CN101830475A - Method for preparing magnesium silicate and magnesium hydroxide from serpentine or tailings thereof - Google Patents
Method for preparing magnesium silicate and magnesium hydroxide from serpentine or tailings thereof Download PDFInfo
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- CN101830475A CN101830475A CN 201010125793 CN201010125793A CN101830475A CN 101830475 A CN101830475 A CN 101830475A CN 201010125793 CN201010125793 CN 201010125793 CN 201010125793 A CN201010125793 A CN 201010125793A CN 101830475 A CN101830475 A CN 101830475A
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Abstract
The invention discloses a method for preparing magnesium silicate and magnesium hydroxide from serpentine or tailings thereof, comprising the steps of acid leaching, purification, alkaline leaching, separation, synthetic reaction, washing and drying. The method is characterized in that serpentine mineral powder is used as a raw material. The invention has the advantages of low production cost, favorable economic benefit, fewer three wastes and low energy consumption.
Description
Technical field
The present invention relates to the technical field of serpentine and mine tailing deep processing comprehensive utilization thereof and inorganic salt preparation, more specifically saying so a kind of is the method that raw material is produced Magnesium Silicate q-agent and magnesium hydroxide with serpentine or its mine tailing.
Background technology
(general formula is Mg to serpentine
3Si
2O
5(OH)
4) be 1: 1 type layer silicate mineral by silicon-oxy tetrahedron and the octahedra be combined into of oxyhydrogen magnesium.China's serpentine mineral resource is very abundant, and serpentine mainly is used to make fused(calcium magnesium)phosphate at present, as metallurgical fusing assistant and finishing material.Because serpentine ore has foliated lamellar or phosphorus form of flake crystal, the differentiation layer is bigger, and China is strip mining transformation, produces a large amount of broken ores in recovery process, and granularity＜2cm is commonly referred to as serpentine fine ore or mine tailing, accounts for the 1/2-1/3 of produced quantity.The mine tailing of this granularity is unwell to the manufacturing fused(calcium magnesium)phosphate, makes metallurgical fusing assistant and finishing material usefulness, often is taken as waste material and abandons.So not only waste a large amount of Mineral resources, and stacking can cause environmental pollution.Test result shows that the chemical constitution of this mine tailing and serpentine raw ore are more or less the same, and all contain more rich magnesium oxide, silicon-dioxide etc.As the major ingredient of Wan Nan serpentine tailing for being MgO 37-39% by weight percentage; SiO
239-41%.If can effectively utilize its each useful component, then not only solve the useless fine ore of serpentine and stack the pollution of environment, effectively utilize serpentine mineral products resource, but also can obtain certain economic benefits.
Magnesium Silicate q-agent belongs to the britesorb of silicic acid and magnesium compound formation, belongs to the silicate series product.Different according to magnesium oxide in the Magnesium Silicate q-agent with silica molar ratios, be divided into Magnesium Trisilicate and hexa-magnesium silicate.Wherein, Magnesium Trisilicate (2MgO3SiO
25H
2O) pharmaceutically as acid inhibitor, in the energy and hydrochloric acid in gastric juice and protection ulcer surface, be mainly used in treatment gastric and duodenal ulcer disease and hyperchlorhydria, also can cook deodorizing composition and discoloring agent etc., also be used for pottery or rubber manufacturing.Hexa-magnesium silicate (2MgO6SiO
2XH
2O) be amorphous, cellular structure, have bigger specific surface area, in chemical industry, be widely used in the trace impurity of removing in the organic products, as be used for refining polyethers etc.; Can be used for aspects such as medical and health, foodstuff additive in addition.At present, the method for industrial production Magnesium Silicate q-agent mainly contains magnesia decomposition method and sal epsom-soluble glass method.Wherein, the magnesia decomposition method is to be raw material with magnesia, sulfuric acid, water glass, caustic soda etc., makes Magnesium Silicate q-agent through operations such as acidolysis, refining and edulcoration, replacement(metathesis)reaction, separation, drying, pulverizing; Sal epsom-soluble glass method is to be raw material with sal epsom, water glass, caustic soda etc., makes Magnesium Silicate q-agent through operations such as replacement(metathesis)reaction, separation, drying, pulverizing, all adopts industrial raw material in the above method, and production cost is higher, energy consumption is higher.
Magnesium hydroxide is mainly as free of contamination neutralizing agent in the environment-friendly engineering, the weighting agent in the paper industry, and the sweetening agent of gas sweetening, boiler smoke is used for also that magnesium salts manufacturing, granulated sugar are refining, pharmacy, lagging material etc.; Surface treated magnesium hydroxide is the good fire retardant and the weighting agent of plastics.At present, the method for industrial production magnesium hydroxide mainly contains the selection calcination method of synthesis method and rhombspar.Wherein, synthesis method is to be raw material and alkaline matter with the bittern that contains magnesium chloride, reacts in the aqueous solution as calcium hydroxide, ammoniacal liquor, sodium hydroxide etc., generates magnesium hydrate precipitate, after filtration, operation such as washing, drying and make product.The selection calcination method of rhombspar is different with the magnesiumcarbonate decomposition temperature according to lime carbonate, when dolomite calcination, temperature is controlled at below 750 ℃, obtain dolomite ash, through digestion, operations such as slagging-off and solid-liquid separation, drying make product, exist to adopt industrial raw material, the defective that production cost is higher, energy consumption is higher.
Up to now, be not the relevant report that raw material is produced Magnesium Trisilicate and hexa-magnesium silicate method still with serpentine or its mine tailing.
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, and what provide that a kind of production cost is low, good in economic efficiency, three waste discharge is few, energy consumption is low produces the method for Magnesium Silicate q-agent and magnesium hydroxide by serpentine or its mine tailing.
Technical solution problem of the present invention adopts following technical scheme:
The present invention prepares the method for Magnesium Silicate q-agent and magnesium hydroxide by serpentine or its mine tailing, comprises that acidleach, purification, alkali soak, separation, building-up reactions, washing and drying, and it is characterized in that: with the serpentine breeze is raw material,
Described acidleach is in the serpentine breeze of granularity less than 200 μ m, by serpentine breeze and acid solution weight ratio is that 1: 2.0～5.0 adding concentration are the acid solution of 15～50wt%, after reacting 2～4 hours under 90～100 ℃ of temperature, filter acidleach filter cake and acidleach filtrate, with described acidleach filter cake with clear water washing to neutral; Described acid solution is sulfuric acid or hydrochloric acid;
Described purification is after described acidleach filtrate is 6.8～8.5 with the lye pH adjustment value, adds hydrogen peroxide and reacts Fe to the solution
2+All be oxidized to Fe
3+After-filtration, gained filtrate are magnesium salt solution;
It is to be that 1: 2.5～5.0 to add concentration be the sodium hydroxide solution of 10～30wt% by acidleach filter cake and sodium hydroxide solution weight ratio in described acidleach filter cake that described alkali soaks, below boiling temperature, and the temperature condition that is not less than 85 ℃ reacts filtered while hot after 0.5～2 hour down, and gained filtrate is water glass;
Described building-up reactions is:
Described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 8～20wt%, SiO in molar ratio
2: MgO adds described water glass at 1.5～1.75: 1, separates, washs, is drying to obtain Magnesium Trisilicate after reacting 10～40 minutes under the temperature condition of room temperature～50 ℃;
Perhaps described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 4～20wt%, SiO in molar ratio
2: MgO adds described water glass at 3～3.75: 1, and adding the lye pH adjustment value again is 9～10, separates, washs, is drying to obtain hexa-magnesium silicate after reacting 0.5～2 hour under the temperature condition of temperature room temperature～75 ℃;
Perhaps described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 5～30wt%, Mg in molar ratio
2+: NH
4 +/ Na
+Be 1: 2～8 to add concentration 10～28wt% alkali lye, after reacting 15～60 minutes hours under the temperature condition of room temperature～90 ℃, separate, wash, be drying to obtain magnesium hydroxide.
Each step reaction equation of the inventive method is:
The acidleach of a, serpentine or its mine tailing (is example with sulfuric acid)
Mg
3Si
2O
5(OH)
4+H
2SO
4→MgSO
4+SiO
2·nH
2O
Fe
2O
3+3H
2SO
4→Fe
2(SO
4)
3+3H
2O
The purification of b, serpentine or its mine tailing acidleach filtrate and washing lotion (is example with ammoniacal liquor)
Fe
2(SO
4)
3+6NH
3·H
2O→2Fe(OH)
3↓+3(NH
4)
2SO
4
The alkali of c, serpentine or its mine tailing acidleach filter cake soaks
SiO
2·nH
2O+2NaOH→Na
2O·nSiO
2+(n+1)H
2O
The preparation of Magnesium Trisilicate
MgSO
4+Na
2O·nSiO
2+H
2O→2MgO·3SiO
2·xH
2O↓+Na
2SO
4
The hexa-magnesium silicate preparation
MgSO
4+Na
2O·nSiO
2+H
2O→2MgO·6SiO
2·yH
2O↓+Na
2SO
4
Magnesium hydroxide preparation (is example with sodium hydroxide)
MgSO
4+2NaOH→Mg(OH)
2↓+Na
2SO
4
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the inventive method is produced Magnesium Silicate q-agent and magnesium hydroxide, has made full use of useful components such as the magnesium oxide in the serpentine, silicon-dioxide and ferric oxide, production closed cycle, basic three-waste free discharge.
2, required magnesium oxide, the silicon-dioxide of the inventive method production Magnesium Silicate q-agent all comes from serpentine ore, need not to adopt industrial raw material, and its production cost is effectively reduced.
3, the energy consumption that the inventive method produces that the energy consumption of water glass extensively adopts in present industrial production when being raw material production by quartz sand can be significantly reduced.
Embodiment
Present embodiment prepares according to the following procedure
Step 1: the acidleach of serpentine or its mine tailing
In the serpentine fine ore of granularity less than 200 μ m, by serpentine breeze and acid solution weight ratio is 1: it is sulfuric acid or the hydrochloric acid soln of 15-50% that 2.0-5.0 adds weight percent concentration, heating makes it after stirring reaction 2-4 under 90-100 ℃ the temperature hour, filter filter cake and acidleach filtrate, the acidleach filter cake is neutral with the clear water washing, collects acidleach filter cake, acidleach filtrate and washing lotion respectively;
Step 2: the purification of serpentine or its mine tailing acidleach filtrate and washing lotion
After step 1 gained acidleach filtrate and washing lotion mixing, adding weight percent concentration is ammoniacal liquor or the sodium hydroxide solution of 10%-28%, makes the pH value of solution be 6.8-8.5; Adding weight percent concentration again in solution is the hydrogen peroxide of 10%-30%, under the room temperature stirring reaction 2-3 hour, makes the Fe in the solution
2+All be oxidized to Fe
3+, under 40 ℃-80 ℃, leave standstill 1-3 hour after-filtration again, filter cake is washed to sulfate radical-free ion or chlorion with clear water; Filtrate and washing lotion are merged into and are promptly got sal epsom or magnesium chloride solution; Mainly contain ironic hydroxide in the filter cake, can recycle.
Step 3: the alkali of serpentine or its mine tailing acidleach filter cake soaks
In step 1 gained acidleach filter cake, by acidleach filter cake and sodium hydroxide weight ratio is that 1: 2.5～5.0 adding weight percent concentration are 10%～30% sodium hydroxide solution, below the boiling temperature and be not less than under 85 ℃ the temperature condition heated and stirred reaction 0.5～2 hour, filtered while hot again, gained filtrate is standby water glass; The gained filter cake mainly contains unreacted serpentine, can be back in the acid-leaching reaction after cleaning.
Step 4: building-up reactions
Magnesium Trisilicate preparation: it is 8%～20% solution that step 2 gained sal epsom or magnesium chloride solution are mixed with weight percent concentration, again SiO in molar ratio
2: MgO adds step 3 gained water glass at 1.5～1.75: 1, and stirring reaction is 10～40 minutes under the temperature condition of room temperature～50 ℃, still aging again 1～2 hour, filters then; With filter cake washing to there not being SO
4 2-Ion (or chlorion), and under 100 ℃-110 ℃, be dried to water ratio and be not more than 15%, the Magnesium Trisilicate product.
Hexa-magnesium silicate preparation: it is 4%～20% solution that step 2 gained sal epsom or magnesium chloride solution are mixed with weight percent concentration, again SiO in molar ratio
2: MgO is 3～3.75: 1 adding step 3 gained water glass, add weight percent concentration after stirring again and be 4%～20% sodium hydroxide solution its pH value is transferred to 9～10, stirring reaction is 0.5～2 hour under the temperature condition of room temperature～75 ℃, through 1～3 hour still aging after-filtration, with filter cake washing to there not being SO
4 2-Ion, and under 100 ℃-110 ℃ temperature, be dried to water ratio and be not more than 10%, the hexa-magnesium silicate product.
The preparation of magnesium hydroxide: being mixed with weight percent concentration at step 2 gained sal epsom or magnesium chloride solution is 5%～30% solution, again Mg in molar ratio
2+: NH
4 +(or Na
+) be that 1: 2～8 to add weight percent concentration be 10%～28% ammoniacal liquor or sodium hydroxide solution, stirring reaction is 15～60 minutes under the temperature condition of room temperature～90 ℃, the still aging after-filtration through 0.5～2 hour, with filter cake washing to there not being SO
4 2-Ion (or chlorion), and under 100 ℃-110 ℃, be dried to water ratio and be not more than 2.5%, magnesium hydroxide products.
Embodiment 1: present embodiment carries out as follows:
1, be in the serpentine fine ore of 75 μ m in granularity, be that to add weight percent concentration at 1: 3.0 be 40% sulphuric acid soln by weight, heated and stirred is 3 hours under 95 ℃ temperature condition, filtered while hot, and filter cake washing is extremely neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively with standby.
2, the acidleach filtrate in the step 1 and washing lotion being mixed the back, to add weight percent concentration be 15% ammoniacal liquor, and the pH value that makes solution is 7.2, adds the hydrogen peroxide that concentration is 30wt% again, the stirring reaction 3 hours Fe to the solution under room temperature
2+All be oxidized to Fe
3+, under 70 ℃, left standstill 2 hours again, filter, and with filter cake washing to the sulfate radical-free ion.Filtrate and washing lotion are merged into standby Adlerika.
3, in step 1 gained acidleach filter cake, be that to add weight percent concentration at 1: 3.0 be 20% sodium hydroxide solution by weight, in 85 ℃ of following heated and stirred 1.5 hours, filtered while hot, filtrate is water glass.
4, Magnesium Trisilicate preparation
It is the solution of 12wt%, SiO in molar ratio that step 2 gained Adlerika thin up is become concentration
2: MgO adds step 3 gained water glass at 3: 1.8,40 ℃ of following stirring reactions 20 minutes, filter, with filter cake washing to there not being SO
4 2-Ion, and under 100 ℃～110 ℃, be dried to water ratio smaller or equal to 15%, get the Magnesium Trisilicate product.Content of magnesia is 24.7% in surveying the Magnesium Trisilicate product, dioxide-containing silica is 53.2%, calcination loss is 21.1%, has reached the requirement in the pharmacopeia (version was two ones in 2005).
Embodiment 2: present embodiment carries out as follows:
1, be in the serpentine fine ore of 96 μ m in granularity, be that 1: 4.0 adding concentration is the hydrochloric acid soln of 25wt% by weight, heated and stirred is 3.5 hours under 95 ℃ temperature condition, filtered while hot, and filter cake washing is extremely near neutral, collect acidleach filter cake, acidleach filtrate and washing lotion respectively with standby.
2, step 1 gained acidleach filtrate and washing lotion being mixed the back, to add weight percent concentration be that the pH value of 20% sodium hydroxide solution regulator solution is 7.8, adding concentration again in solution is the hydrogen peroxide of 30wt%, stirring reaction is 2.5 hours under room temperature, the Fe to the solution
2+All be oxidized to Fe
3+, under 60 ℃, left standstill 2.5 hours again, filter then, with filter cake washing to there not being chlorion.Filtrate and washing lotion are merged into standby magnesium chloride solution.Filter cake mainly contains ironic hydroxide, recyclable utilization.
3, in step 1 gained acidleach filter cake, be that to add concentration at 1: 2.5 be the sodium hydroxide solution of 25wt% by weight, in 95 ℃ of following heated and stirred 1 hour, filtered while hot, filtrate is standby water glass.
4, step 2 gained magnesium chloride solution thin up being become concentration is the solution of 8wt%, SiO in molar ratio
2: MgO is 3: 0.8 adding step 3 gained water glass, the sodium hydroxide solution that with concentration is 10wt% transfers to 9～10 with its pH value, stirring reaction is 1 hour under 65 ℃ of temperature, still aging again 2 hours, filter, filter cake washing to there not being chlorion, and is dried to water ratio smaller or equal to 10% under 100 ℃-110 ℃, the hexa-magnesium silicate product.Content of magnesia is 13.8% in surveying the hexa-magnesium silicate product, dioxide-containing silica is 61.5%, has reached the requirement of quality standard.
Embodiment 3: present embodiment carries out as follows:
1, be in the serpentine fine ore of 120 μ m in granularity, be that 1: 4.0 adding concentration is the sulphuric acid soln of 25wt% by weight, heated and stirred is 4 hours under 95 ℃ temperature condition, filtered while hot, and with filter cake washing to neutral, it is standby to collect acidleach filter cake, acidleach filtrate and washing lotion respectively.
2, step 1 gained acidleach filtrate and washing lotion being mixed the back, to add concentration be that the ammoniacal liquor adjust pH of 25wt% is 8.2, and adding concentration again in solution is the hydrogen peroxide of 30wt%, and stirring reaction is 3 hours under room temperature, the Fe to the solution
2+All be oxidized to Fe
3+, under 50 ℃, left standstill 2 hours again, filter then, to the sulfate radical-free ion, filtrate and washing lotion are merged into standby Adlerika with filter cake washing; Filter cake mainly contains ironic hydroxide, recyclable utilization.
3, step 2 gained Adlerika thin up being become concentration is the solution of 12wt%, presses ammonium magnesium mol ratio 6: 1 and adds 25wt% ammoniacal liquor, and 50 ℃ of following stirring reactions 30 minutes, still aging through 1 hour filtered then again, with filter cake washing to there not being SO
4 2-Ion, and under 100 ℃～110 ℃, be dried to water ratio smaller or equal to 2.5%, get magnesium hydroxide products.Content of magnesia is 66.83% in surveying magnesium hydroxide products, calcium oxide content is 0.064%, has reached the requirement of I type among the HG/T 3067-2000 (mainly as fire retardant material).
Claims (1)
1. one kind prepares the method for Magnesium Silicate q-agent and magnesium hydroxide by serpentine or its mine tailing, comprises that acidleach, purification, alkali soak, separation, building-up reactions, washing and drying, and it is characterized in that: with the serpentine breeze is raw material;
Described acidleach is in the serpentine breeze of granularity less than 200 μ m, by serpentine breeze and acid solution weight ratio is that 1: 2.0～5.0 adding concentration are the acid solution of 15～50wt%, after reacting 2～4 hours under 90～100 ℃ of temperature, filter acidleach filter cake and acidleach filtrate, with described acidleach filter cake with clear water washing to neutral; Described acid solution is sulfuric acid or hydrochloric acid;
Described purification is after described acidleach filtrate is 6.8～8.5 with the lye pH adjustment value, adds hydrogen peroxide and reacts Fe to the solution
2+All be oxidized to Fe
3+After-filtration, gained filtrate are magnesium salt solution;
It is to be that 1: 2.5～5.0 to add concentration be the sodium hydroxide solution of 10～30wt% by acidleach filter cake and sodium hydroxide solution weight ratio in described acidleach filter cake that described alkali soaks, below boiling temperature, and the temperature condition that is not less than 85 ℃ reacts filtered while hot after 0.5～2 hour down, and gained filtrate is water glass;
Described building-up reactions is:
Described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 8～20wt%, SiO in molar ratio
2: MgO adds described water glass at 1.5～1.75: 1, separates, washs, is drying to obtain Magnesium Trisilicate after reacting 10～40 minutes under the temperature condition of room temperature～50 ℃;
Perhaps described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 4～20wt%, SiO in molar ratio
2: MgO adds described water glass at 3～3.75: 1, and adding the lye pH adjustment value again is 9～10, separates, washs, is drying to obtain hexa-magnesium silicate after reacting 0.5～2 hour under the temperature condition of room temperature～75 ℃;
Perhaps described magnesium salt solution is mixed with the solution that magnesium salt concentrations is 5～30wt%, Mg in molar ratio
2+: NH
4 +/ Na
+Be 1: 2～8 to add concentration 10～28wt% alkali lye, after reacting 15～60 minutes under the temperature condition of room temperature～90 ℃, separate, wash, be drying to obtain magnesium hydroxide.
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| CN102855985A (en) * | 2012-09-12 | 2013-01-02 | 上海安捷防火电缆有限公司 | High-flame-retardance fireproof cable made of inorganic materials |
| CN104292042A (en) * | 2014-09-15 | 2015-01-21 | 江苏湛蓝科技开发有限公司 | Silicon-magnesium compound fertilizer and preparation method thereof |
| CN105948084A (en) * | 2016-05-17 | 2016-09-21 | 山东理工大学 | Method for producing magnesium sulfate monohydrate with copper tailings taken as raw material |
| CN106573197A (en) * | 2014-04-10 | 2017-04-19 | 剑桥碳捕集有限公司 | Method and system of activation of mineral silicate minerals |
| CN108670976A (en) * | 2018-04-13 | 2018-10-19 | 安徽宇宁果胶股份有限公司 | A kind of production method of the special pectin of tartro-bismuthate |
| CN110330023A (en) * | 2019-07-17 | 2019-10-15 | 刘显海 | A kind of preparation of magnesium trisilicate and drying means |
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| CN102855985A (en) * | 2012-09-12 | 2013-01-02 | 上海安捷防火电缆有限公司 | High-flame-retardance fireproof cable made of inorganic materials |
| CN102855985B (en) * | 2012-09-12 | 2015-01-07 | 上海安捷防火电缆有限公司 | High-flame-retardance fireproof cable made of inorganic materials |
| CN106573197A (en) * | 2014-04-10 | 2017-04-19 | 剑桥碳捕集有限公司 | Method and system of activation of mineral silicate minerals |
| CN106573197B (en) * | 2014-04-10 | 2019-08-23 | 剑桥碳捕集有限公司 | The method and system of activated silicates minerals |
| CN104292042A (en) * | 2014-09-15 | 2015-01-21 | 江苏湛蓝科技开发有限公司 | Silicon-magnesium compound fertilizer and preparation method thereof |
| CN105948084A (en) * | 2016-05-17 | 2016-09-21 | 山东理工大学 | Method for producing magnesium sulfate monohydrate with copper tailings taken as raw material |
| CN108670976A (en) * | 2018-04-13 | 2018-10-19 | 安徽宇宁果胶股份有限公司 | A kind of production method of the special pectin of tartro-bismuthate |
| CN108670976B (en) * | 2018-04-13 | 2019-12-17 | 安徽宇宁果胶股份有限公司 | production method of special pectin for bismuth tartrate |
| CN110330023A (en) * | 2019-07-17 | 2019-10-15 | 刘显海 | A kind of preparation of magnesium trisilicate and drying means |
| CN113955775A (en) * | 2021-10-28 | 2022-01-21 | 北京润捷浩达科技有限公司 | Method for extracting lithium carbonate from lithium-rich clay by acid-base combination method |
| CN113955775B (en) * | 2021-10-28 | 2022-06-14 | 潘爱芳 | Method for extracting lithium carbonate from lithium-rich clay by acid-base combined method |
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Application publication date: 20100915 |