CN101235440A - Method of comprehensively utilizing serpentine - Google Patents
Method of comprehensively utilizing serpentine Download PDFInfo
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- CN101235440A CN101235440A CNA2008100846486A CN200810084648A CN101235440A CN 101235440 A CN101235440 A CN 101235440A CN A2008100846486 A CNA2008100846486 A CN A2008100846486A CN 200810084648 A CN200810084648 A CN 200810084648A CN 101235440 A CN101235440 A CN 101235440A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a method for comprehensively utilizing serendipities, which comprises: magnetically separating the serpentinites in a strong magnetic field, obtaining amorphous silica powder which contains silicon dioxide more than 90% through filtering acid dipping solution, dissolving the amorphous silica powder through using caustic soda under high temperature, which is used for manufacturing soluble glass with medium high modulus or taken as raw materials for producing white carbon black, then, mixing sulphuric acid and hydrochloric acid or nitric acid or mixing the sulphuric acid, the hydrochloric acid and nitric acid, adding acid dipping additive to carry out compound alternative and circulating acid dipping for ore powder which is magnetically separated and processed, fractionally depositing, filtering, and removing impurity for magnesium sulfate solution which is filtered through the acid dipping and contains the impurity, through adjusting the pH value, obtaining inorganic industrial dyes which mainly contain iron oxide yellow, ferric hydroxide and aluminum hydroxide, enriching the nickel, which is convenient for abstracting the nickel from the serpentinites, finally obtaining high purity magnesium oxide through refining refined magnesium sulfate solution whose impurity is removed after ammonium hydrogen carbonate and ammonial solution or sodium sulfide is used to deposit, and also obtaining ammonium sulfate or sodium sulfate which contains magnesium and calcium after liquid which is filtered is evaporated.
Description
Technical field
The invention belongs to the ore deposit rock and refine technical field of chemistry and chemical engineering, be specifically related to a kind of method that fully utilizes serpentine.
Background technology
Serpentine is the layer silicate mineral that is composited by the silica octahedron, and its chemical formula is: 3MgO2SiO
22H
2O.Serpentine is with MgO and SiO
2For mainly can utilizing composition, and contain the ferric oxide about 8%, about 3 ‰ nickel and a certain amount of crystal water (about 12%), also have elements such as a small amount of manganese, chromium, aluminium, calcium.
China's serpentine reserves are huge, but to the utilization of serpentine, only are limited in following aspect: make the raw material that the jade raw material is used for general building and ornament materials; As refractory materials and chemical fertilizer raw material; As the aspect such as raw material of pottery, flux for metallurgy or do and fill out road stone and use, its added value is all very low.A large amount of serpentine resources are in the situation of throwing something aside.Extraction for the magnesium oxide and the silicon of high level in the serpentine, though taked certain methods, as dry process technology with the calcination processing serpentine, see Chinese patent application 88109764.9 and 92101146.6 etc., handle the wet processes technology of serpentine with acidleach, a large amount of bibliographical informations is also arranged, as Chinese patent application 89106821.X and 01131802.3 etc.But, the domestic industry of serpentine comprehensively being refined processing that do not form.Its major cause is, although serpentine contains relatively large magnesium and silicon, these technology only are the individual event developments and utilizations at these materials, can not assurance obtain stable income.And, in the course of processing, there is careless omission just may bring serious three wastes problem slightly, destroy resource, contaminate environment greatly.So, to the exploitation of serpentine, must be not only to consider its elementary composition, and will consider the overall technology exploitation of its comprehensive utilization and improvement.
Summary of the invention
The object of the present invention is to provide a kind ofly to be processed as the basis novel method of the comprehensive treating process serpentine of attaching most importance to snake stone flour acid leaching process with the serpentine breeze.What this method had improved serpentine utilizes the degree and the added value of industry, has reduced the generation and the discharging of pollutent.
Technical scheme of the present invention is as follows: a kind of method that fully utilizes serpentine comprises the steps:
(1) serpentine ore is crushed to 80～200 orders;
(2) isolate magnetic thing in the breeze with the above high-intensity magnetic field of 4500 oersteds, obtain magnetic iron powder;
(3) be that 80～200 purpose snake stone flours join in the pickling liquor with the granularity behind iron removal by magnetic separation, the acidleach temperature is controlled in 80 ℃～115 ℃ scopes, normal pressure stirred 1～4 hour, filtered to isolate acid content magnesium salt solution seldom, with filter residue through washing after as first leaching slag;
(4) first leaching slag is joined in the pickling liquor again, temperature is controlled in 80 ℃～115 ℃ scopes carries out the acidleach second time, and normal pressure stirred 2～5 hours down;
(5) filter to isolate acidleach mother liquor that contains magnesium salts and the filter residue that contains silicon-dioxide;
(6) filter residue obtains silicon-dioxide through washing precipitation after the drying.
The method of aforesaid comprehensive utilization serpentine, wherein, described pickling liquor is that concentration is that the hydrochloric acid of 90%～98% sulfuric acid or 30%～37% joins in the water of 0.5～5 times of weight that contains 0.1%～20% acidleach auxiliary agent is formulated.
The method of aforesaid comprehensive utilization serpentine, wherein, in the step (6) silicon-dioxide of gained under 80 ℃～120 ℃ of normal pressure and temperature, the water glass of high-module in making; With sulfuric acid or hydrochloric acid,, make white carbon black again stirring under 60 ℃～90 ℃ conditions between adjustment pH value to 7～9.
The method of aforesaid comprehensive utilization serpentine wherein, is carried out recycle with the acidleach mother liquor of gained in the step (5), as the pickling liquor of next circulation time acidleach for the first time.
The method of aforesaid comprehensive utilization serpentine wherein, is finished liquid behind hydrogen peroxide oxidation with what acidleach filtered out, adds ammoniacal liquor, and when regulating pH value to 1.8, solution filters and obtains iron oxide yellow.
The method of aforesaid comprehensive utilization serpentine wherein, is finished liquid behind hydrogen peroxide oxidation with what acidleach filtered out, adds ammoniacal liquor, and when adjusting pH value was 3.7-6, solution filtered the inorganic industrial dye that obtains based on ironic hydroxide and aluminium hydroxide.
The method of aforesaid comprehensive utilization serpentine wherein, is finished liquid behind hydrogen peroxide oxidation with what acidleach filtered out, and adding ammoniacal liquor when the pH value is 6.8-10, gets up the nickel enrichment, so that further extract the nickel in the serpentine.
The method of aforesaid comprehensive utilization serpentine, wherein, if pickling liquor is to adopt the sulfuric acid preparation, with the pure magnesium sulfate solution behind the refining and edulcoration, press magnesian content in the solution, with 45-90g/mol bicarbonate of ammonia and 100-200g/mol ammoniacal liquor or use to stir down at 60 ℃～90 ℃ and generate magnesiumcarbonate, clean wherein sulfate ion through post precipitation with the yellow soda ash of sal epsom reaction respective amount and sodium hydroxide, dry more than 20 hours down at 100 ℃～160 ℃, obtain high-purity magnesium basic carbonate; Through 900 ℃～1000 ℃ high-temperature calcinations, obtain high-purity magnesium oxide again, after the reaction solution evaporation after it filters, obtain magniferous ammonium sulfate and high-purity sodium sulfate.
Method provided by the present invention is all fully utilized each effective ingredient in the serpentine fully, and solids is all taken in the course of processing; Washing lotion when liquid has only product to finish just can be discharged by simple processing; Obnoxious flavour is effectively controlled fully.1 ton of serpentine original ore powder can obtain the industrial dye raw material that contains the about 30kg of high-grad iron ore deposit slag, the high-purity magnesium oxide 330～400kg of chromium, nickel, the about 300kg of high-purity white carbon black, contains the about 1300kg of magnesium ammonium sulfate (or sodium sulfate 1300kg), the about 2kg of nickelous sulfide and about 40kg in such comprehensive utilization process.
Embodiment
The present invention is processed as the basis with the serpentine breeze, a kind of novel method of the comprehensive treating process serpentine of attaching most importance to snake stone flour acid leaching process.Breeze choose the high quality that has guaranteed acidleach, the high quality of acidleach has directly determined the comprehensive utilization situation and the generation of waste situation of each composition in the serpentine again.
At first, the processing treatment of serpentine breeze, be to be machined to the 80-325 order with carrying out grinding after the fragmentation of serpentine breeze, use the mode of magnetic separation again, magnetic substance in the serpentine breeze is separated, by reducing iron content and the impurity content in the breeze, alleviated the pressure of subsequent process removal of impurities, help the extraction of magnesium oxide and silicon., with sulfuric acid and hydrochloric acid, nitric acid or three acid mix, add the acidleach auxiliary agent the finished breeze of magnetic separation is carried out compound alternate cycles acidleach, promptly by repeatedly acidleach of leaching target classification thereafter.Such acidleach is not only separated magnesium in the breeze and silicon well, and has improved the ununiformity of breeze significantly, makes the acidleach process more stable.Acid recycles in system in addition, and process does not have acid solution and washing lotion discharging, the pollution of having stopped solid, liquid.Gaseous emission in the process all reclaims by closed system is actual, can not cause environmental problem.After the acidleach, obtain rich magnesium pickling liquor respectively and contain the acidleach filter residue of silicon-dioxide more than 90%, just immersion liquid and solids separately can be carried out purification processes by filtering.Pickling liquor is by filtering, and its insolubles-contain the amorphous silica powder of silicon-dioxide more than 90% directly can be made industrial filtering medium.Continue processing treatment, also can by with caustic soda at high temperature with its molten opening, the water glass of high-module in being used for making can be used as the raw material of system white carbon black, further improves its added value.
The leaching liquid that acidleach filters out-impure Adlerika then carries out fractionation precipitation filtering and impurity removing to pickling liquor by oxidation and adjust pH with hydrogen peroxide, ammoniacal liquor and sodium sulphite.This deimpurity process can be referred to as to make with extra care.When refining, adjust pH 1.3～2.1 o'clock, solution filters and obtains iron oxide yellow; Adjust pH is 3.7～6 o'clock, and solution filters the inorganic industrial dye that obtains based on ironic hydroxide and aluminium hydroxide; In the pH value is 6.8～10 o'clock, the nickel enrichment can be got up, with convenient extraction with nickel in the serpentine; By the POV magnesium liquid of refining and edulcoration, use bicarbonate of ammonia and ammoniacal liquor or yellow soda ash and sodium hydroxide post precipitation more at last,, obtain high-purity magnesium oxide (purity reaches 98%～99%) through 800 ℃～1300 ℃ high-temperature calcinations.Behind the liquid evaporation after its filter, also can obtain magniferous ammonium sulfate or sodium sulfate, these all are common used in industry raw material and product.
Example 1: the 80-200 order is pulverized and be milled to serpentine ore, and the high-intensity magnetic field magnetic above with 4500 oersteds goes out wherein magnetic thing, obtains magnetic iron powder, through simply processing, obtains meeting the powdered iron ore of industrial requirements.
From the breeze that magnetic is crossed, filter out the 400g breeze, join in the acidleach mother liquor (eo-acid is through once soaking the immersion liquid of breeze) of 1500g, do acidleach for the first time (when technology begins, adopt concentration be 17% sulphuric acid soln as pickling liquor, do acidleach for the first time).At this moment, acidleach is controlled in 80 ℃ of-115 ℃ of temperature ranges, and normal pressure stirred 2 hours, filtered to isolate acid content rich Adlerika seldom, was the liquid of finishing for acidleach.Its filter residue is cleaned magnesium salts through secondary becomes the first silica flour that soaks, and prepares as acidleach for the second time.With 450g, 98% sulfuric acid slowly joins in the clear water of the 675g that contains the acidleach auxiliary agent, is taking advantage of the first silica flour that soaks of reaction heat acidleach for the first time to join in the acidleach again, does acidleach for the second time in 80 ℃ of-115 ℃ of temperature ranges.Normal pressure stirred 2.5 hours down, filtered to isolate acidleach mother liquor that is rich in magnesium salts and the acidleach insolubles that contains silicon-dioxide.Through washing precipitation, filter residue drying, get the thick silicon dioxide powder (SiO of off-white color
2Content 90%, amorphous).The acidleach mother liquor is prepared as the pickling liquor first time of next batch.In this circulation, the magnesium oxide in the serpentine 99% is transferred in the acid dip solution.
The thick silicon dioxide powder that obtains through removal of impurities and high-temperature activation, directly can be done industrial absorbent and filtering medium.Further deep processing can be pressed 1mol～3mol: the amount of 80～250g, the water glass of high-module in the making under normal pressure and 80 ℃～120 ℃.With sulfuric acid or hydrochloric acid, under 60 ℃～90 ℃ conditions, stir and adjust pH value again, make white carbon black between the 7-9.
Acidleach filters out finishes liquid-Adlerika, with pressing magnesian content in the solution behind the hydrogen peroxide oxidation again, is 22% ammoniacal liquor with the concentration of 30ml/mol, and when transferring pH value 1.8, solution filters and obtains iron oxide yellow; When adjust pH was 3.7-6, solution filtered the inorganic industrial dye that obtains based on ironic hydroxide and aluminium hydroxide; When the pH value is 6.8-10, the nickel enrichment can be got up, with convenient extraction with nickel in the serpentine.
Pure magnesium sulfate solution behind the refining and edulcoration is pressed magnesian content in the solution, stirs down at 60 ℃～90 ℃ with 45-90g/mol bicarbonate of ammonia and 100-200g/mol ammoniacal liquor and generates magnesiumcarbonate.Through the clean sulfate ion wherein of post precipitation, dry more than 20 hours down at 100 ℃～160 ℃, obtain high-purity magnesium basic carbonate.Through 900 ℃～1000 ℃ high-temperature calcinations, obtain high-purity magnesium oxide (purity reaches 98.5%～99.6%) again.After the reaction solution evaporation after it filters, also can obtain containing the ammonium sulfate of magnesium and calcium.If pure magnesium sulfate solution is sunk magnesium with the yellow soda ash of 100-200g/mol and sodium hydroxide, under the similarity condition, can obtain high-purity magnesium oxide (95%-98.5%) and high-purity sodium sulfate.
Example 2: the 80-200 order is pulverized and be milled to serpentine ore, and the high-intensity magnetic field magnetic above with 4500 oersteds goes out wherein magnetic thing, obtains thick magnetic iron powder.Thick magnetic iron powder carries out the rewetting magnetic separation, obtains meeting the powdered iron ore of industrial requirements.
From the breeze that magnetic is crossed, filter out the 400g breeze, join in the acidleach mother liquor (eo-acid is through once soaking the immersion liquid of breeze) of 1500g, do acidleach for the first time.At this moment, acidleach is controlled in 80 ℃ of-135 ℃ of temperature ranges, and normal pressure stirred 2 hours, filtered to isolate acid content rich Adlerika seldom, was the liquid of finishing for acidleach.Its filter residue is cleaned magnesium salts through secondary becomes the first silica flour that soaks, and prepares as acidleach for the second time.98% the sulfuric acid of 450g is slowly joined in the clear water of the 675g that contains the acidleach auxiliary agent, taking advantage of the first silica flour that soaks of reaction heat acidleach for the first time to join in the acidleach again, in 80 ℃ of-115 ℃ of temperature ranges, do acidleach for the second time.Normal pressure stirred 2.5 hours down, filtered to isolate acidleach mother liquor that is rich in magnesium salts and the acidleach insolubles that contains silicon-dioxide.Through washing precipitation, filter residue drying, get the thick silicon dioxide powder (SiO of off-white color
2Content 90%, amorphous).The acidleach mother liquor is prepared as the pickling liquor first time of next batch.In this circulation, the magnesium oxide in the serpentine 99% is transferred in the acid dip solution.
The thick silicon dioxide powder that obtains through removal of impurities and high-temperature activation, directly can be done industrial absorbent and filtering medium.If further deep processing, can under normal pressure and 80 ℃-120 ℃, press 1mol-3mol: the amount of 80-250g, the water glass of high-module in the making.With sulfuric acid or hydrochloric acid, under 60 ℃ of-90 ℃ of conditions, stir and adjust pH value again, make white carbon black between the 7-9.
Acidleach filters out finishes liquid-Adlerika, press magnesian content in the solution again through behind the hydrogen peroxide oxidation, with the concentration of 30ml/mol is 22% ammoniacal liquor, and when adjust pH was 3.7-6, solution filtered the inorganic industrial dye that obtains based on ironic hydroxide and aluminium hydroxide; When the pH value is 6.8-10, the nickel enrichment can be got up, with convenient extraction with nickel in the serpentine.In the process of this refining and edulcoration, do not produce waste.
Pure magnesium sulfate solution behind the refining and edulcoration is pressed magnesian content in the solution, with 115g/mol yellow soda ash and 35g/mol sodium hydroxide, stirs generation magnesiumcarbonate down at 60 ℃-90 ℃.Filter through post precipitation, clean sulfate ion wherein again, dried 20 hours down, obtain high purity magnesium carbonate at 100 ℃-150 ℃.Through 900 ℃ of-1000 ℃ of high-temperature calcinations, obtain high-purity magnesium oxide (purity reaches 98%～99%) again.After the reaction solution evaporation after it filters, also can obtain high-purity sulphuric acid sodium.
Example 3: under all identical situation of other condition, do pickling liquor with 20% hydrochloric acid, the leaching rate of its magnesium can reach 95%-98%.The yield of silica flour can reach 98%.The intermediate product magnesium chloride, magnesian purity is still at 97%-98%.Except that the acidleach operating environment than sulfuric acid weaker, the efforts at environmental protection amount is big, other situation is basic identical, just not in this repetition.
Example 4: under all identical situation of other condition, do pickling liquor with 30%～40% nitric acid, the leaching rate of its magnesium can reach 96%-99%.The yield of silica flour can reach 98%.Magnesian purity is still at 97%-98%.The acidleach operational condition is worse than vitriol lixiviation, and other situation is identical, not in this repetition.
Example 5: under all identical situation of other condition, did pickling liquor in 2: 1: 1 in molar ratio with sulfuric acid, hydrochloric acid, nitric acid, the leaching rate of its magnesium can reach 97%-98%.The yield of silica flour can reach 99%.The intermediate product magnesium chloride, magnesian purity is still at 97%-99%.It operates more complicated, and also very high to the requirement of equipment, other situation is identical, or else repeats.
Claims (8)
1. a method that fully utilizes serpentine comprises the steps:
(1) serpentine ore is crushed to 80～200 orders;
(2) isolate magnetic thing in the breeze with the above high-intensity magnetic field of 4500 oersteds, obtain magnetic iron powder;
(3) be that 80～200 purpose snake stone flours join in the pickling liquor with the granularity behind iron removal by magnetic separation, the acidleach temperature is controlled in 80 ℃～115 ℃ scopes, normal pressure stirred 1～4 hour, filtered to isolate acid content magnesium salt solution seldom, with filter residue through washing after as first leaching slag;
(4) first leaching slag is joined in the pickling liquor again, temperature is controlled in 80 ℃～115 ℃ scopes carries out the acidleach second time, and normal pressure stirred 2～5 hours down;
(5) filter to isolate acidleach mother liquor that contains magnesium salts and the filter residue that contains silicon-dioxide;
(6) filter residue obtains silicon-dioxide through washing precipitation after the drying.
2. the method for comprehensive utilization serpentine as claimed in claim 1 is characterized in that: described pickling liquor is that concentration is that the hydrochloric acid of 90%～98% sulfuric acid or 30%～37% joins in the water of 0.5～5 times of weight that contains 0.1%～20% acidleach auxiliary agent is formulated.
3. the method for comprehensive utilization serpentine as claimed in claim 1 or 2 is characterized in that: in the step (6) silicon-dioxide of gained under 80 ℃～120 ℃ of normal pressure and temperature, the water glass of high-module in making; Adjust between pH value to 7～9 in stirring under 60 ℃～90 ℃ conditions with sulfuric acid or hydrochloric acid again, make white carbon black.
4. the method for comprehensive utilization serpentine as claimed in claim 1 or 2 is characterized in that: the acidleach mother liquor of gained in the step (5) is carried out recycle, as the pickling liquor of next circulation time acidleach for the first time.
5. the method for comprehensive utilization serpentine as claimed in claim 4 is characterized in that: finish liquid behind hydrogen peroxide oxidation with what acidleach filtered out, add ammoniacal liquor, when regulating pH value to 1.8, solution filters and obtains iron oxide yellow.
6. the method for comprehensive utilization serpentine as claimed in claim 4, it is characterized in that: finish liquid behind hydrogen peroxide oxidation what acidleach filtered out, add ammoniacal liquor, when adjusting pH value was 3.7-6, solution filtered the inorganic industrial dye that obtains based on ironic hydroxide and aluminium hydroxide.
7. the method for comprehensive utilization serpentine as claimed in claim 4, it is characterized in that: finish liquid behind hydrogen peroxide oxidation with what acidleach filtered out, add ammoniacal liquor, when adjusting pH value is 6.8-10, the nickel enrichment is got up, so that further extract nickel in the serpentine.
8. the method for comprehensive utilization serpentine as claimed in claim 4, it is characterized in that: if pickling liquor is to adopt the sulfuric acid preparation, with the pure magnesium sulfate solution behind the refining and edulcoration, press magnesian content in the solution, with 45-90g/mol bicarbonate of ammonia and 100-200g/mol ammoniacal liquor or use to stir down at 60 ℃～90 ℃ and generate magnesiumcarbonate with the yellow soda ash of sal epsom reaction respective amount and sodium hydroxide, through the clean sulfate ion wherein of post precipitation, dry more than 20 hours down at 100 ℃～160 ℃, obtain high-purity magnesium basic carbonate; Through 900 ℃～1000 ℃ high-temperature calcinations, obtain high-purity magnesium oxide again, after the reaction solution evaporation after it filters, obtain magniferous ammonium sulfate and high-purity sodium sulfate.
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| CN102167563A (en) * | 2011-01-05 | 2011-08-31 | 上海大学 | Method for producing ceramic chips by using calcium fluoride sludge and abandoned serpentine mine tailing |
| CN102190333A (en) * | 2011-04-12 | 2011-09-21 | 铜陵化学工业集团有限公司 | Method for processing serpentine with titanium white waste acid |
| CN101929121B (en) * | 2009-06-26 | 2012-05-30 | 中国矿业大学(北京) | Method for filling modified road asphalt comprehensively using serpentine acid leaching residue |
| CN102491345A (en) * | 2011-12-01 | 2012-06-13 | 安徽安纳达钛业股份有限公司 | Carbonization method for preparing precipitated white carbon black |
| CN102530947A (en) * | 2012-01-11 | 2012-07-04 | 新疆世全黄金矿业股份有限公司 | Application of serpentine to producing compounds |
| CN102583458A (en) * | 2011-01-18 | 2012-07-18 | 马猛 | Method for extracting basic magnesium carbonate, iron hydroxide and calcium sulfate from serpentine under normal temperature and pressure |
| CN102602938A (en) * | 2012-01-17 | 2012-07-25 | 合肥工业大学 | Method for preparing precipitate white carbon black by utilizing serpentine tailings |
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| CN103189529B (en) * | 2010-08-27 | 2016-01-20 | 生态工程有限公司 | For the method that magnesium is produced |
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