CN102234116B - Method for preparing nano white carbon black by utilizing iron tailings - Google Patents
Method for preparing nano white carbon black by utilizing iron tailings Download PDFInfo
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- CN102234116B CN102234116B CN 201110071373 CN201110071373A CN102234116B CN 102234116 B CN102234116 B CN 102234116B CN 201110071373 CN201110071373 CN 201110071373 CN 201110071373 A CN201110071373 A CN 201110071373A CN 102234116 B CN102234116 B CN 102234116B
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- iron tailings
- sodium silicate
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- silicate solution
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Abstract
The invention relates to a method for preparing nano white carbon black by taking iron tailings as raw materials. The method comprises the following steps of: mixing and calcining the iron tailings activated at a high temperature and caustic soda at the temperature of 400-500 DEG C, then directly pouring the mixture into a water bath at the temperature of 70-90 DEG C to fully react, filtering to obtain a sodium silicate solution, adding a dispersing agent NaCl and a surfactant normal butanol into the sodium silicate solution, slowly dropwise adding 5-10wt% HCl for acidification under the stirring condition to generate massive white flocculent precipitates, and then ageing, filtering, washing and drying, thus the nano white carbon black product is obtained. The method is simple to operate and has low cost, high product yield and fine particle size and is applicable to industrialization production.
Description
Technical field
The present invention relates to the method that a kind of iron tailings prepares Nano carbon white, belong to field of inorganic nonmetallic material.
Background technology
Along with the continuous progress of science and technology, how industrial production constantly towards intelligent, low energy consumption, high-environmental future development, realizes taking full advantage of of existing resource, has become the problem of various circles of society's extensive concern.Iron tailings is a kind of solid waste, and along with the fast development of steel and iron industry, iron tailings shared ratio in industrial solid castoff is also increasing.Under the restriction of the factors such as technology and ore-dressing technique, the iron ore deposit rate of recovery is on the low side in history in China.The characteristics such as the quantity of adding iron tailings itself is huge, structural behaviour is complicated, type is more make it very low in China's utilization rate, only are 7%.Causing puzzlement on the one hand our environment, also is the waste of resource on the other hand.It not only makes the mineral resources of China not be fully used, and has also taken a large amount of land resource, has consumed a large amount of funds, has affected the economic benefit of enterprise.Main component is SiO in the iron tailings
2And a small amount of Fe
2O
3, MgO, Al
2O
3, CaO etc. (place of production is different, and composition is slightly variant).Wherein, SiO
2Content generally greater than 50wt%, have very large value of exploiting and utilizing.Therefore, from iron tailings, extract white carbon (being hydrated SiO 2), can realize to a greater extent effectively utilization of resource, and improve value-added content of product.
Application number is that 200710012954.4 patent of invention has proposed a kind of method of utilizing iron tailings to prepare white carbon, the steps such as the method is molten through alkali, acidifying, precipitation, washing are prepared white carbon, but this method is because the alkali solubility temperature is lower, be 50-120 ℃, the productive rate of white carbon is not high, and product granularity is also thicker.Application number is that 96115532.9 patent of invention has proposed a kind of method of producing active carbon white with gangue, the method adopts comminuted coal spoil and soda ash batch mixing, and, shrend molten in 1400-1500 ℃ of high temperature smelting, soak the steps such as molten, concentrated, acidifying, ageing, washing and prepare white carbon, because this method needs the high temperature smelting molten, therefore energy consumption is too high, side reaction also occuring under the hot conditions in addition easily, cause the impurity generations such as indissoluble silicate, reduces purity and the productive rate of white carbon black product.
The present invention is different from above-mentioned report, mainly for the present situation of utilizing of China's iron tailings, has proposed a kind of new technology and new technology of utilizing iron tailings to prepare Nano carbon white.This technique has that technique is simple, energy consumption is low, cost is low, product cut size can reach nanoscale, added value of product is high, comprehensive utilization of tailing rate high; be suitable for suitability for industrialized production, for the development of comprehensive utilization, environmental protection and even the stake holder economy of iron tailings all tool be of great significance.
Summary of the invention
The present invention relates generally to a kind of method for preparing Nano carbon white take iron tailings as raw material, and concrete summary of the invention is as follows:
1) calcining and activating of iron tailings: below iron tailings ball milling to 200 order, 800～900 ℃ of calcinings of Muffle furnace, 2～4h.
2) iron tailings and caustic soda mixed calcining: the iron tailings after will activating and solid NaOH are by mass fraction iron tailings: NaOH=100: 200～300 mix, and place Muffle furnace in 400～500 ℃ of calcining 0.5～2h.
3) prepare silicon acid sodium solution: above-mentioned compound is taken out in mass ratio compound under calcining heat: water=15: 100～200 are poured rapidly quenching 70～90 ℃ the water into, and react 0.5～2h under stirring, make SiO
2Fully react with NaOH, after the filtration, gained filtrate is sodium silicate solution.
4) precipitating Nano carbon white: in above-mentioned sodium silicate solution, activate in mass ratio iron tailings: NaCl=100: 40～60, add solid NaCl as dispersant, sodium silicate solution by volume: n-butanol=100: 4～6 add n-butanol as surfactant, and drip the HCl acidifying of 5～10wt% under slow stirrings, until pH is adjusted to 7～9, produce a large amount of white flocculent deposits, ageing 1～2h filters the thick product that obtains Nano carbon white.
5) washing of white carbon: the thick product of white carbon is washed, until check Na in the product
+, Cl
-Till content is qualified, Na wherein
+＜1wt%, Cl
-＜1wt%.
6) calcining of white carbon: the product after the washing is pulverized in 100～200 ℃ of drying 1～2h, obtains final products.
Description of drawings
Fig. 1 is the process chart that iron tailings of the present invention prepares Nano carbon white.
Fig. 2 is the scanning electron microscope (SEM) photograph with the Nano carbon white of preparing under example 1 process conditions.
The specific embodiment
The present invention is described in detail below in conjunction with embodiment, and the present invention is not limit by these manufacturing examples.
Example 1
Below iron tailings ball milling to 200 order, 850 ℃ of calcinings of Muffle furnace 3h mixes the 100g iron tailings after the activation with the NaOH of 300g, and places Muffle furnace in 500 ℃ of calcining 1h; Pour rapidly 4500ml into after compound after the calcining taken out under the calcining heat, in 90 ℃ of water-baths, and stirring reaction 2h, filter, obtain sodium silicate solution; Add 60gNaCl and n-butanol 200ml in sodium silicate solution, and drip the HCl acidifying of 5wt% under slow stirring, until pH is adjusted to 7, produce a large amount of white flocculent deposits, ageing 1h filters the thick product that obtains Nano carbon white; The thick product of white carbon is washed, checked Cl
-, Na
+Content is all less than till the 1wt%; In 200 ℃ of dry 2h, pulverize after the product washing, obtain final products, product cut size can reach 30～50nm.
Example 2
Below iron tailings ball milling to 200 order, 800 ℃ of calcinings of Muffle furnace 4h mixes the 100g iron tailings after the activation with the NaOH of 250g, and places Muffle furnace in 400 ℃ of calcining 2h; Pour rapidly 3000ml into after compound after the calcining taken out under the calcining heat, in 80 ℃ of water-baths, and stirring reaction 1h, filter, obtain sodium silicate solution; Add 50gNaCl and n-butanol 150ml in sodium silicate solution, and drip the HCl acidifying of 10wt% under slow stirring, until pH is adjusted to 9, produce a large amount of white flocculent deposits, ageing 1.5h filters the thick product that obtains Nano carbon white; The thick product of white carbon is washed, checked Cl
-, Na
+Content is all less than till the 1wt%; In 200 ℃ of dry 1h, pulverize after the product washing, obtain final products, product cut size can reach 50～100nm.
Example 3
Below iron tailings ball milling to 200 order, 900 ℃ of calcinings of Muffle furnace 3h mixes the 100g iron tailings after the activation with the NaOH of 200g, and places Muffle furnace in 450 ℃ of calcining 1h; Pour rapidly 2000ml into after compound after the calcining taken out under the calcining heat, in 70 ℃ of water-baths, and stirring reaction 0.5h, filter, obtain sodium silicate solution; Add 45gNaCl and n-butanol 90ml in sodium silicate solution, and drip the HCl acidifying of 10wt% under slow stirring, until pH is adjusted to 8, produce a large amount of white flocculent deposits, ageing 1h filters the thick product that obtains Nano carbon white; The thick product of white carbon is washed, checked Cl
-, Na
+Content is all less than till the 1wt%; In 100 ℃ of dry 2h, pulverize after the product washing, obtain final products, product cut size can reach 50～80nm.
Claims (1)
1. method for preparing Nano carbon white from iron tailings is characterized in that its processing step is:
Below iron tailings ball milling to 200 order, and in 800～900 ℃ of calcinings of Muffle furnace, 2～4h activation, iron tailings after the activation and solid NaOH activate iron tailings: NaOH=100 in mass ratio: 200～300 mix, place Muffle furnace in 400～500 ℃ of calcining 0.5～2h, above-mentioned compound directly takes out under calcining heat, and compound in mass ratio: water=15: 100～200 are poured into rapidly in 70～90 ℃ the water and are cooled off, and under stirring, react 0.5～2h, after the filtration, gained filtrate is sodium silicate solution, in sodium silicate solution, activate in mass ratio iron tailings: NaCl=100: 40～60, add solid NaCl and make dispersant, sodium silicate solution by volume: n-butanol=100: 4～6, add n-butanol and make surfactant, and under slow stirring, drip the HCl acidifying of 5～10wt%, until pH is adjusted to 7～9, produce a large amount of white flocculent deposits, ageing 1～2h, filtration obtains the thick product of Nano carbon white, the thick product of white carbon is washed, until check Na in the product
+, Cl
-Till content is qualified, Na wherein
+＜1wt%, Cl
-＜1wt%, the product after the washing pulverize in 100～200 ℃ of drying 1～2h, obtain final products.
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| CN102234116B true CN102234116B (en) | 2013-04-10 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011881B (en) * | 2012-12-27 | 2015-04-29 | 山东宏艺科技股份有限公司 | Method for increasing quartz sand tailing powder content in aerated concrete product |
| CN103086488B (en) * | 2013-01-20 | 2014-04-09 | 河北联合大学 | Method for preparing flocculating agent, namely polyaluminum ferric silicate from galvanized sludge and 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 |
| CN103435053A (en) * | 2013-09-04 | 2013-12-11 | 沈阳化工大学 | Method for preparing high-dispersion nano white black carbon from sodium silicate |
| CN103626189A (en) * | 2013-12-04 | 2014-03-12 | 沈阳化工大学 | Method for preparing high-dispersion nano silica from organic acid and sodium silicate |
| CN105752994A (en) * | 2016-04-29 | 2016-07-13 | 攀枝花学院 | Method for preparing white carbon black from graphite tailings |
| CN109516466A (en) * | 2017-09-18 | 2019-03-26 | 湖南行者环保科技有限公司 | A method of high-purity white carbon is prepared by silicon-containing material |
| CN108910900A (en) * | 2018-07-18 | 2018-11-30 | 浙江工业大学 | A method of iron oxide and silica nano material are prepared simultaneously from iron tailings |
| CN108658130B (en) * | 2018-07-18 | 2020-08-25 | 浙江工业大学 | Method for simultaneously preparing iron oxide and silicon dioxide aerogel from iron tailings |
| CN109133072B (en) * | 2018-08-28 | 2020-08-11 | 浙江工业大学 | Method for preparing hydrophobic silica aerogel by using iron tailings as raw materials at ultra-fast speed |
| CN109012517B (en) * | 2018-08-28 | 2020-09-29 | 浙江工业大学 | Method for preparing composite silicon-based aerogel by taking iron tailings as raw materials |
| CN109622576B (en) * | 2019-01-31 | 2021-04-06 | 河北工业大学 | Method for treating high-salt solid waste by using iron tailings |
| CN110284004B (en) * | 2019-06-25 | 2021-03-23 | 中南大学 | Method for synergistically recycling copper slag and sodium sulfate waste slag |
| CN113353950A (en) * | 2021-07-02 | 2021-09-07 | 鞍钢集团矿业有限公司 | Method for preparing SBA-15 molecular sieve by using iron tailings |
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| CN1174168A (en) * | 1996-08-15 | 1998-02-25 | 鞠馥阳 | Production process of active silica white from gangue |
| CN100484873C (en) * | 2007-04-29 | 2009-05-06 | 东北大学 | Method for preparing white carbon black by using oil shale ash |
| CN101164879A (en) * | 2007-09-26 | 2008-04-23 | 东北大学 | Method for producing white carbon black using by iron tailings |
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