CN106673026A - Process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and by-product - Google Patents
Process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and by-product Download PDFInfo
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- CN106673026A CN106673026A CN201611058710.5A CN201611058710A CN106673026A CN 106673026 A CN106673026 A CN 106673026A CN 201611058710 A CN201611058710 A CN 201611058710A CN 106673026 A CN106673026 A CN 106673026A
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- Prior art keywords
- magnesium
- calcium carbonate
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- solution
- calcium
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Classifications
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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
-
- 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and a by-product. The process for producing magnesium hydrate from a byproduct magnesium chloride solution generated in the production of potassium nitrate is combined with the process for producing crystal whisker calcium carbonate from byproduct calcium chloride generated in the production of magnesium hydrate; a mother liquor containing calcium chloride and magnesium chloride, obtained in the production of magnesium hydrate, is used to prepare crystal whisker calcium carbonate; produced magnesium carbonate is taken as an intermediate; the calcium carbonate crystal whisker is then promoted to grow through the conversion reaction; the high-quality calcium carbonate crystal whisker product is obtained; and magnesium chloride is recycled in the system but is not consumed, the process is simple, and the production cost is low.
Description
Technical field
Present invention relates particularly to chemical products production technical field, and in particular to a kind of co-producing high-purity magnesium hydroxide and its pair
The technique that product prepares calcium carbonate whisker.
Background technology
In the existing side product chlorinated magnesium solution production magnesium hydroxide technique to produce potassium nitrate, the magnesium hydroxide of preparation
Often purity is not high, and the impurity such as ferrum, manganese and the heavy metal for wherein containing, and raw materials technology utilization rate is not high, gained hydroxide
Magnesium products purity is not high, and impurity is more, and granularity is uneven, and the side product chlorinated calcium that production is obtained can not be effectively utilized,
The significant wastage of resource is caused, therefore, now it is badly in need of a kind of and hydrogen-oxygen is produced with the side product chlorinated magnesium solution for producing potassium nitrate
Change the joint production process that magnesium technique matches, complement each other with production magnesium hydroxide technique, the utilization existing resource of maximal efficiency is obtained
To maximum yield, reduce the waste to raw material.
The content of the invention
In order to solve the deficiencies in the prior art, the present invention there is provided a kind of co-producing high-purity magnesium hydroxide and its by-product system
The technique of standby calcium carbonate whisker.
The present invention adopt technical solution be：A kind of co-producing high-purity magnesium hydroxide and its by-product prepare whisker carbonic acid
The technique of calcium, comprises the following steps：
（1）The magnesium chloride containing precipitate collected during the mother liquid disposal tank after production potassium nitrate is added in magnesium chloride solution and flocculation
Agent, reaction are filtered after a period of time, obtain purified magnesium chloride solution；
（2）Calx and water mixing are carried out into lime slaking, the lime cream for obtaining is then added in lime cream treatment tank, after process
To refined lime breast；
（3）Purified magnesium chloride solution is added in precipitation tank, while adding refined lime solution to be reacted, hydrogen is obtained
Magnesium oxide precipitation；
（4）Reaction solution containing magnesium hydrate precipitate is transferred in aging tank carries out ageing reaction, and reaction solution overflow is extremely
Mother liquid disposal tank, remaining precipitation are filtrated to get magnesium hydroxide crude product；
（5）In mother liquid disposal tank, the thick slag of Calx collected in lime cream treatment tank is added to carry out mother liquid disposal, solution overflow is extremely
In lime cream treatment tank, precipitate refined for magnesium chloride solution；
（6）The magnesium hydroxide crude product for obtaining is washed with water, is filtered, crushed after being dried obtains final product magnesium hydroxide products；
（7）By step（5）In the chloride containing calcium that obtains and magnesium chloride mother solution in add magnesium chloride, and control calcium ions and magnesium ions ratio
Example, adds soda, and reaction obtains magnesium carbonate and Calcium Carbonate mixed precipitation and sodium chloride solution；
（8）The mixed precipitation for obtaining is added in excessive calcium chloride solution carries out conversion reaction, is totally converted magnesium carbonate
For Calcium Carbonate, and increase calcium carbonate crystal whisker；
（9）Calcium carbonate crystal whisker crude product is filtrated to get, then by washing, being dried to obtain calcium carbonate crystal whisker product, it is mother liquid obtained for chlorine
Change the mixed solution of calcium and magnesium chloride, return precipitation tank circular batching.
Described step（8）Middle conversion reaction is carried out under the conditions of 60~90 DEG C.
Described step（7）The middle calcium ions and magnesium ions ratio for controlling is 1:0.5~2.
Described step（7）The sodium chloride solution for obtaining obtains Sodium Chloride product by evaporation and concentration, filtration, washing.
The invention has the beneficial effects as follows：The invention provides a kind of co-producing high-purity magnesium hydroxide and its by-product prepare whisker
The technique of Calcium Carbonate, by magnesium hydroxide technique will be produced with production hydroxide with the side product chlorinated magnesium solution for producing potassium nitrate
The side product chlorinated calcium of magnesium prepares the process integration production of calcium carbonate whisker, by the chloride containing calcium for obtaining production magnesium hydroxide
Production calcium carbonate whisker is prepared with the mother solution of magnesium chloride, is intermediate using the magnesium carbonate for generating, then is promoted by conversion reaction
Calcium carbonate crystal whisker increases, and obtains the calcium carbonate crystal whisker product of high-quality, and magnesium chloride is recycled in system and do not consumed, technique letter
It is single, low production cost.
Description of the drawings
Fig. 1 is present invention production high purity magnesium hydroxide process chart.
Fig. 2 is coproduction calcium carbonate whisker process chart of the present invention.
Specific embodiment
The present invention is further described in conjunction with Fig. 1, Fig. 2,
High purity magnesium hydroxide preparation technology
Comprise the following steps：
（1）The magnesium chloride containing precipitate collected during the mother liquid disposal tank after production potassium nitrate is added in magnesium chloride solution and flocculation
Agent, reaction are filtered after a period of time, obtain purified magnesium chloride solution；
（2）Calx and water mixing are carried out into lime slaking, the lime cream for obtaining is then added in lime cream treatment tank, after process
To refined lime breast；
（3）Purified magnesium chloride solution is added in precipitation tank, while adding refined lime solution to be reacted, hydrogen is obtained
Magnesium oxide precipitation；
（4）Reaction solution containing magnesium hydrate precipitate is transferred in aging tank carries out ageing reaction, and reaction solution overflow is extremely
Mother liquid disposal tank, remaining precipitation are filtrated to get magnesium hydroxide crude product；
（5）In mother liquid disposal tank, the thick slag of Calx collected in lime cream treatment tank is added to carry out mother liquid disposal, solution overflow is extremely
In lime cream treatment tank, precipitate refined for magnesium chloride solution；
（6）The magnesium hydroxide crude product for obtaining is washed with water, is filtered, crushed after being dried obtains final product magnesium hydroxide products；
The technique is added lime cream to be reacted, produces hydroxide to produce the side product chlorinated magnesium solution of potassium nitrate as raw material
Magnesium products.The characteristics of production technology is：It is easy to product filtration washing using ageing reaction controlling product granularity；It is female using reaction
Liquid water is diluted to lime cream and by settling the thick slag removed in lime cream, obtains the refined lime solution clarified, it is ensured that
In magnesium hydrate precipitate reaction, the abundant reaction of Calx, reduces the calcium impurities content in product；Thick slag in using lime cream
Refinement treatment is carried out to reaction mother liquor water and magnesium chloride solution, the impurity such as ferrum, manganese and heavy metal in reduction product, while improving
The utilization rate of Calx；The raw materials technology utilization rate is high, low production cost, and gained magnesium hydroxide products purity is high, and impurity is few, grain
Degree is uniform.
The technique for preparing calcium carbonate whisker
（7）Magnesium chloride is added during the mother solution of the chloride containing calcium and magnesium chloride obtained in high purity magnesium hydroxide technique will be prepared, and is controlled
Calcium ions and magnesium ions ratio processed is 1:0.5~2, soda is added, reaction obtains magnesium carbonate and Calcium Carbonate mixed precipitation and Sodium Chloride is molten
Liquid；
（8）The mixed precipitation for obtaining is added in excessive calcium chloride solution under the conditions of 60~90 DEG C carries out conversion reaction,
Make magnesium carbonate be completely converted into Calcium Carbonate, and increase calcium carbonate crystal whisker；
（9）Calcium carbonate crystal whisker crude product is filtrated to get, then by washing, being dried to obtain calcium carbonate crystal whisker product, it is mother liquid obtained for chlorine
Change the mixed solution of calcium and magnesium chloride, return precipitation tank circular batching.
Described step（7）The sodium chloride solution for obtaining obtains Sodium Chloride product by evaporation and concentration, filtration, washing.
The present invention is by will produce magnesium hydroxide technique with production hydrogen-oxygen with the side product chlorinated magnesium solution for producing potassium nitrate
Change process integration production prepared by the side product chlorinated calcium of magnesium, by chloride containing calcium and magnesium chloride that magnesium hydroxide is obtained will be produced
Mother solution prepare production calcium carbonate whisker, be intermediate using the magnesium carbonate for generating, then promote Calcium Carbonate brilliant by conversion reaction
Must increase, obtain the calcium carbonate crystal whisker product of high-quality, magnesium chloride is recycled in system and do not consumed, process is simple, production
Low cost.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned enforcement
Example, all technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art
Those of ordinary skill for, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (4)
1. the technique that a kind of co-producing high-purity magnesium hydroxide and its by-product prepare calcium carbonate whisker, it is characterised in that including following
Step：
（1）The magnesium chloride containing precipitate collected during the mother liquid disposal tank after production potassium nitrate is added in magnesium chloride solution and flocculation
Agent, filters after reaction, obtains purified magnesium chloride solution；
（2）Calx and water mixing are carried out into lime slaking, the lime cream for obtaining is then added in lime cream treatment tank, after process
To refined lime breast；
（3）Purified magnesium chloride solution is added in precipitation tank, while adding refined lime solution to be reacted, hydrogen is obtained
Magnesium oxide precipitation；
（4）Reaction solution containing magnesium hydrate precipitate is transferred in aging tank carries out ageing reaction, and reaction solution overflow is extremely
Mother liquid disposal tank, remaining precipitation are filtrated to get magnesium hydroxide crude product；
（5）In mother liquid disposal tank, the thick slag of Calx collected in lime cream treatment tank is added to carry out mother liquid disposal, solution overflow is extremely
In lime cream treatment tank, precipitate refined for magnesium chloride solution；
（6）The magnesium hydroxide crude product for obtaining is washed with water, is filtered, crushed after being dried obtains final product magnesium hydroxide products；
（7）By step（5）In the chloride containing calcium that obtains and magnesium chloride mother solution in add magnesium chloride, and control calcium ions and magnesium ions ratio
Example, adds soda, and reaction obtains magnesium carbonate and Calcium Carbonate mixed precipitation and sodium chloride solution；
（8）The mixed precipitation for obtaining is added in excessive calcium chloride solution carries out conversion reaction, is totally converted magnesium carbonate
For Calcium Carbonate, and increase calcium carbonate crystal whisker；
（9）Calcium carbonate crystal whisker crude product is filtrated to get, then by washing, being dried to obtain calcium carbonate crystal whisker product, it is mother liquid obtained for chlorine
Change the mixed solution of calcium and magnesium chloride, return precipitation tank circular batching.
2. a kind of co-producing high-purity magnesium hydroxide according to claim 1 and its by-product prepare the technique of calcium carbonate whisker,
Characterized in that, described step（8）Middle conversion reaction is carried out under the conditions of 60~90 DEG C.
3. a kind of co-producing high-purity magnesium hydroxide according to claim 1 and its by-product prepare the technique of calcium carbonate whisker,
Characterized in that, described step（7）The middle calcium ions and magnesium ions ratio for controlling is 1:0.5~2.
4. a kind of co-producing high-purity magnesium hydroxide according to claim 1 and its by-product prepare the technique of calcium carbonate whisker,
Characterized in that, described step（7）The sodium chloride solution for obtaining obtains Sodium Chloride product by evaporation and concentration, filtration, washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611058710.5A CN106673026A (en) | 2016-11-28 | 2016-11-28 | Process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and by-product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611058710.5A CN106673026A (en) | 2016-11-28 | 2016-11-28 | Process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and by-product |
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| Publication Number | Publication Date |
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| CN106673026A true CN106673026A (en) | 2017-05-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611058710.5A Pending CN106673026A (en) | 2016-11-28 | 2016-11-28 | Process for preparing crystal whisker calcium carbonate through combined production of high-purity magnesium hydrate and by-product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255596A (en) * | 2019-06-19 | 2019-09-20 | 常熟美特钙业有限公司 | A kind of continuous carbonation technique preparing calcium carbonate |
| CN112760483A (en) * | 2019-11-06 | 2021-05-07 | 有研稀土新材料股份有限公司 | Method for metal smelting separation and co-production of high-purity calcium product and high-purity calcium product prepared by method |
-
2016
- 2016-11-28 CN CN201611058710.5A patent/CN106673026A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 何欣: "氢氧化镁脱硫脱硝新工艺", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 赵丽娜等: "文石型碳酸钙晶须的制备及其力学性能研究", 《化学通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255596A (en) * | 2019-06-19 | 2019-09-20 | 常熟美特钙业有限公司 | A kind of continuous carbonation technique preparing calcium carbonate |
| CN112760483A (en) * | 2019-11-06 | 2021-05-07 | 有研稀土新材料股份有限公司 | Method for metal smelting separation and co-production of high-purity calcium product and high-purity calcium product prepared by method |
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