CN104402027A - Method for extraction of ludwigite from low-grade paigeite - Google Patents
Method for extraction of ludwigite from low-grade paigeite Download PDFInfo
- Publication number
- CN104402027A CN104402027A CN201410609124.XA CN201410609124A CN104402027A CN 104402027 A CN104402027 A CN 104402027A CN 201410609124 A CN201410609124 A CN 201410609124A CN 104402027 A CN104402027 A CN 104402027A
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- CN
- China
- Prior art keywords
- filtrate
- paigeite
- iron
- magnesium
- boron
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1045—Oxyacids
- C01B35/1054—Orthoboric acid
- C01B35/1063—Preparation from boron ores or borates using acids or salts
-
- 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
- C01F5/40—Magnesium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention relates to a method for extraction of ludwigite from low-grade paigeite, and the method comprises the following steps: adding paigeite powder into a three-mouth flask, wetting into a paste by a small amount of distilled water, then adding H2SO4 solution into the flask, stirring for reaction in a water bath, then filtering; adding a small amount of H2O2 into the filtrate to oxidize Fe<2 +> in the filtrate, adjusting the pH value of the filtrate by MgO, then adding a certain amount of anhydrous ethanol for crystallization, filtering to obtain magnesium sulfate solid; collecting the filtrate with magnesium extracted, distilling for recovery of ethanol, adding proper amount of scrap iron in distilled liquid, filtering and adjusting the pH value; adding anhydrous ethanol into the solution for crystallization, quick filtering by suck to obtain ferrous sulfate solid; after distillation recovery of ethanol in the extracting iron filtrate, continuing evaporation and concentration of distilled liquid, crystallizing the concentrated solution at low temperature to obtain the ludwigite, collecting boron extraction mother liquor for a plurality of times, and repeatedly recycling. The method is relatively-mild in operating conditions, low in energy consumption and high in extraction rate, and the used ethanol can be distilled for recovery.
Description
Technical field
The present invention relates to a kind of paigeite extractive technique, particularly relate in a kind of low-grade paigeite and extract boron magnesium iron method.
Background technology
Although the boron resource of China enriches, being that boron samples lower poor boron mineral mostly, is wherein maximum with paigeite.Only the paigeite reserves of Liaoning Area, northeast are just up to 2.8 hundred million tons, wherein B
2o
3reserves reach 2,814 ten thousand tons, account for 58% of national boron resource total reserves.Magnesium in paigeite ore, iron level are higher, and main valuable mineral is szaibelyite and magnetite, and gangue mineral is serpentine and clinohumite, and trace quantity mineral is uraninite and boron magnesium ore deposit.Because essential mineral symbiotic relationship is very close, crystal stock is complicated, and development difficulty is large, and complete processing is complicated, not yet has highly effective method extraction and isolation boron, magnesium and iron from paigeite at present.Along with exploitation for many years, the reserves being easy to the boron magnesium stone ore exploited sharply reduce, and can not meet the demand of China's boron industry.So, accelerate development the exploitation to paigeite, the boron resource of China can not only be made full use of, and the raw material pressure alleviating China's boronation industry is had great significance.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of method operational condition is relatively gentle, and energy consumption is lower, and extraction yield is high, and ethanol used can Distillation recovery.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: extract boron magnesium iron method in a kind of low-grade paigeite, comprise the steps:
Paigeite powder is put into there-necked flask, soaks into pasty state with a small amount of distilled water, then add H in flask
2sO
4solution, filters after stirring reaction in a water bath;
A small amount of H is added in filtrate
2o
2with oxidation Fe wherein
2+, then the pH value of filtrate is regulated with MgO, then add a certain amount of dehydrated alcohol crystallization, filtration can obtain magnesium sulfate solid;
Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds appropriate waste iron filing in distillate, after filtration with adjust ph after;
In solution, add dehydrated alcohol crystallization, then rapid filtration under suction obtains ferrous sulfate solid;
Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization under low temperature, obtains boron magnesium iron, collects and repeatedly carries boron mother liquor, repeats to reclaim.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described paigeite powder is put into there-necked flask, soak into pasty state with a small amount of distilled water, then add H in flask
2sO
4solution, being in a water bath implemented as follows of filtration step after stirring reaction:
The paigeite powder taking 10 ~ 20g puts into there-necked flask, soaks into pasty state with a small amount of distilled water, then adds 58.8 ~ 60mL30%H in flask
2sO
4solution, filters after 80 ~ 90 DEG C of stirred in water bath reaction 110 ~ 125min.
Further, describedly in solution, add dehydrated alcohol crystallization, then rapid filtration under suction obtains being implemented as follows of ferrous sulfate solid step:
1 ~ 2g30%H is added in filtrate
2o
2with oxidation Fe wherein
2+, then regulate the pH value of filtrate to be 7 ~ 8 with MgO, then add the dehydrated alcohol crystallization of 10 ~ 20ml, filtration can obtain magnesium sulfate solid.
Further, the filtrate after magnesium is carried in described collection, and Distillation recovery ethanol adds appropriate waste iron filing in distillate, after filtration with adjust ph after being implemented as follows of step:
Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds the waste iron filing of 5 ~ 9g in distillate, is 7 ~ 8 after filtration with adjust ph.
Further, described in carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization under low temperature, obtains boron magnesium iron, collects and repeatedly carries boron mother liquor, repeats being implemented as follows of recycling step:
Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization at low temperature is less than 10 DEG C, can obtain boric acid product, finally collect and repeatedly carry boron mother liquor, repeats to reclaim.
The invention has the beneficial effects as follows: method operational condition is relatively gentle, and energy consumption is lower, and extraction yield is high, and ethanol used can Distillation recovery.
Embodiment
Be described principle of the present invention and feature below in conjunction with embodiment, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Extract boron magnesium iron method in a kind of low-grade paigeite, comprise the steps:
Paigeite powder is put into there-necked flask, soaks into pasty state with a small amount of distilled water, then add H in flask
2sO
4solution, filters after stirring reaction in a water bath;
A small amount of H is added in filtrate
2o
2with oxidation Fe wherein
2+, then the pH value of filtrate is regulated with MgO, then add a certain amount of dehydrated alcohol crystallization, filtration can obtain magnesium sulfate solid;
Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds appropriate waste iron filing in distillate, after filtration with adjust ph after;
In solution, add dehydrated alcohol crystallization, then rapid filtration under suction obtains ferrous sulfate solid;
Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization under low temperature, obtains boron magnesium iron, collects and repeatedly carries boron mother liquor, repeats to reclaim.
Embodiment 1:
The paigeite powder taking 10g puts into there-necked flask, soaks into pasty state with a small amount of distilled water, then adds 58.8mL30%H in flask
2sO
4solution, filters after 80 DEG C of stirred in water bath reaction 110min; 1g30%H is added in filtrate
2o
2with oxidation Fe wherein
2+, then regulate the pH value of filtrate to be 7 with MgO, then add the dehydrated alcohol crystallization of 10ml, filtration can obtain magnesium sulfate solid; Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds the waste iron filing of 5g in distillate, is 7 after filtration with adjust ph; Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization at low temperature 10 DEG C, can obtain boric acid product, finally collect and repeatedly carry boron mother liquor, repeats to reclaim.
Embodiment 2:
The paigeite powder taking 15g puts into there-necked flask, soaks into pasty state with a small amount of distilled water, then adds 59mL30%H in flask
2sO
4solution, filters after 85 DEG C of stirred in water bath reaction 118min; 1.5g30%H is added in filtrate
2o
2with oxidation Fe wherein
2+, then regulate the pH value of filtrate to be 7.5 with MgO, then add the dehydrated alcohol crystallization of 15ml, filtration can obtain magnesium sulfate solid; Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds the waste iron filing of 6g in distillate, is 7.5 after filtration with adjust ph; Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization at low temperature 8 DEG C, can obtain boric acid product, finally collect and repeatedly carry boron mother liquor, repeats to reclaim.
Embodiment 3:
The paigeite powder taking 20g puts into there-necked flask, soaks into pasty state with a small amount of distilled water, then adds 60mL30%H in flask
2sO
4solution, filters after 90 DEG C of stirred in water bath reaction 125min; 2g30%H is added in filtrate
2o
2with oxidation Fe wherein
2+, then regulate the pH value of filtrate to be 8 with MgO, then add the dehydrated alcohol crystallization of 20ml, filtration can obtain magnesium sulfate solid; Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds the waste iron filing of 9g in distillate, is 8 after filtration with adjust ph; Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization at low temperature 6 DEG C, can obtain boric acid product, finally collect and repeatedly carry boron mother liquor, repeats to reclaim.
Claims (5)
1. extract a boron magnesium iron method in low-grade paigeite, it is characterized in that, comprise the steps:
Paigeite powder is put into there-necked flask, soaks into pasty state with a small amount of distilled water, then add H in flask
2sO
4solution, filters after stirring reaction in a water bath;
A small amount of H is added in filtrate
2o
2with oxidation Fe wherein
2+, then the pH value of filtrate is regulated with MgO, then add a certain amount of dehydrated alcohol crystallization, filtration can obtain magnesium sulfate solid;
Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds appropriate waste iron filing in distillate, after filtration with adjust ph after;
In solution, add dehydrated alcohol crystallization, then rapid filtration under suction obtains ferrous sulfate solid;
Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization under low temperature, obtains boron magnesium iron, collects and repeatedly carries boron mother liquor, repeats to reclaim.
2. extract boron magnesium iron method in a kind of low-grade paigeite according to claim 1, it is characterized in that, described paigeite powder is put into there-necked flask, soak into pasty state with a small amount of distilled water, then add H in flask
2sO
4solution, being in a water bath implemented as follows of filtration step after stirring reaction:
The paigeite powder taking 10 ~ 20g puts into there-necked flask, soaks into pasty state with a small amount of distilled water, then adds 58.8 ~ 60mL30%H in flask
2sO
4solution, filters after 80 ~ 90 DEG C of stirred in water bath reaction 110 ~ 125min.
3. extracts boron magnesium iron method in a kind of low-grade paigeite according to claim 1, it is characterized in that, describedly in solution, add dehydrated alcohol crystallization, then rapid filtration under suction obtains being implemented as follows of ferrous sulfate solid step:
1 ~ 2g30%H is added in filtrate
2o
2with oxidation Fe wherein
2+, then regulate the pH value of filtrate to be 7 ~ 8 with MgO, then add the dehydrated alcohol crystallization of 10 ~ 20ml, filtration can obtain magnesium sulfate solid.
4. extract boron magnesium iron method in a kind of low-grade paigeite according to claim 1, it is characterized in that, the filtrate after magnesium is carried in described collection, Distillation recovery ethanol, in distillate, add appropriate waste iron filing, after filtration with adjust ph after being implemented as follows of step:
Collect the filtrate carried after magnesium, Distillation recovery ethanol, adds the waste iron filing of 5 ~ 9g in distillate, is 7 ~ 8 after filtration with adjust ph.
5. extract boron magnesium iron method in a kind of low-grade paigeite according to claim 1, it is characterized in that, describedly carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization under low temperature, obtain boron magnesium iron, collect and repeatedly carry boron mother liquor, repeat being implemented as follows of recycling step:
Carry iron filtrate after Distillation recovery ethanol, distillate continues evaporation concentration, by concentrated solution crystallization at low temperature is less than 10 DEG C, can obtain boric acid product, finally collect and repeatedly carry boron mother liquor, repeats to reclaim.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410609124.XA CN104402027A (en) | 2014-10-31 | 2014-10-31 | Method for extraction of ludwigite from low-grade paigeite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410609124.XA CN104402027A (en) | 2014-10-31 | 2014-10-31 | Method for extraction of ludwigite from low-grade paigeite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104402027A true CN104402027A (en) | 2015-03-11 |
Family
ID=52639714
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410609124.XA Pending CN104402027A (en) | 2014-10-31 | 2014-10-31 | Method for extraction of ludwigite from low-grade paigeite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104402027A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036162A (en) * | 2015-08-21 | 2015-11-11 | 东北大学 | Paigeite comprehensive utilization method for separating and extracting boron, magnesium and iron |
| CN109665568A (en) * | 2019-01-09 | 2019-04-23 | 无锡日月水处理有限公司 | A kind of extraction method of purification of ferrous iron |
-
2014
- 2014-10-31 CN CN201410609124.XA patent/CN104402027A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036162A (en) * | 2015-08-21 | 2015-11-11 | 东北大学 | Paigeite comprehensive utilization method for separating and extracting boron, magnesium and iron |
| CN105036162B (en) * | 2015-08-21 | 2016-11-30 | 东北大学 | A kind of paigeite method of comprehensive utilization of separation and Extraction boron magnesium ferrum |
| CN109665568A (en) * | 2019-01-09 | 2019-04-23 | 无锡日月水处理有限公司 | A kind of extraction method of purification of ferrous iron |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150311 |
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| WD01 | Invention patent application deemed withdrawn after publication |