CN101045538A - Method for preparing modified silicon oxide using coal series kaolin rock or flyash - Google Patents
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Abstract
A process for preparing the modified silicon oxide from the coal kaolinite or powdered coal ash includes such steps as baking, grinding, magnetic separation, calcining, extracting in organic acid to obtain Si-enriched deposit and Al-enriched solution, processing said Al-enriched solution through refining, concentrating and crystallizing to obtain Al salt, processing the Si-enriched deposit through alkali dissolving and acid depositing to obtain crude silicon oxide, activating it by acid, hydroxylating, filtering, washing, and surface modifying by coupling agent.
Description
Technical field
The present invention relates to coal series kaolin rock or Ash Utilization deep processing and utilization field, particularly a kind of method with coal series kaolin rock or fly-ash Preparation modified silicon oxide.
Background technology
Coal series kaolin rock and flyash are mainly by Al
2O
3And SiO
2Form, in that coal series kaolin rock and flyash are counted as trade waste traditionally, near coal-mine and coal washery in the Chinese large-sized colliery, and large-scale coal fired thermal power plant all has coal series kaolin rock and the flyash that pile up like a mountain, and in speed increase with several hundred million tons of every year, not only occupied a large amount of soils, and serious pollution of ecological environment, big public hazards become.
The expansion of China's aluminum smelting technology industry production capacity makes the aluminum oxide of domestic and international market the situation that supply falls short of demand occur, also cause domestic bauxite resource critical shortage, for guaranteeing China's bauxite resource supply security, and alleviate the unbalance contradiction of world market bauxite resource supply and demand, the technical need of extracting aluminum oxide and fully utilize silicon oxide from coal gangue and flyash seems very urgent.
The recycling direction of coal series kaolin rock or flyash mainly is to be used for extracting aluminium salt and to produce aluminum oxide, but remaining white residue is only as trade waste or be used to produce cement, annual output 1 ten thousand t aluminum oxide and 10 ten thousand t Cement Production lines have been built up in nineteen fifty-three with this technology as Poland, this technology exists unreasonable products structure and problems such as high material-consumption, high energy consumption, is difficult to further develop.High-purity silicon oxide is the important materials of many new high-tech industries, be widely used in fields such as polymer composite, special ink, paint, coating, pottery, electronic devices and components and precision optics glass, fast development along with new high-tech industry, high-grade, the high purity of many kinds, the market requirement of functional modification silica product constantly increase, and have the vigorous market requirement.Therefore, utilize coal series kaolin rock or fly-ash Preparation high-purity silicon oxide and modified product thereof significant.
Also as the raw material of preparation white carbon black class, because product orientation mainly is primary products, added value is low traditionally for China's coal series kaolin rock or flyash white residue, economic benefit is not obvious, high-purity white carbon black production of China and modification technology are relatively backward, can only manufacture experimently on a small scale, and second-rate.The market of present Chinese modified white carbon black is captured by The foreign chicken products such as the U.S., Germany, Japan basically.
Summary of the invention
The purpose of this invention is to provide a kind of method with coal series kaolin rock or fly-ash Preparation modified silicon oxide.
With the method for coal series kaolin rock or fly-ash Preparation modified silicon oxide is to be raw material with coal series kaolin rock or flyash, be processed into Silicon-rich solid phase and rich aluminum solutions mutually by acidleach, the Silicon-rich solid phase is molten through alkali, Acid precipitation, acid activation purification, surface modification make modified silicon oxide, and concrete step is as follows:
1) with the oven dry of coal series kaolin rock or flyash, pulverize, dry magnetic separation then 550～850 ℃ of calcinings 1～4 hour down, is that 20～35% acid mixes with mass percent concentration, 100～250 ℃ of following lixiviates 1～4 hour; Filter or centrifugation, with the Silicon-rich solid phase molten generation water glass of alkali, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the acid of 1～3M is 60～90 ℃ of activation 2～3 hours in temperature with step 1) gained crude product silicon oxide concentration, the pH of the hierarchy of control is not higher than 4, filter, and washing, drying promptly gets active oxidation silicon;
3) with step 2) gained active oxidation silicon is that 1: 5～10 ratio is scattered in the organic solvent in solid-to-liquid ratio, add the coupling agent that is equivalent to active oxidation silicon weight 0.5～10% in addition, be warming up to back flow reaction 0.5～2 hour, and filtered, filtration cakes torrefaction then obtains modified silicon oxide.
Described acid is hydrochloric acid, sulfuric acid or nitric acid.Organic solvent is methyl alcohol, ethanol, propyl alcohol or Virahol.Coupling agent is silane coupling agent, titanate coupling agent or stearic acid coupling agent.Silane coupling agent is trimethylethoxysilane, methyltrimethoxy silane, vinyltriethoxysilane, four butoxy silanes or hexamethyldisilazane.Titanate coupling agent is the positive butyl ester of metatitanic acid (four) isopropyl ester or metatitanic acid (four).The stearic acid coupling agent is stearic acid, iron stearate, calcium stearate or Magnesium Stearate.
Operational condition gentleness of the present invention, technology is simple, and facility investment and energy consumption are little; Raw material sources are wide, and price is low; Compare with existing coal series kaolin rock or flyash deep process technology, the product of preparation has higher market orientation, can be widely used in new high-tech industries such as polymer composite, special ink, paint, coating, pottery, electronic devices and components and precision optics glass, have good economic and social benefit.
Embodiment
The present invention is a metakaolin with coal series kaolin rock or flyash oven dry, grinding, magnetic separation, calcining, by forming Silicon-rich precipitated phase and rich aluminum solutions with inorganic acid leaching mutually, rich aluminium liquid phase through refining, concentrate, crystallization gets aluminium salt; The Silicon-rich solid phase is filtered through the molten water glass that gets of alkali, adds the mineral acid precipitation and makes the silicon oxide crude product.The method of removal of impurities, activation, soda acid lixiviate is well-known.
The silicon oxide surface modification comprises activation pre-treatment and surface modification two steps, and (OH) content is the key factor that influences modified effect to hydroxy on the silicon oxide surface.Method with coal series kaolin rock or fly-ash Preparation modified silicon oxide product provided by the present invention, it is characterized in that utilizing the katalysis in the mineral acid, make siloxane bond (Si-O-Si) fracture, obtain fully hydroxylated (silicon oxide particle OH) in surface, improve the effect of follow-up coupling agent surface modification, can improve its dispersiveness and consistency in organic phase.
In addition, coal series kaolin rock or flyash are after acidleach is got, foreign matter contents such as iron, titanium, calcium, magnesium are lower in the white residue, but contain a certain amount of aluminum oxide of not carried by acidleach, when with alkali lye and silicon oxide reaction, also there is aluminum oxide to participate in simultaneously, generate sodium metaaluminate and enter in the solution, in post-order process, mix among white carbon black, influence quality product with the amorphous aluminosilicate form; Method with coal series kaolin rock or fly-ash Preparation modified silicon oxide product provided by the present invention, in the operation of active oxidation silicon, after filtration, washing can further remove impurity such as aluminium, iron, calcium, magnesium, refining, activation two steps unite two into one, technology is simple.
The present invention is further described in conjunction with following example, but content of the present invention is not limited only to content related among the embodiment.
Embodiment 1
1) with the oven dry of coal series kaolin rock or flyash, pulverize, dry magnetic separation, then 550 ℃ of calcinings 1 hour down, with mass percent concentration be 20% mixed in hydrochloric acid, 100 ℃ of following lixiviates 1 hour; Filter or centrifugation, with the Silicon-rich solid phase molten generation water glass of alkali, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the hydrochloric acid of 1M is 60 ℃ of activation 2 hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=2 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon;
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the methyl alcohol organic solvent in solid-to-liquid ratio, add the trimethylethoxysilane that is equivalent to active oxidation silicon weight 0.5% in addition, be warming up to back flow reaction 0.5 hour, and filtered, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 2
1) with the oven dry of coal series kaolin rock or flyash, pulverize, dry magnetic separation then 850 ℃ of calcinings 4 hours down, is that 35% sulfuric acid mixes with mass percent concentration, 250 ℃ of following lixiviates 4 hours; Filter or centrifugation, with the Silicon-rich solid phase molten generation water glass of alkali, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the sulfuric acid of 3M is 90 ℃ of activation 3 hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=3 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon;
3) with step 2) gained active oxidation silicon is that 1: 10 ratio is scattered in the organic solvent in solid-to-liquid ratio, add metatitanic acid (four) isopropyl ester that is equivalent to active oxidation silicon weight 10% in addition, be warming up to back flow reaction 2 hours, and filtered, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 3
1) with coal series kaolin rock oven dry, pulverize, dry magnetic separation, then 550 ℃ of calcinings 4 hours down, with mass percent concentration be 20% mixed in hydrochloric acid, 100 ℃ of following lixiviates 1 hour; Filter, the Silicon-rich solid phase is generated water glass with dissolution of sodium hydroxide, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the hydrochloric acid of 1M is 60 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=3.8 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the methyl alcohol in solid-to-liquid ratio, add the trimethylethoxysilane that is equivalent to active oxidation silicon weight 0.5% in addition, be warming up to back flow reaction 0.5 hour, and filtered, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 4
1) with coal series kaolin rock oven dry, to pulverize, dry magnetic separation then 850 ℃ of calcinings 1 hour down, is that 35% sulfuric acid mixes with mass percent concentration, 250 ℃ of following lixiviates 4 hours; Centrifugation generates water glass with the Silicon-rich solid phase with the yellow soda ash dissolving, through precipitation, and filtration, washing, the dry crude product silicon oxide that gets;
2) be that the sulfuric acid of 1M is 90 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=3 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the ethanol in solid-to-liquid ratio, adds the hexamethyldisilazane that is equivalent to active oxidation silicon weight 10% in addition, is warming up to back flow reaction 2 hours, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 5
1) with flyash oven dry, to pulverize, dry magnetic separation then 650 ℃ of calcinings 2 hours down, is that 25% nitric acid mixes with mass percent concentration, 125 ℃ of following lixiviates 2 hours; Filter, the Silicon-rich solid phase is generated water glass with the yellow soda ash dissolving, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the nitric acid of 1M is 70 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=2 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the propyl alcohol in solid-to-liquid ratio, adds metatitanic acid (four) isopropyl ester that is equivalent to active oxidation silicon weight 2% in addition, is warming up to back flow reaction 1 hour, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 6
1) with coal series kaolin rock oven dry, to pulverize, dry magnetic separation then 700 ℃ of calcinings 2 hours down, is that 25% sulfuric acid mixes with mass percent concentration, 200 ℃ of following lixiviates 2 hours; Filter, the Silicon-rich solid phase is generated water glass with dissolution of sodium hydroxide, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the sulfuric acid of 1M is 90 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=1 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the Virahol in solid-to-liquid ratio, adds the positive butyl ester of the metatitanic acid (four) that is equivalent to active oxidation silicon weight 5% in addition, is warming up to back flow reaction 1.5 hours, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 7
1) with coal measures flyash oven dry, to pulverize, dry magnetic separation then 750 ℃ of calcinings 1.5 hours down, is that 30% nitric acid mixes with mass percent concentration, 150 ℃ of following lixiviates 3 hours; Filter or centrifugation, the Silicon-rich solid phase is generated water glass with the yellow soda ash dissolving, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the nitric acid of 1M is 80 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=2.5 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the ethanol in solid-to-liquid ratio, adds the stearic acid that is equivalent to active oxidation silicon weight 2% in addition, is warming up to back flow reaction 1.5 hours, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 8
1) with coal measures flyash oven dry, pulverize, dry magnetic separation, then 600 ℃ of calcinings 4 hours down, with mass percent concentration be 35% mixed in hydrochloric acid, 150 ℃ of following lixiviates 3.5 hours; Filter or centrifugation, the Silicon-rich solid phase is generated water glass with dissolution of sodium hydroxide, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the hydrochloric acid of 1M is 60 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=2.5 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the Virahol in solid-to-liquid ratio, adds the calcium stearate that is equivalent to active oxidation silicon weight 4% in addition, is warming up to back flow reaction 2 hours, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Embodiment 9
1) with coal series kaolin rock oven dry, to pulverize, dry magnetic separation then 650 ℃ of calcinings 4 hours down, is that 35% sulfuric acid mixes with mass percent concentration, 180 ℃ of following lixiviates 2 hours; Centrifugation generates water glass with the Silicon-rich solid phase with the yellow soda ash dissolving, through precipitation, and filtration, washing, the dry crude product silicon oxide that gets;
2) be that the sulfuric acid of 1M is 70 ℃ of activation two hours in temperature with step 1) gained crude product silicon oxide concentration, the pH=1 of the hierarchy of control filters, washing, and drying promptly gets active oxidation silicon.
3) with step 2) gained active oxidation silicon is that 1: 5 ratio is scattered in the ethanol in solid-to-liquid ratio, adds the Magnesium Stearate that is equivalent to active oxidation silicon weight 6% in addition, is warming up to back flow reaction 1.5 hours, filters, filtration cakes torrefaction then obtains modified silicon oxide.
Claims (7)
1. method with coal series kaolin rock or fly-ash Preparation modified silicon oxide, it is characterized in that it is is raw material with coal series kaolin rock or flyash, be processed into Silicon-rich solid phase and rich aluminum solutions mutually by acidleach, the Silicon-rich solid phase is molten through alkali, Acid precipitation, acid activation purification, surface modification make modified silicon oxide, and concrete step is as follows:
1) with the oven dry of coal series kaolin rock or flyash, pulverize, dry magnetic separation then 550～850 ℃ of calcinings 1～4 hour down, is that 20～35% acid mixes with mass percent concentration, 100～250 ℃ of following lixiviates 1～4 hour; Filter or centrifugation, with the Silicon-rich solid phase molten generation water glass of alkali, through precipitation, filtration, washing, the dry crude product silicon oxide that gets;
2) be that the acid of 1～3M is 60～90 ℃ of activation 2～3 hours in temperature with step 1) gained crude product silicon oxide concentration, the pH of the hierarchy of control is not higher than 4, filter, and washing, drying promptly gets active oxidation silicon;
3) with step 2) gained active oxidation silicon is that 1: 5～10 ratio is scattered in the organic solvent in solid-to-liquid ratio, add the coupling agent that is equivalent to active oxidation silicon weight 0.5～10% in addition, be warming up to back flow reaction 0.5～2 hour, and filtered, filtration cakes torrefaction then obtains modified silicon oxide.
2. as claimed in claim 1 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described acid is hydrochloric acid, sulfuric acid or nitric acid.
3. as claimed in claim 1 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described organic solvent is methyl alcohol, ethanol, propyl alcohol or Virahol.
4. as claimed in claim 1 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described coupling agent is silane coupling agent, titanate coupling agent or stearic acid coupling agent.
5. as claimed in claim 4 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described silane coupling agent is trimethylethoxysilane, methyltrimethoxy silane, vinyltriethoxysilane, four butoxy silanes or hexamethyldisilazane.
6. as claimed in claim 4 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described titanate coupling agent is the positive butyl ester of metatitanic acid (four) isopropyl ester or metatitanic acid (four).
7. as claimed in claim 4 a kind of be the method for feedstock production modified silicon oxide with coal series kaolin rock or flyash, it is characterized in that described stearic acid coupling agent is stearic acid, iron stearate, calcium stearate or Magnesium Stearate.
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| CN101962188A (en) * | 2010-11-15 | 2011-02-02 | 西藏大为建筑环保工程有限责任公司 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
| CN105698489A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Normal-pressure drying method of glass wool/aluminum silicon aerogel composite heat preserving board |
| CN106925594A (en) * | 2015-12-29 | 2017-07-07 | 中国神华能源股份有限公司 | A kind of processing method of flyash acid dissolution slag |
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| CN101962188A (en) * | 2010-11-15 | 2011-02-02 | 西藏大为建筑环保工程有限责任公司 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
| CN106925594A (en) * | 2015-12-29 | 2017-07-07 | 中国神华能源股份有限公司 | A kind of processing method of flyash acid dissolution slag |
| CN105698489A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Normal-pressure drying method of glass wool/aluminum silicon aerogel composite heat preserving board |
| CN107513283A (en) * | 2017-08-24 | 2017-12-26 | 浙江科屹耐火材料有限公司 | A kind of environment protective fire-proof plate material and preparation method thereof |
| CN107998996A (en) * | 2017-12-06 | 2018-05-08 | 辽宁科技大学 | A kind of preparation method of sial composite aerogel powder |
| CN107998996B (en) * | 2017-12-06 | 2021-05-07 | 辽宁科技大学 | Preparation method of silicon-aluminum composite aerogel powder |
| CN108560312A (en) * | 2018-05-08 | 2018-09-21 | 宝艺新材料股份有限公司 | A kind of novel anti-ultraviolet paint for corrugated board surface |
| CN108927104A (en) * | 2018-08-02 | 2018-12-04 | 深圳市深港产学研环保工程技术股份有限公司 | A kind of preparation method protonating flyash |
| CN109665534A (en) * | 2018-11-22 | 2019-04-23 | 山西大学 | A method of mesopore silicon oxide is prepared using flyash acid leaching residue |
| CN109665534B (en) * | 2018-11-22 | 2022-05-20 | 山西大学 | Method for preparing mesoporous silicon oxide by using fly ash acid leaching residue |
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