CN1315723C - Method for preparing high-purity ultrnfine silicone powder and aluminium sulphate using kadin as raw material - Google Patents
Method for preparing high-purity ultrnfine silicone powder and aluminium sulphate using kadin as raw material Download PDFInfo
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- CN1315723C CN1315723C CNB2005100491076A CN200510049107A CN1315723C CN 1315723 C CN1315723 C CN 1315723C CN B2005100491076 A CNB2005100491076 A CN B2005100491076A CN 200510049107 A CN200510049107 A CN 200510049107A CN 1315723 C CN1315723 C CN 1315723C
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- kaolinite
- metakaolin
- ace
- tai
- dioxide
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Abstract
The present invention discloses a method for preparing superfine silicone powder with high purity and aluminium sulphate by using kaolinite as a raw material. After being processed by drying, lapping, magnetic selection and calcination, ore is dissolved in dilute sulfuric acid. By filtration or centrifugal separation, an obtained solution is made into aluminum sulfate through concentration and cooling. A residue which is dissolved by acid is processed by chemical purification, granularity separation, re-magnetic selection and spray drying to obtain superfine silicone powder with high purity. Compared with the deep processing patent of the existing kaolinite, the present invention simultaneously uses aluminum elements and silicon elements in the kaolinite, improves the use factor of raw materials, reduces the discharge of waste materials and lowers production cost and energy consumption. The obtained superfine silicone powder with high purity is an important raw material in high technology industry, and aluminium sulphate is an important chemical and industrial raw material.
Description
Technical field
The present invention relates to kaolinite class mineral is the method for feedstock production silicon-dioxide and Tai-Ace S 150.
Background technology
Kaolinite class mineral are a kind of aluminium silicate minerals, extensive in distributed in nature, there is the huge kaolinite of reserves mineral deposit in China, kaolin is remained in deposition kaolin and weathering as south China, the coal series hard kaolinite in North China, the hydrothermal solution kaolin of southeastern coast, dickite (dickite), nakrite (nacrite) and halloysite (hallyosite claims halloysite again).In kaolinite class mineral, aluminium Siliciumatom ratio is 1: 1 relation.
Kaolinite class mineral are being used as ceramic raw material, papermaking paint and filler traditionally.Kaolinite also is used as the raw material of producing aluminum oxide and aluminium chlorohydroxide in recent years, as Chinese patent ZL95103368.9, ZL03147968.5, ZL91111359.2, ZL85107358 and ZL90107796.8 etc.In these patented technologies, only utilized the aluminium element in the kaolinite, element silicon then is used as waste sludge discharge, has wasted precious natural resources on the one hand, has also caused environmental pressure simultaneously.
Silicon materials are one of most important starting material of many new high-tech industries, are widely used in fields such as electronic component, optical fiber cable, solar cell, fine chemistry industry, synthetic crystal.Silicon-dioxide has the vigorous market requirement in fields such as silicon carbide, silicon nitride ceramics, electronic devices and components and precision optics glass.Therefore, utilize element silicon and aluminium element in the kaolinite class mineral to have important economic implications simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of is the method for feedstock production silicon-dioxide and Tai-Ace S 150 with kaolinite class mineral.
The molecular formula of kaolinite class mineral is Al
4[Si
4O
10] (OH)
6NH
2O, n=0 or 4.Kaolinite, dickite and nakrite do not contain crystal water, contain four crystal water in the halloysite molecule.
The preparation silicon-dioxide that the present invention proposes and the method steps of Tai-Ace S 150 are as follows:
1) with the oven dry of kaolinite class mineral, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 1～4 hour down at 600～800 ℃ then, product is a metakaolin;
2) using the ratio of 1.4～1.6 mol sulfuric acid in each hectogram metakaolin, is that 20～35% sulfuric acid mixes with metakaolin and concentration, is heated to 100～110 ℃, constant temperature stirring 2～3 hours;
3) filtered while hot or centrifugation, the crystallization of gained solution concentration promptly obtains Tai-Ace S 150;
4) use the ratio of 2～10 gram reductive agents in each hectogram metakaolin, with step 3) gained solid and concentration is that 0.2～0.5% reductant solution mixes, and the pH value of mixed solution is adjusted to 2～2.5 with sulfuric acid, and being heated to 40～60 ℃, constant temperature stirred 2～5 hours;
5) filtration or centrifugation solid-liquid two-phase, and water cleaning gained solid are higher than 6.5 until the pH value;
6) add the ratio of 0.2～0.3 liter of dispersant solution in each hectogram metakaolin, it with step 5) gained solid and concentration 0.1～0.3% dispersant, high-speed stirring makes the back hydrocyclone that is uniformly dispersed, or remove granularity greater than 5 microns particle with the precipitator method, use the high gradient magnetic separator wet magnetic separation then, remove magnetic impurity;
7) suspension filtered or the centrifugation after the purification, and water cleans solid phase 1～3 time, adds the ratio of 0.1 5～0.2 premium on currency in each hectogram metakaolin, adds water again and mixes, high-speed stirring makes the back spraying drying that is uniformly dispersed, and products therefrom is silicon-dioxide.
Said kaolinite class mineral are class natural mineral, and its chemical structural formula is Al
4[Si
4O
10] (OH)
6NH
2O, n=0 or 4.
Said metakaolin is a kaolinite class calcination of minerals dehydration after product, and its chemical structural formula is Al
2O
32SiO
2
Said reductive agent is V-Brite B (molecular formula Na
2S
2O
4), S-WAT (molecular formula Na
2SO
3), Sulfothiorine (molecular formula Na2S
2O
3) in one or more.
Said dispersion agent is tripoly phosphate sodium STPP (molecular formula Na
5P
3O
10) or Sodium hexametaphosphate 99 (molecular formula (NaPO
3)
6).
Advantage of the present invention is, technical process is simple, and facility investment is few; The main raw material wide material sources, cheap.Compare with existing kaolinite deep processing patented technology, the present invention has utilized aluminium element and the element silicon in the kaolinite class mineral simultaneously, has improved raw material availability, has reduced trash discharge, has reduced production cost and energy consumption.Products obtained therefrom silicon-dioxide is the important starting material of new high-tech industry, and Tai-Ace S 150 also is important chemistry and industrial chemicals.
Embodiment
With kaolinite class mineral is that the foundation of feedstock production silicon-dioxide and Tai-Ace S 150 is, sial is the basic comprising component of kaolinite class mineral, and they have different behaviors in the molten process of acid; Impure mineral and impurity element contained in the kaolinite class mineral can be removed by physics and chemical process.
Deposition kaolin, coal series hard kaolinite (being commonly called as coal gangue), hydrothermal solution kaolin, dickite (dickite), nakrite (nacrite) or halloysite (hallyosite) mineral deposit are mainly by the mineral composition of kaolinite class, impure mineral content is low, can directly use, and that kaolinite content is remained in the kaoline deposit in weathering is low, needs just can be used for the present invention through separating to purify.Kaolinic separating and purifying method is well-known.
All contain the iron titanium oxide mineral that quantity does not wait in the dissimilar kaolinite ores, as limonite, rhombohedral iron ore, ilmenite, anatase octahedrite, rutile etc., these mineral all have magnetic, after grinding, powder is carried out dry magnetic separation, can effectively reduce the content of magnetic impurity with intensity magnetic separator.Ore is calcined the organic matter that can remove on the one hand in the ore, can make kaolinite class mineral lose crystal water and hydroxyl simultaneously, change metakaolin into, the latter's acid acceptance is significantly less than the former, helps the sour molten of ore.
In the molten process of acid, the Al in the kaolinite class mineral
2O
3Enter solution, and SiO
2Remain in the solid phase.Excess sulfuric acid or sour molten overlong time all can cause SiO
2Enter solution with the silicic acid form, the quality of Tai-Ace S 150 in the solution is reduced.Separating the solid-liquid two-phase while hot is to reduce for fear of temperature to cause Tai-Ace S 150 crystallization from solution.
To obtaining the Tai-Ace S 150 crystallization after the solution concentration cooling, it need not further purification can satisfy most of industrial uses.Tai-Ace S 150 can directly be put on market, also can use known technology further to refine Al
2O
3And sulfuric acid, the latter can reuse on stream.If need to improve the purity level of Tai-Ace S 150, can from alum liquor, extract iron with alkyl organic acid (6～10 carbon atoms of carbon chain lengths), be that 10～25% dilute sulphuric acid is stripped the repeated use so that organic acid circulates to organic acid with concentration then.After the organic acid extraction, iron level greatly reduces in the alum liquor, can obtain the chemical pure product after concentrating cooling.
The acid soluble leftover of metakaolin is mainly amorphous Si O
2, under acidic conditions, handle with reductive agent, can remove the ferrimanganic of trace and residual Al
2O
3The consumption of reductive agent can suitably be adjusted according to the iron level in the kaolinite ore.
Impure mineral capacity antacid in the kaolinite generally all is better than metakaolin, and some ferrotianium oxide minerals that originally wrapped up by kaolinite are monomer and exist after acid is molten, solid phase is carried out particle size separation and wet magnetic separation after, these impurity all can be removed.Using dispersion agent before purifying is in order to overcome amorphous Si O
2Between reunion, use the high-shear dispersion machine to improve and disperse and refining effect.If use the precipitator method to carry out particle size separation, the degree of depth of suspension and sedimentation time can be calculated with following experimental formula:
Y＝0.124X+0.017
X is the degree of depth (unit centimetre) of suspension in the formula, and Y is sedimentation time (unit hour).The degree of depth of suspension should be controlled in one meter, to improve the rate of recovery.
Silica flour after purifying is filtered or centrifugation and washing, is in order further to remove soluble impurity.Should control water consumption when adding water slurrying again, to reduce the energy consumption of drying process.Use spray drying technology can effectively avoid the reunion of material, obtain superfine powder in drying process.Spray-dired temperature suggestion is controlled at 120～180 ℃.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: with deposition kaolin is feedstock production silicon-dioxide and Tai-Ace S 150.
1) raw material is a deposition kaolin of taking from the somewhere, south China.With raw material stoving, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 4 hours down at 600 ℃ then, obtain metakaolin;
2) get one kilogram of metakaolin, add 5.5 liters of concentration and be 30% sulfuric acid, mix post-heating to 100 ℃, constant temperature stirred 3 hours;
3) filter with vacuum filter while hot, the crystallization of gained solution concentration is obtained Tai-Ace S 150;
4) be that 0.3% SODIUM HYDROSULPHITE sodium solution mixes with step 3) gained solid and 2.5 liters of concentration, and the pH value of mixed solution be adjusted to 2.3 that be heated to 50 ℃, constant temperature stirred 4 hours with sulfuric acid;
5) filter with vacuum filter, and water cleaning gained solid, equal 6.7 until the pH value;
6) be that 0.1% sodium tripolyphosphate solution mixes with step 5) gained solid and 3 liters of concentration, high-speed stirring makes the back that is uniformly dispersed remove granularity greater than 5 microns particle with hydrocyclone, uses the high gradient magnetic separator wet magnetic separation then, removes magnetic impurity;
7) suspension after the purification filters with vacuum filter, and water cleaning solid phase, adds 2 premium on currency after filtering once more, and high-speed stirring makes the back spraying drying under 160 ℃ of temperature that is uniformly dispersed, and products therefrom is silicon-dioxide.
Embodiment 2: be feedstock production silicon-dioxide and Tai-Ace S 150 with the coal series hard kaolinite.
1) raw material is a coal series hard kaolinite (being coal gangue) of taking from the somewhere, North China.With raw material stoving, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 2 hours down at 800 ℃ then, obtain metakaolin;
2) get one kilogram of metakaolin, add 6 liters of concentration and be 25% sulfuric acid, mix post-heating to 105 ℃, constant temperature stirred 2 hours;
3) centrifugation while hot obtains Tai-Ace S 150 with the crystallization of gained solution concentration;
4) be that 0.3% sodium sulfite solution mixes with step 3) gained solid and 3 liters of concentration, and the pH value of mixed solution be adjusted to 2.4 that be heated to 60 ℃, constant temperature stirred 3 hours with sulfuric acid;
5) centrifugation, and water cleaning gained solid equal 6.6 until the pH value;
6) be that 0.2% sodium hexametaphosphate solution mixes with step 5) gained solid and 3 liters of concentration, pour the degree of depth after high-speed stirring makes and is uniformly dispersed into and be in 80 centimetres the plastic barrel, after leaving standstill 10 hours, with siphonage sucking-off suspension, with high gradient magnetic separator suspension is carried out wet magnetic separation then, remove magnetic impurity;
7) solid phase is cleaned in the suspension centrifugation after the purification, and water, and recentrifuge adds 1.5 premium on currency after separating, and high-speed stirring makes the back spraying drying under 140 ℃ of temperature that is uniformly dispersed, and products therefrom is silicon-dioxide.
Embodiment 3: be feedstock production silicon-dioxide and Tai-Ace S 150 with the dickite.
1) raw material is a dickite of taking from the somewhere, Zhejiang.With raw material stoving, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 3 hours down at 700 ℃ then, obtain metakaolin;
2) get one kilogram of metakaolin, add 4.5 liters of concentration and be 35% sulfuric acid, mix post-heating to 110 ℃, constant temperature stirred 2 hours;
3) centrifugation while hot obtains Tai-Ace S 150 with the crystallization of gained solution concentration;
4) be that 0.3% hypo solution mixes with step 3) gained solid and 3 liters of concentration, and the pH value of mixed solution be adjusted to 2.5 that be heated to 50 ℃, constant temperature stirred 3 hours with sulfuric acid;
5) centrifugation, and water cleaning gained solid equal 6.8 until the pH value;
6) be that 0.2% sodium tripolyphosphate solution mixes with step 5) gained solid and 2 liters of concentration, pour the degree of depth after high-speed stirring makes and is uniformly dispersed into and be in 50 centimetres the plastic barrel, after leaving standstill 6 hours 12 minutes, with siphonage sucking-off suspension, with high gradient magnetic separator suspension is carried out wet magnetic separation then, remove magnetic impurity;
7) solid phase is cleaned in the suspension centrifugation after the purification, and water, and recentrifuge adds 1.5 premium on currency after separating, and high-speed stirring makes the back spraying drying under 180 ℃ of temperature that is uniformly dispersed, and products therefrom is silicon-dioxide.
Embodiment 4: be feedstock production silicon-dioxide and Tai-Ace S 150 with the halloysite.
1) raw material is a halloysite of taking from the somewhere, south China.With raw material stoving, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 3 hours down at 600 ℃ then, obtain metakaolin;
2) get one kilogram of metakaolin, add 5 liters of concentration and be 30% sulfuric acid, mix post-heating to 100 ℃, constant temperature stirred 2 hours;
3) centrifugation while hot obtains Tai-Ace S 150 with the crystallization of gained solution concentration;
4) be that 0.2% SODIUM HYDROSULPHITE sodium solution mixes with step 3) gained solid and 3 liters of concentration, and the pH value of mixed solution be adjusted to 2.3 that be heated to 40 ℃, constant temperature stirred 5 hours with sulfuric acid;
5) centrifugation, and water cleaning gained solid equal 6.6 until the pH value;
6) be that 0.2% sodium tripolyphosphate solution mixes with step 5) gained solid and 3 liters of concentration, high-speed stirring makes the back that is uniformly dispersed remove granularity greater than 5 microns particle with hydrocyclone, uses the high gradient magnetic separator wet magnetic separation then, removes magnetic impurity;
7) solid phase is cleaned in the suspension centrifugation after the purification, and water, and recentrifuge adds 2 premium on currency after separating, and high-speed stirring makes the back spraying drying under 140 ℃ of temperature that is uniformly dispersed, and products therefrom is silicon-dioxide.
Claims (4)
1. one kind is the method for feedstock production silicon-dioxide and Tai-Ace S 150 with kaolinite class mineral, it is characterized in that its step is as follows:
1) with the oven dry of kaolinite class mineral, be ground to less than 300 orders, use intensity magnetic separator that powder is carried out dry magnetic separation, remove magnetic impurity, calcined 1～4 hour down at 600～800 ℃ then, product is a metakaolin;
2) using the ratio of 1.4～1.6 mol sulfuric acid in each hectogram metakaolin, is that 20～35% sulfuric acid mixes with metakaolin and concentration, is heated to 100～110 ℃, constant temperature stirring 2～3 hours;
3) filtration or centrifugation, the crystallization of gained solution concentration promptly obtains Tai-Ace S 150;
4) use the ratio of 2～10 gram reductive agents in each hectogram metakaolin, with step 3) gained solid and concentration is that 0.2～0.5% reductant solution mixes, and the pH value of mixed solution is adjusted to 2～2.5 with sulfuric acid, and being heated to 40～60 ℃, constant temperature stirred 2～5 hours;
5) filtration or centrifugation solid-liquid two-phase, and water cleaning gained solid are higher than 6.5 until the pH value;
6) add the ratio of 0.2～0.3 liter of dispersant solution in each hectogram metakaolin, it with step 5) gained solid and concentration 0.1～0.3% dispersant, high-speed stirring makes the back hydrocyclone that is uniformly dispersed, or remove granularity greater than 5 microns particle with the precipitator method, use the high gradient magnetic separator wet magnetic separation then, remove magnetic impurity;
7) suspension filtered or the centrifugation after the purification, and water cleans solid phase 1～3 time, adds the ratio of 0.15～0.2 premium on currency in each hectogram metakaolin, adds water again and mixes, high-speed stirring makes the back spraying drying that is uniformly dispersed, and products therefrom is silicon-dioxide.
2. according to claim 1 a kind of be the method for feedstock production silicon-dioxide and Tai-Ace S 150 with kaolinite class mineral, it is characterized in that, said kaolinite class mineral, its chemical structural formula is Al
4[Si
4O
10] (OH)
6NH
2O, n=0 or 4, it comprises kaolinite, dickite, nakrite or halloysite.
3. according to claim 1 a kind of be the method for feedstock production silicon-dioxide and Tai-Ace S 150 with kaolinite class mineral, it is characterized in that said reductive agent is one or more in V-Brite B, S-WAT or the Sulfothiorine.
4. according to claim 1 a kind of be the method for feedstock production silicon-dioxide and Tai-Ace S 150 with kaolinite class mineral, it is characterized in that said dispersion agent is tripoly phosphate sodium STPP or Sodium hexametaphosphate 99.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986412B (en) * | 2005-12-22 | 2011-02-16 | 赵振民 | Low pressure leaching process of coal-bearing kaolin powder for producing industrial aluminum sulfate |
| CN105108172B (en) * | 2015-09-14 | 2017-05-10 | 山东大学 | Method for preparing silicon powder |
| CN105800615B (en) * | 2016-02-23 | 2017-11-14 | 吉林大学 | A kind of method that porous elemental silicon powder is prepared using natural silicon aluminium acid salt mineral |
| CN106277009A (en) * | 2016-07-28 | 2017-01-04 | 青岛惠城环保科技股份有限公司 | A kind of preparation method of aluminum sulfate |
| CN109574024B (en) * | 2019-01-14 | 2022-03-25 | 中国科学院兰州化学物理研究所 | Method for preparing silicon dioxide nano material by using natural one-dimensional nano clay mineral |
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2005
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Patent Citations (5)
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| CN1037363A (en) * | 1988-05-07 | 1989-11-22 | 山西师范大学 | The method of comprehensive utilization of low-grade aluminium ore |
| CN1046507A (en) * | 1989-04-21 | 1990-10-31 | 李抚立 | Kaolin is produced the method for poly aluminium chloride and white carbon black |
| CN1094696A (en) * | 1994-03-28 | 1994-11-09 | 余有宏 | A kind of new production process of precipitated silica |
| CN1116609A (en) * | 1994-08-06 | 1996-02-14 | 温宝礼 | Method for producing aluminium fluoride and cryolite with kaoline |
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| Title |
|---|
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