CN101723419B - Method for preparing high purity magnesium carbonate by one-step iron removal method - Google Patents
Method for preparing high purity magnesium carbonate by one-step iron removal method Download PDFInfo
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- CN101723419B CN101723419B CN2009102486827A CN200910248682A CN101723419B CN 101723419 B CN101723419 B CN 101723419B CN 2009102486827 A CN2009102486827 A CN 2009102486827A CN 200910248682 A CN200910248682 A CN 200910248682A CN 101723419 B CN101723419 B CN 101723419B
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- iron
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- heavy magnesium
- magnesium water
- magnesium carbonate
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Abstract
The invention relates to a method for preparing high purity magnesium carbonate by a one-step iron removal method, which relates to the field of the chemistry and the chemical industry of inorganic salts. The method comprises the following preparation steps of: according to the iron content in heavy magnesium water at the normal temperature, adding a reducing agent namely sodium hydrosulfite (Na2S2O4) which is 1.2 to 1.5 times that of the theoretical molar content of iron, and simultaneously stirring the mixture to perform reaction for 3 to 5 minutes so as to completely convert ferric irons in the heavy magnesium water into ferrous irons; taking the heavy magnesium water after complete reaction, adding sodium sulfide which is 1.2 to 1.5 times that of the theoretical molar content of the iron at the normal temperature into the heavy magnesium water, and stirring the mixture evenly to obtain black cloudy solution; and standing the black cloudy solution to ensure that ferrous sulfide is completely deposited so as to separate out clear solution of the heavy magnesium water, namely adding soft burning powder namely a product obtained by calcinating magnesite in the reaction or not, and performing vacuum filtration to obtain the clear solution of the heavy magnesium water. The method does not need to change the original production process, does not need to additionally establish treatment facilities, and has less investment and good iron removal effect, and the iron content of an obtained high purity magnesium carbonate product is about 0.004 percent and exceeds that of the national top grade product requirement with the iron content of 0.02 percent.
Description
Technical field
The present invention relates to the inorganic salt chemical field, particularly relate to a kind of new method for removing iron and prepare high purity magnesium carbonate.
Background technology
Magnesium basic carbonate is a kind of important inorganic salt product, has good filling property and dispersiveness, can improve the tensile strength and the wear resistance of rubber, plastics.It is good weighting agent of rubber, plastics and strengthening agent, also can be used as the weighting agent of industry such as paint and coating and toothpaste, makeup, medicine simultaneously.Along with rapid development of national economy, high-quality magnesiumcarbonate demand is risen year by year, because the existence of metallic impurity such as iron affects the quality of magnesiumcarbonate to a great extent, the content that how to reduce iron is an important step that improves the magnesiumcarbonate quality, the chemical removal of iron method all has bibliographical information at home and abroad, and the most frequently used method is to add oxygenant to make iron with Fe (OH) at present
3Sedimentary form is removed, but Fe (OH)
3Precipitate slowlyer and not easily separated, bring very big inconvenience to actual production, moreover be to add reductive agent earlier, ferric iron is reduced into ferrous iron, again with the complexing agent complexing to reach the purpose of deironing.But this method cost is higher and DeGrain is unfavorable for large-scale industrial production.
Summary of the invention
The object of the present invention is to provide a kind of method for removing iron for preparing in the high purity magnesium carbonate process.This method obtains the high purity magnesium carbonate product on the basis that does not change original production technique, iron-holder is 0.004% (national top grade product standard is 0.02%) in the high purity magnesium carbonate product that obtains.
The objective of the invention is to be achieved through the following technical solutions:
One method for preparing high purity magnesium carbonate by one-step iron removal method, its step is as follows:
(1) under the normal temperature, according to the iron-holder in the heavy magnesium water, the reductive agent V-Brite B (Na that the theoretical molar content of adding iron is 1.2～1.5 times
2S
2O
4), stirring reaction 3～5min is converted into ferrous iron fully with the ferric iron in the heavy magnesium water simultaneously;
(2) get the heavy magnesium water of above-mentioned complete reaction, normal temperature adds the sodium sulphite of 1.2～1.5 times of the theoretical molar content of iron down, stirs, and obtains the black turbid solution;
(3) the static Iron sulfuret that makes of black turbid solution is precipitated fully, isolate the heavy magnesium water clear liquid, in the reaction or to add light burnt powder be product after the magnesite calcining, vacuum filtration obtains the heavy magnesium water clear liquid.
A described method for preparing high purity magnesium carbonate by one-step iron removal method, it adds a kind of main reductive agent vat powder and time reductive agent sodium sulphite.
A described method for preparing high purity magnesium carbonate by one-step iron removal method, its used reduction reaction terminal point detects with potassium thiocyanate solution, ferric ion and potassium thiocyanate reaction, famous apparent colour-change, if there is blood red appearance then not react completely, should continue to add reductive agent, till can't check ferric iron with potassium thiocyanate.
Advantage of the present invention and effect are:
1. do not need to change original production technique, do not need to build in addition treatment facility, less investment, good iron removal effect, the iron-holder in the high purity magnesium carbonate product that obtains surpass national top grade product and require 0.02% about 0.004%.
2. in iron removal, Mn
2+Also obtain removing along with the Iron sulfuret coprecipitation on metal, reach the effect of achieving many things at one stroke with the form of sulfide.
3. speed of response is fast, and is simple to operate, convenient, good operation conditions, and cost is low, and calculating production magnesiumcarbonate product deironing cost per ton by the market value of present medicine is 50～60 yuans
Embodiment
Below the present invention is described in detail:
Under the normal temperature,, add the reductive agent V-Brite B (Na of the theoretical molar content 1.2～1.5 of iron according to the iron-holder in the heavy magnesium water
2S
2O
4), stirring reaction 3～5min is converted into ferrous iron fully with the ferric iron in the heavy magnesium water simultaneously.Reaction end detects with potassium thiocyanate solution, and concrete operations are: get reduction back solution 5～10ml, drip 2～3 potassium thiocyanate solution, if there is blood red appearance then not react completely, should continue to add reductive agent, till can't check ferric iron with potassium thiocyanate.Get the heavy magnesium water of above-mentioned complete reaction, normal temperature adds the sodium sulphite of the theoretical molar content 1.2～1.5 of iron down, stirs.Obtain the black turbid solution.The static Iron sulfuret that makes of black turbid solution is precipitated fully, isolate the heavy magnesium water clear liquid.(also can add a certain amount of light burnt powder (product after the magnesite calcining) in this step reaction, vacuum filtration obtains the heavy magnesium water clear liquid).By known method, heavy magnesium water filters by pyrolysis, and drying obtains the high purity magnesium carbonate product.
The present invention is directed to ferruginous heavy magnesium water (magnesium bicarbonate solution), add the reductive agent V-Brite B ferric iron is reduced to ferrous iron, add sodium sulphite again, generation Iron sulfuret precipitation, obtain the heavy magnesium water clear liquid after the natural subsidence, heavy magnesium water by pyrolysis, is filtered, and drying obtains the high purity magnesium carbonate product.This method obtains the high purity magnesium carbonate product on the basis that does not change original production technique, iron-holder is 0.004% (national top grade product standard is 0.02%) in the high purity magnesium carbonate product that obtains.And do not need to change original production technique, do not need to build in addition treatment facility, less investment, good iron removal effect, the iron-holder in the high purity magnesium carbonate product that obtains surpass national top grade product and require 0.02% about 0.004%.Speed of response is fast, and is simple to operate, convenient, good operation conditions, and cost is low, and calculating production magnesiumcarbonate product deironing cost per ton by the market value of present medicine is 50～60 yuans.In iron removal, Mn
2+Also obtain removing along with the Iron sulfuret coprecipitation on metal, reach the effect of achieving many things at one stroke with the form of sulfide.
Embodiment: getting iron-holder is the heavy magnesium water 100ml of 0.19g/L, adding 5ml 0.1mol/L V-Brite B stirred two minutes, the sodium sulphite that adds 5ml 0.1mol/L again stirs the turbid solution that obtains black, add 0.1 gram left and right sides light burnt powder vacuum filtration and obtain the heavy magnesium water clear liquid, filter 95 ℃ of pyrolysis, drying obtains the magnesiumcarbonate product, and detecting and obtaining iron-holder is 0.004%.
Claims (2)
1. a method for preparing high purity magnesium carbonate by one-step iron removal method is characterized in that the step of a method for preparing high purity magnesium carbonate by one-step iron removal method is as follows:
(1) under the normal temperature, according to the iron-holder in the heavy magnesium water, the reductive agent V-Brite B (Na that the theoretical molar content of adding iron is 1.2～1.5 times
2S
2O
4), stirring reaction 3～5min is converted into ferrous iron fully with the ferric iron in the heavy magnesium water simultaneously;
(2) get the heavy magnesium water of above-mentioned complete reaction, normal temperature adds the sodium sulphite of 1.2～1.5 times of the theoretical molar content of iron down, stirs, and obtains the black turbid solution;
(3) the static Iron sulfuret that makes of black turbid solution is precipitated fully, isolate the heavy magnesium water clear liquid, in the reaction or to add light burnt powder be product after the magnesite calcining, vacuum filtration obtains the heavy magnesium water clear liquid; By known method, heavy magnesium water filters by pyrolysis, and drying obtains the high purity magnesium carbonate product.
2. a method for preparing high purity magnesium carbonate by one-step iron removal method according to claim 1, it is characterized in that used reduction reaction terminal point detects with potassium thiocyanate solution, ferric ion and potassium thiocyanate reaction, there is obvious color to change, if there is blood red appearance then not react completely, should continue to add reductive agent, till can't check ferric iron with potassium thiocyanate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102486827A CN101723419B (en) | 2009-12-23 | 2009-12-23 | Method for preparing high purity magnesium carbonate by one-step iron removal method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009102486827A CN101723419B (en) | 2009-12-23 | 2009-12-23 | Method for preparing high purity magnesium carbonate by one-step iron removal method |
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| Publication Number | Publication Date |
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| CN101723419A CN101723419A (en) | 2010-06-09 |
| CN101723419B true CN101723419B (en) | 2011-11-16 |
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| CN2009102486827A Expired - Fee Related CN101723419B (en) | 2009-12-23 | 2009-12-23 | Method for preparing high purity magnesium carbonate by one-step iron removal method |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773169B (en) * | 2012-08-06 | 2014-01-29 | 辽宁科技大学 | Collecting agent capable of achieving iron removal during reverse flotation and desiliconization of magnesite ore and preparation method thereof |
| CN103626211A (en) * | 2013-12-04 | 2014-03-12 | 沈阳化工大学 | Method for preparing heavy magnesium carbonate through heavy magnesium water |
| CN109775735B (en) * | 2019-03-27 | 2022-06-17 | 河北镁神科技股份有限公司 | Preparation method of high-purity superfine magnesium carbonate for battery material |
| CN110203952A (en) * | 2019-05-25 | 2019-09-06 | 邢台镁熙环保材料有限公司 | A kind of production technology of low iron, low violent magnesium carbonate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410352A (en) * | 2001-10-08 | 2003-04-16 | 中国科学院过程工程研究所 | Comprehensive utilization method of converting chromium slag totally into light magnesium carbonate and fine iron breeze |
| CN1623926A (en) * | 2003-12-01 | 2005-06-08 | 北京化工大学 | Preparing composite iron powder by aluminium magnesium alloy for degrading organics contained halogen in water |
-
2009
- 2009-12-23 CN CN2009102486827A patent/CN101723419B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410352A (en) * | 2001-10-08 | 2003-04-16 | 中国科学院过程工程研究所 | Comprehensive utilization method of converting chromium slag totally into light magnesium carbonate and fine iron breeze |
| CN1623926A (en) * | 2003-12-01 | 2005-06-08 | 北京化工大学 | Preparing composite iron powder by aluminium magnesium alloy for degrading organics contained halogen in water |
Non-Patent Citations (4)
| Title |
|---|
| JP特开2004-82115A 2004.03.18 |
| 司卫华等.碳酸镁产品除铁工艺的研究.《当代化工》.2009,第38卷(第5期),448-449. * |
| 王全.中小型联碱生产母液除铁研究.《纯碱工业》.1991,(第4期),28-33. * |
| 袁延英.高岭土的几种除铁方法.《国外金属矿选矿》.2000,(第9期),19-23. * |
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| CN101723419A (en) | 2010-06-09 |
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Granted publication date: 20111116 Termination date: 20211223 |