CN105621418B - A kind of method for preparing Ludox - Google Patents
A kind of method for preparing Ludox Download PDFInfo
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- CN105621418B CN105621418B CN201511015065.4A CN201511015065A CN105621418B CN 105621418 B CN105621418 B CN 105621418B CN 201511015065 A CN201511015065 A CN 201511015065A CN 105621418 B CN105621418 B CN 105621418B
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- acid
- ludox
- mine tailing
- roasted ore
- ore
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Environmental & Geological Engineering (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of method for preparing Ludox, it is characterized in that：Comprise the following steps：（1）With Bayan Obo mine tailing as the inorganic Ore Leaching of raw material, pickle liquor and acid leaching residue are obtained after filtering；（2）Acid leaching residue is calcined 2 ~ 6h under the conditions of 500~900 DEG C and obtains roasted ore；（3）Under the regulation of conditioning agent, roasted ore is slowly added into the sodium hydroxide solution that mass concentration is 5% ~ 15%, the mass ratio of roasted ore and sodium hydroxide solution is 1:0.3~1:1,60 ~ 100 DEG C of reaction temperature, the 8h of reaction time 2, stir speed (S.S.) is 200r/min, and its advantage of obtained Ludox is：Raw material is obtained acid leaching residue after Bayan Obo mine tailing acidleach, and silicone content is high, and impurity is few, and the purity of prepared Ludox is high；This craft science is simple, and cost is low, and the rate of recovery of silicon reaches more than 95%, and production process is generated without " three wastes ", while the rare earth in recyclable mine tailing；The present invention is applicable not only to Bayan Obo mine tailing, is also applied for the high mineral deposit of other silicone contents.
Description
Technical field
The present invention relates to a kind of method for preparing Ludox, belong to chemical field.
Background technology
Ludox as a kind of fine chemical product, be widely used in chemical industry, hot investment casting, papermaking, coating, weaving,
The fields such as food, electronics.Ludox is the optimum feed stock for preparing catalyst, using carrier of the Ludox as catalyst, can be carried
The selectivity of high catalyst and the yield of product.Waterglass is substituted as the bonding of accurate device casting process using Ludox
Agent, can change the coarse present situation of casting dimension poor accuracy, surface quality.Ludox is added in paper-making process, paper can be made
Smoothly, video is distinct, increases its exposure scope.Ludox is added in coating, anti-pollution and the strong epithelium of dust tightness can be formed,
The water resistance of coating, endurance enhancing.Ludox also widely applies the fields such as weaving, food, electronics, and different degrees of improves
The performance of these field products.
Baiyuneboite is polymetallic mixed rawore, and with a large amount of exploitations of iron and rare earth resources, the mine tailing of generation is dumped
Tailing dam is placed on, so far still without being effectively utilized.But also containing substantial amounts of niobium, rare earth, iron and silicon etc. in mine tailing
The content of silicon may be up to 40% or so in precious resources, wherein mine tailing, but not have not only during conventional comprehensive utilization of resources
Have and proposed silicon as product, but also as the obstruction during the resource concentration such as niobium, rare earth, iron, can be with mainly due to silicon
Acid, alkali generate the larger silicic acid and sodium metasilicate of two kinds of viscosity, so as to hinder the leaching of other elements.Therefore, want to realize in vain
The comprehensive utilization of cloud pile of stones, earth or grass resource, first effective extraction to silicon resource and utilization just turn into key.Application No.
CN103395792A patent research Bayan Obo mine tailing prepares the method for white carbon, but be due to the technique process length, it is useless
Water is big and the shortcomings of high energy consumption, actual production is still not used for so far.So, to realize the industrial metaplasia of Bayan Obo silicon resource
Production and accelerate the paces that utilize of resource comprehensive utilization, develop a kind of method of recovery silicon efficiently, economical and environmentally friendly have it is important
Realistic meaning.
The content of the invention
The invention aims to the technological deficiency for overcoming the above, there is provided the silicon resource that a kind of utilization Bayan Obo enriches
The method for preparing Ludox, this method SiO2Leaching rate reach more than 95%, and can other productions such as Extraction of rare earth from technique
Product, are a kind of methods of recovery silicon resource efficiently, economical and environmentally friendly.
The technical solution of the present invention is as follows：
The present invention comprises the following steps：（1）With Bayan Obo mine tailing as the inorganic Ore Leaching of raw material, acid is obtained after filtering
Immersion liquid and acid leaching residue（The purpose of acidleach is to remove the impurity such as iron, aluminium, rare earth in mine tailing）, the concentration of inorganic acid is：1~
6mol/L；Raw material is 1 with inorganic acid mass volume ratio:3~1:9；（2）Acid leaching residue is calcined 2 ~ 6h under the conditions of 500~900 DEG C
Obtain roasted ore；（3）In conditioning agent（Effect is the reaction rate for adjusting roasted ore and alkali）Regulation under, roasted ore is slowly added
Enter to mass concentration in 5% ~ 15% sodium hydroxide solution, the mass ratio of roasted ore and sodium hydroxide is 1:0.3~1:1, instead
60 ~ 100 DEG C of temperature is answered, reaction time 2-8h, stir speed (S.S.) is 200r/min, Ludox is made.
Step（1）Described inorganic acid is the one or more in hydrochloric acid, sulfuric acid, nitric acid.
Step（3）Described conditioning agent is：One kind or several in ethyl acetate, citric acid, malic acid, sulfuric acid, ammonium chloride
Kind.
Step（3）The consumption of middle conditioning agent is according to SiO in roasted ore2Content determine, SiO in conditioning agent and roasted ore2
Mol ratio be：0.3:1~1.2.
The beneficial effects of the invention are as follows：1. raw material of the present invention is obtained acidleach after Bayan Obo mine tailing acidleach
Slag, silicone content is high, and impurity is few, and the purity of prepared Ludox is high.2. a craft science is simple, cost is low, the rate of recovery of silicon
More than 95% is reached, production process is generated without " three wastes ", while the rare earth in recyclable mine tailing.3. promotional value of the present invention is high, no
The recovery of silicon in Bayan Obo mine tailing is only applicable to, the high mineral deposit of other silicone contents is also applied for.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
Embodiment 1：
Take 50g baiyuneboite mine tailings, 3h leached at a temperature of 80 DEG C with 360ml, 2N hydrochloric acid, obtain pickle liquor with
Acid leaching residue, then in Muffle furnace 800 DEG C roasting 5h, cooling take out, obtain roasted ore, by roasted ore ethyl acetate regulation
Under, it is slowly added into 300ml, 5at% sodium hydroxide solution, 60 DEG C of reaction 5h obtain Ludox, the rate of recovery of silicon is
90%, SiO2Content be 30 at %.
Embodiment 2：
50g Bayan Obo mine tailings are taken, 3h is leached at a temperature of 80 DEG C with 360ml, 2N hydrochloric acid, obtains acid leaching residue, so
Afterwards in Muffle furnace 600 DEG C roasting 5h, cooling take out, obtain roasted ore, by roasted ore by roasted ore ethyl acetate tune
Under section, it is slowly added into 150ml, 10 at % sodium hydroxide solution, 70 DEG C of reaction 5h obtain Ludox, the rate of recovery of silicon
For 92%, SiO2Content be 25 at %.
Embodiment 3：
50g Bayan Obo mine tailings are taken, 3h is leached at a temperature of 80 DEG C with 500ml, 2N hydrochloric acid, obtains acid leaching residue, so
800 DEG C of roasting 5h in Muffle furnace, cooling taking-up, obtain roasted ore, under the regulation of sulfuric acid, are slowly added into 100ml, 15 afterwards
In at % sodium hydroxide solution, 90 DEG C of reaction 3h obtain Ludox, the rate of recovery of silicon is 97%, SiO2Content be 24 at
%。
Embodiment 4：
100g Bayan Obo mine tailings are taken, 3h is leached at a temperature of 80 DEG C with 500ml, 2N hydrochloric acid, obtains acid leaching residue, so
700 DEG C of roasting 5h in Muffle furnace, cooling taking-up, obtain roasted ore, under the regulation of malic acid and citric acid, are slowly added to afterwards
Into 300ml, 5 at % sodium hydroxide solution, 70 DEG C of reaction 8h obtain Ludox, the rate of recovery of silicon is 96%, SiO2Contain
Measure as 23 at %.
Embodiment 5：
100g Bayan Obo mine tailings are taken, 3h is leached at a temperature of 100 DEG C with 200ml, 2N hydrochloric acid, obtains acid leaching residue,
Then 900 DEG C of roasting 3h in Muffle furnace, cooling taking-up, obtain roasted ore, under the regulation of ammonium chloride, are slowly added into
In 600ml, 5 at % sodium hydroxide solution, 80 DEG C of reaction 6h obtain Ludox, the rate of recovery of silicon is 75%, SiO2Content
For 18 at %.
Claims (2)
1. a kind of method for preparing Ludox, it is characterized in that：Comprise the following steps：（1）Used with Bayan Obo mine tailing as raw material
Pickle liquor and acid leaching residue are obtained after inorganic Ore Leaching, filtering, the concentration of inorganic acid is：1~6mol/L, raw material and inorganic acid quality
Volume ratio is 1:3~1:9；（2）Acid leaching residue is calcined 2 ~ 6h under the conditions of 500~900 DEG C and obtains roasted ore；（3）In conditioning agent
Regulation under, by roasted ore be slowly added into mass concentration be 5% ~ 15% sodium hydroxide solution in, roasted ore and hydroxide
The mass ratio of sodium is 1:0.3~1:1,60 ~ 100 DEG C of reaction temperature, reaction time 2-8h, stir speed (S.S.) is 200r/min, and silicon is made
Colloidal sol, wherein conditioning agent are the one or more in ethyl acetate, citric acid, malic acid, sulfuric acid, ammonium chloride.
2. the method according to claim 1 for preparing Ludox, it is characterized in that：Step（1）Described inorganic acid be hydrochloric acid,
One or more in sulfuric acid, nitric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511015065.4A CN105621418B (en) | 2015-12-31 | 2015-12-31 | A kind of method for preparing Ludox |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511015065.4A CN105621418B (en) | 2015-12-31 | 2015-12-31 | A kind of method for preparing Ludox |
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| Publication Number | Publication Date |
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| CN105621418A CN105621418A (en) | 2016-06-01 |
| CN105621418B true CN105621418B (en) | 2017-09-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112299427B (en) * | 2020-10-29 | 2022-06-07 | 王庆乐 | Extraction process of vanadium extraction tailings |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164879A (en) * | 2007-09-26 | 2008-04-23 | 东北大学 | Method for producing white carbon black using by iron tailings |
| CN103359744A (en) * | 2013-07-17 | 2013-10-23 | 内蒙古科技大学 | Method for extracting white carbon black from mine tailing |
| CN103395792A (en) * | 2013-07-17 | 2013-11-20 | 内蒙古科技大学 | White carbon black preparation method |
-
2015
- 2015-12-31 CN CN201511015065.4A patent/CN105621418B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164879A (en) * | 2007-09-26 | 2008-04-23 | 东北大学 | Method for producing white carbon black using by iron tailings |
| CN103359744A (en) * | 2013-07-17 | 2013-10-23 | 内蒙古科技大学 | Method for extracting white carbon black from mine tailing |
| CN103395792A (en) * | 2013-07-17 | 2013-11-20 | 内蒙古科技大学 | White carbon black preparation method |
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| CN105621418A (en) | 2016-06-01 |
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