, cobalt and manganese from laterite nickel ore acid leaching solution |
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