CN106467314A - Prepare light magnesium oxide and the technique of micron order calcium carbonate powder using bitter alkali water - Google Patents
Prepare light magnesium oxide and the technique of micron order calcium carbonate powder using bitter alkali water Download PDFInfo
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- CN106467314A CN106467314A CN201610889334.8A CN201610889334A CN106467314A CN 106467314 A CN106467314 A CN 106467314A CN 201610889334 A CN201610889334 A CN 201610889334A CN 106467314 A CN106467314 A CN 106467314A
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- calcium carbonate
- water
- micron order
- technique according
- magnesium oxide
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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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- 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
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Abstract
The invention discloses a kind of use bitter alkali water prepares light magnesium oxide and the technique of micron order calcium carbonate powder, including：1）Take picrin water filtration；2）Under stirring, add soluble carbonate salt to be simultaneously added dropwise hydrochloric acid in the bitter alkali water to after filter and keep pH value of solution<10, the control response time is 10 40min, after the completion of reaction, filters, residue washing, drying, obtains micron order Calcium Carbonate；3）To step 2）In the filtrate obtaining after filtration, add water soluble alkali, produce Mg (OH)2Precipitation, dries and forms Mg (OH)2；4）Step 3）Gained Mg (OH)2Calcine at 450 600 DEG C, you can prepared lightweight active oxidation magnesium granules.The present invention is reasonable in design, and energy consumption is low, can effectively utilize bitter alkali water and micron order Calcium Carbonate and light magnesium oxide powder body be obtained for raw material, purity can reach more than 93%, can significantly reduce the impact to environment for the bitter alkali water, and produce economic benefit.
Description
Technical field
The present invention relates to a kind of use bitter alkali water prepares light magnesium oxide and the technique of micron order calcium carbonate powder.
Background technology
In the water of bitter alkali water, salinity content is higher, and the main component of salinity is calcium, magnesium, the heavy carbonate of sodium, chlorination
Thing and sulfate.
A kind of industrial particularly important inorganic chemicals industry product of light magnesium oxide, is mainly used in refractory material, magnesium metal
Refinement, high function fine inorganic material, ink, harmful gass adsorbent, paper pulp, carry the fields such as uranium, construction material.Additionally should
For medicine, food, military project and electron trade.
Micron order Calcium Carbonate is also a kind of important inorganic material, is widely used in rubber, plastics, coating, papermaking, building
Etc. industry, larger to the demand of this product.Domestic predominant methods are dolomite carbonizatin method at present, but because dolomite is solid
Body mineral, impurity content is high, and Calcium Carbonate separating-purifying process is complicated, and cost of investment is high, and unstable product quality, and deposit
In high energy consumption, have the shortcomings that certain environment pollution, waste sludge discharge amount are big.Calcium Carbonate, due to the difference of synthetic method, has difference
Size and crystal formation and physicochemical properties, thus there are different purposes, micron order Calcium Carbonate is due to having preferable physics
Characteristic, is with a wide range of applications in different field.
Content of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide one kind prepares light magnesium oxide using bitter alkali water
Technique with micron order calcium carbonate powder.This technique can make full use of the Mg in bitter alkali water2+And Ca2+, it is obtained and meet industrial wanting
The high value added product asked.This technical process energy consumption is low, high efficiency, popularization convenient to carry out.
For achieving the above object, the present invention takes technical scheme below：
What the present invention provided prepares light magnesium oxide and the technique of micro-calcium carbonate powder body using bitter alkali water, comprises the steps：
1）Filter：Take picrin water filtration, remove suspended impurity；
2）Micron order precipitation of calcium carbonate：Under quick stirring, in the bitter alkali water to after filter, soluble carbonate salt is added to be simultaneously added dropwise
Hydrochloric acid keeps pH value of solution<10, the control response time is 10-40min, after the completion of reaction, filters, residue washing, drying, obtains micro-
Meter level Calcium Carbonate；
3）Mg(OH)2Precipitation：To step 2）In the filtrate obtaining after filtration, add water soluble alkali, produce Mg (OH)2Precipitation, dries
Form becomes Mg (OH)2；
4）The preparation of light magnesium oxide：Step 3）Gained Mg (OH)2Calcine at 450-600 DEG C, you can prepared lightweight active oxygen
Change magnesium granules.
Preferably, described soluble carbonate salt is Na2CO3Or K2CO3.
Preferably, described water soluble alkali is NaOH or KOH.
Preferably, step 2）In, according to Ca2+：CO3 2-=1:0.5 ~ 1 ratio adds soluble carbonate salt.
Preferably, step 2）In middle soluble carbonate salt, the concentration of carbonate is 0.1 ~ 10 mol/L.
Preferably, step 3）The concentration of middle water soluble alkali is 1 ~ 50 mol/L.
Preferably, step 3）After middle addition water soluble alkali, under the conditions of 20-30 DEG C, react 10-30min, produce Mg (OH)2
Precipitation.
Preferably, step 4）Middle calcination time is 1 ~ 2h.
Preferably, step 2）Middle Deca hydrochloric acid keeps pH value of solution between 9 ~ 10.
Preferably, step 1）The hydraulic screen of middle below use aperture 1mm is filtered.
It is an advantage of the invention that preparing light magnesium oxide and micron order Calcium Carbonate technological design rationally using bitter alkali water, energy consumption
Low, prepared light magnesium oxide and pure calcium carbonate are all more than 95%, and can significantly reduce the shadow for environment for the bitter alkali water
Ring, be worthy to be popularized enforcement.
Brief description
Fig. 1 prepares light magnesium oxide and the process chart of micron order Calcium Carbonate for the present invention's using bitter alkali water.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, so that those skilled in the art is permissible
It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
The invention provides a kind of use bitter alkali water prepares light magnesium oxide and the technique of micron order calcium carbonate powder.Pass through
It is used somewhere bitter alkali water as raw materials for production, main component is MgCl2And CaCl2、MgSO4.
The sub-terrain mines well water that bitter alkali water used by the present invention produces during coming from mine coal-cutting, through preliminary pretreatment
It is emitted into ground, form aqueous alkali lake.This lake water calcium ions and magnesium ions concentration is high, salinity is high, by using this bitter alkali water, can be effective
Ground reduces the hardness in water body, and produces the magnesium oxide with economic worth and Calcium Carbonate.The present invention uses coal mining process
The waste water of middle generation is recycled.
The technique of the present invention, specifically includes following steps：
1）Filter：Take picrin water filtration, remove suspended impurity；
2）Micron order precipitation of calcium carbonate：Under quick stirring, in the bitter alkali water to after filter, soluble carbonate salt is added to be simultaneously added dropwise
Hydrochloric acid keeps pH value of solution<10, the control response time is 10-40min, after the completion of reaction, filters, residue washing, drying, obtains micro-
Meter level Calcium Carbonate；Bitter alkali water produces muddiness after being passed through sodium carbonate immediately, now produces a large amount of nanometer grade calcium carbonate nucleus, now needs
Regulate and control reaction pH<10 and quickly stir, control the response time in 10-40min, prevent nucleus from overrunning growth, formation grade
Granule.
3）Mg(OH)2Precipitation：To step 2）In the filtrate obtaining after filtration, add water soluble alkali, produce Mg (OH)2Precipitation,
Dry and form Mg (OH)2；
4）The preparation of light magnesium oxide：Step 3）Gained Mg (OH)2Calcine at 450-600 DEG C, you can prepared lightweight active oxygen
Change magnesium granules.
A kind of use bitter alkali water of the present invention prepares light magnesium oxide and the technique of micron order calcium carbonate powder, using picrin
Water is raw materials for production, and whole production process includes the filtration treatment of raw water, the precipitation preparation of micron order Calcium Carbonate, magnesium hydroxide
The calcination process such as preparation and magnesium hydroxide.
After bitter alkali water raw water is filtered, according to Ca2+：CO3 2-=1:0.5 ~ 1 ratio is added thereto to 1mol/L's
Na2CO3Mix and blend 10 ~ 40min, and it is simultaneously added dropwise the HCl of 0.1mol/L, in order to control pH value in reaction to be located between 9 ~ 10, will
Micron order calcium carbonate powder is produced after precipitation filtering and concentrating, drying.
Calcium Carbonate production technology in this technique, including by Na2CO3It is passed through mix and blend in solution and reacts 10 ~ 40min, obtain final product
Precipitation of calcium carbonate, precipitation, filter, be dried after can be prepared by micron order Calcium Carbonate.
By the filtrate after micron order precipitation of calcium carbonate according to NaOH:Mg2+=1.5-2:1 ratio NaOH, reacts 10-
30min, filter cake obtains light magnesium oxide powder body through washing, being dried to obtain magnesium hydrate precipitate, precipitation through calcining.
Magnesium hydroxide calcination process：Dried magnesium hydroxide is calcined under the conditions of 450 ~ 600 DEG C 1 ~ 2h, that is, be obtained light
Matter magnesium oxide product.
A kind of use bitter alkali water of the present invention prepares the picrin in light magnesium oxide and the technique of micron order calcium carbonate powder
Ca in water raw water2+And Mg2+Concentration be about 20mmol/L and 32mmol/L.
The residual filtrate of the present invention predominantly contains the saline solution of a small amount of calcium ions and magnesium ions, and main component is NaCl and Na2SO4,
Can serve as reverse osmosiss or sodium filters the raw water of desalination process.
With specific embodiment, the present invention is further described below：
Bitter alkali water raw water quality situation analysis table used by the present embodiment, is shown in Table 1：
| Inspection project | Unit | Assay | Inspection project | Unit | Assay |
| Sodium | mg/L | 1159 | Nitrate（In terms of N） | mg/L | <0.16 |
| Calcium | mg/L | 775.7 | Total dissolved solid | mg/L | 15180 |
| Magnesium | mg/L | 705.8 | Strontium | mg/L | |
| Ferrum | mg/L | <0.020 | Barium | mg/L | 0.0248 |
| Manganese | mg/L | 0.018 | Float | mg/L | 7 |
| Chloride（Cl―） | mg/L | 5522.9 | Petroleum-type | mg/L | <0.03 |
| Sulfate（SO42-） | mg/L | 6216.6 | Excrement colibacillus group | Individual/L | 0 |
| Carbonate（CO32-） | mg/L | 0.00 | Total phosphorus（In terms of P） | mg/L | 0.02 |
| Heavy carbonate（HCO3-） | mg/L | 167.96 | Ammonia nitrogen（In terms of N） | mg/L | 0.26 |
| PH value | 8.11 | Silicon dioxide（In terms of SiO2） | mg/L | 8.31 | |
| Total hardness (CaCO3Meter) | mg/L | 4844 | Turbidity | NTU | 0.3 |
| Total alkalinity (CaCO3Meter) | mg/L | 138 |
Raw water, after preliminary filtration, under stirring, adds Na in raw water2CO3React 10 ~ 40min, Ca at room temperature2+:
CO3 2-Molar ratio is 1:0.625, add 0.1mol/L HCl simultaneously, adjust pH between 9 ~ 10, produce after the reaction of 500mL raw water
Raw 0.58g precipitation, after filtration, filtering residue, with water washing, is dried at 105 DEG C and is produced micron order Calcium Carbonate（After testing, particle diameter 50 ~
150 microns）, the purity of micron order Calcium Carbonate is 97% after testing.（Not excessive using carbonate concentration, it is because that carbonate is dense
Spend height to be possible to produce carbonic acid magnesium precipitate, precipitating purity is not high, has magnesium carbonate contamination precipitation.）.
Filtrate after filtration is according to NaOH:Mg2+=1.5~2:1 ratio adds the NaOH solution that concentration is 1 ~ 10mol/L, enters
There is precipitation after row mixing, the response time controls in 10-30min, precipitation is carried out filtering cleaning, after being dried, puts into 450-
Carry out in 600 DEG C of Muffle furnace calcining 1 ~ 2h, be finally made light magnesium oxide powder body (when drying temperature is more than 370 DEG C
Generate light magnesium oxide, the quality of product does not change when temperature is higher than 600 DEG C, therefore general in common application
Using 450-600 DEG C).After testing, the purity of light magnesium oxide powder body is 93.1% ~ 98.1%..
Above content is the further description made with reference to specific preferred embodiment it is impossible to assert this
Invention is embodied as being confined to these explanations above-mentioned.For general technical staff of the technical field of the invention,
On the premise of present inventive concept, some simple modifications or replacement can also be made, all should be considered as belonging to the present invention's
Protection domain.
Claims (10)
1. a kind of use bitter alkali water prepares the technique of light magnesium oxide and micro-calcium carbonate powder body it is characterised in that including as follows
Step：
1）Filter：Take picrin water filtration, remove suspended impurity；
2）Micron order precipitation of calcium carbonate：Under stirring, in the bitter alkali water to after filter, soluble carbonate salt is added to be simultaneously added dropwise hydrochloric acid
Keep pH value of solution<10, the control response time is 10-40min, after the completion of reaction, filters, residue washing, drying, obtains micron order
Calcium Carbonate；
3）Mg(OH)2Precipitation：To step 2）In the filtrate obtaining after filtration, add water soluble alkali, produce Mg (OH)2Precipitation, dries
Form Mg (OH)2；
4）The preparation of light magnesium oxide：Step 3）Gained Mg (OH)2Calcine at 450-600 DEG C, you can prepared lightweight active oxidation
Magnesium granules.
2. technique according to claim 1 is it is characterised in that described soluble carbonate salt is Na2CO3Or K2CO3.
3. technique according to claim 1 is it is characterised in that described water soluble alkali is NaOH or KOH.
4. technique according to claim 1 is it is characterised in that step 2）In, according to Ca2+：CO3 2-=1:0.5 ~ 1 mole
Ratio adds soluble carbonate salt.
5. technique according to claim 1 is it is characterised in that step 2）In middle soluble carbonate salt, the concentration of carbonate is
0.1~10 mol/L.
6. technique according to claim 1 is it is characterised in that step 3）The concentration of middle water soluble alkali is 1 ~ 50 mol/L.
7. technique according to claim 1 is it is characterised in that step 3）After middle addition water soluble alkali, in 20-30 DEG C of condition
Lower reaction 10-30min, produces Mg (OH)2Precipitation.
8. technique according to claim 1 is it is characterised in that step 4）Middle calcination time is 1 ~ 2h.
9. technique according to claim 1 is it is characterised in that step 2）Middle Deca hydrochloric acid keep pH value of solution 9 ~ 10 it
Between.
10. technique according to claim 1 is it is characterised in that step 1）The hydraulic screen of middle below use aperture 1mm is carried out
Filter.
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| CN201610889334.8A CN106467314A (en) | 2016-10-12 | 2016-10-12 | Prepare light magnesium oxide and the technique of micron order calcium carbonate powder using bitter alkali water |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4038365A (en) * | 1975-12-03 | 1977-07-26 | Basf Wyandotte Corporation | Removal of low level hardness impurities from brine feed to chlorine cells |
| CN85105048A (en) * | 1985-07-04 | 1986-12-31 | 金寿培 | Effluent brine reclaims and the recycle method |
| US20110033350A1 (en) * | 2007-08-09 | 2011-02-10 | Ecochem Tech, Ltd. | Process for recovering substances from high salinity liquids |
| CN102001763A (en) * | 2010-10-15 | 2011-04-06 | 天津欧纳海洋科技发展有限公司 | Production method for desalting seawater by de-hardening preprocessing |
| CN103408179A (en) * | 2013-08-22 | 2013-11-27 | 天津滨瀚环保科技发展有限公司 | Production method for desalting seawater by hot film coupling |
-
2016
- 2016-10-12 CN CN201610889334.8A patent/CN106467314A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4038365A (en) * | 1975-12-03 | 1977-07-26 | Basf Wyandotte Corporation | Removal of low level hardness impurities from brine feed to chlorine cells |
| CN85105048A (en) * | 1985-07-04 | 1986-12-31 | 金寿培 | Effluent brine reclaims and the recycle method |
| US20110033350A1 (en) * | 2007-08-09 | 2011-02-10 | Ecochem Tech, Ltd. | Process for recovering substances from high salinity liquids |
| CN102001763A (en) * | 2010-10-15 | 2011-04-06 | 天津欧纳海洋科技发展有限公司 | Production method for desalting seawater by de-hardening preprocessing |
| CN103408179A (en) * | 2013-08-22 | 2013-11-27 | 天津滨瀚环保科技发展有限公司 | Production method for desalting seawater by hot film coupling |
Non-Patent Citations (2)
| Title |
|---|
| 刘维锐: "高效结晶除硬技术处理高盐废水的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 顾翼东: "《化学词典》", 30 September 1989 * |
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Application publication date: 20170301 |