CN111620343B - Production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by dry method - Google Patents
Production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by dry method Download PDFInfo
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Abstract
The invention particularly relates to a production process for preparing and recovering functional ultrapure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by a dry method. The invention adopts the neutralizing agent, the flotation agent and the coupling agent to treat the fluorine-containing silicon-containing slag, can fully and comprehensively utilize the fluorine-containing silicon slag tailing resources through twice flotation processes, reduces the dependence on natural silicon ore, has multiple benefits of reducing environmental pollution, obtaining ultrapure functional nano silicon dioxide and relieving fluorite resource pressure, and can recover ultrapure SiO with different meshes 2 No need of special equipment, siO 2 The recovery rate can reach more than 99%.
Description
Technical Field
The invention relates to a method for extracting silicon dioxide from slag, in particular to a production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing and silicon-containing waste slag by a dry method.
Background
Natural silica has a density of 2.65 and a mohs hardness of 7, and is the second most abundant of all elements in the earth, but high quality natural silica is relatively small. Because the silicon ore belongs to non-pillar mineral resources of national economy in China and is also a plurality of non-metal mineral resources with undetermined reserves in China, the reserves in China are mostly predicted estimated numbers or unknown numbers. Displaying according to the related data: the silicon ore reserves in China reach 140 hundred million tons, and the vein quartz reserves with the silicon dioxide content of more than 99 percent are only 5000 million tons. The natural silicon ore is processed into micro powder through a plurality of processes such as mining, crushing, sand making, magnetic separation, flotation, roasting, acid washing, purification, high-purity water treatment and the like, and the micro powder is customarily called as 'sand' with the particle size of 20-200 meshes; those having a particle size of 200 mesh or more are called "fine silica powder".
Internationally, the siliconizing technology leads the united states, japan, germany, and then the united kingdom, france. The Union corporation of Usinmin in the United states called "the world's exclusive manufacture of the highest purity silica sand to replace crystals", and "IOTA silica" was regarded as "international standard purity". The Japanese chemical industry company and the Nissin iron chemical industry company innovate and develop spherical silicon powder with high purity and low radioactive content, the purity reaches 99.99 percent, the spherical silicon powder is used for packaging large-scale and ultra-large scale integrated circuits, and the ultra-pure silicon powder filler accounts for more than 70 percent of the components of the epoxy plastic packaging material in the chip technology. Japan is a world with a large output of epoxy plastic packaging materials, and accounts for about 90 percent of the world. In recent years, the world energy crisis and industry are upgraded and updated, so that the blowout development of the high-purity sand market is caused, the demand is greatly increased, and domestic production enterprises and scientific research institutions are increasing the strength to research silicon purification technology and obtain great progress, but have great difference with the world, and mainly show that three technical bottlenecks, namely purity, ultra-micro radiation and controllable crystal form, cannot be broken through.
At present, the silicon industry material enterprises in China have smaller group scale, and make little progress in respective production, particularly, the process is not wrong in the aspect of maintaining the product purity in the aspect of the production of quartz glass tube drawing materials, but the purification process is still at a lower level compared with the international level, so that the dependence on raw ores is extremely strong. Most purification processes are operated in workshop mode, so that the yield is limited. And the grade is to be improved. At present, 99.9% of enterprises can achieve the aim of no more than several enterprises with the grain size of less than 200 meshes; the purity of the silicon powder with the particle size of more than 200 meshes basically stays below 99.6 percent, the particle size is basically limited below 600 meshes, and the yield of the silicon powder with the particle size of more than 4000 meshes is very low; no enterprise can achieve the silicon micro powder with 8000 meshes to nano level; the purity of the product of the tap of the world ultra-pure silicon micro powder industry, namely the Unimin company in America reaches a level of 99.9992%, and is closer to 99.9994%, and the particle size and the shape are well controlled. The high-purity sand produced by high-purity silica sand enterprises in China aims to replace American Unimin standard silica sand, but at present, the best level can only be similar, the crucible is used as an outer layer and a middle layer of a crucible to replace materials, and the inner layer still uses high-purity sand produced by expensive American Unimin.
In order to reduce the dependence on natural silicon ore and the environmental pollution caused by mining and metallurgical waste ore, the raw materials of the invention are further waste, namely fluorine-containing silicon-containing waste slag, obtained by primarily processing fluorite from waste slag after metallurgical copper smelting, the water content of the fluorine-containing silicon-containing waste slag is about 35 percent, the F-content of the fluorine-containing silicon-containing waste slag is about 6.5 percent, and SiO 2 About 52% and about 6.5% are other impurities. Usually, waste residue is subjected to landfill treatment after transportation, which not only pollutes the environment, but also needs landfill sites to occupy cultivated lands. Over time, landfills are also a source of pollution. In addition, the silicon slag is packaged and transported by ton bags during transportation. The ton bag needs to be scrapped after being used for a plurality of times, so that new environmental pollution is caused. The fluorine-containing and silicon-containing waste slag is easy to scatter during the process of sending the waste slag into the next working procedure, and causes the environmental pollution along the way. The mode has high labor cost, the loading and unloading are finished by a forklift or a traveling crane, an operator needs to hold a special operation certificate, and the packaging cost is high. More importantly, the fluorine-containing and silicon-containing waste slag has strong acidity, the pH value of the waste slag is less than 1 after being detected for several times, and special equipment is required for transportation and storage. HF in the fluorine-containing silicon-containing waste slag has strong corrosivity, can corrode all metals and even acid glass, and can rust attached substances even if a trace amount of HF remains. The waste produced by the invention can be further recycled.
Disclosure of Invention
The invention aims to provide a production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by a dry method. The method can fully and comprehensively utilize the fluorine-containing silicon slag tailing resources, reduces the dependence on natural silicon ore, and has multiple benefits of reducing environmental pollution, obtaining ultra-pure functional nano silicon dioxide and relieving the pressure of fluorite resources.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by a dry method (the flow is shown in figure 1); the method specifically comprises the following steps:
(1) Taking fluorine-containing silicic acid silica slag, adding recycled wastewater and a neutralizing agent, adjusting the pH, and heating and stirring at a constant temperature of 80 ℃ for 2 hours in a batching tank to obtain a batching A with the pH value of 8 to 9;
(2) Taking the ingredient A, stirring and adding a flotation agent at the temperature of 70-80 ℃ until the pH value is 7, filtering, cleaning precipitates with ultrapure water, dehydrating, and drying at 120 ℃ to obtain precipitates A;
(3) Adding KH570 coupling agent at room temperature, further performing flotation, filtration, cleaning and dehydration on the precipitate A, and then drying and cooling;
(4) And obtaining the ultra-pure silicon micro powder with different meshes after supersonic speed crushing and grading, cyclone dust removal or cloth bag dust removal.
Further, the fluorine-containing silicic acid silicon slag comprises the following raw material components in percentage by mass: 35% by weight of water, F - Content 6.5wt%, si 4+ The content is 52wt%, and other impurities are 6.5wt%.
Wherein F - Is H 2 SiF 6 、SiF 4 Or in the presence of HF; si 4+ Is SiO 2 、H 2 SiF 6 Or SiF 4 Are present.
Further, the neutralizing agent in the step (1) is a self-made neutralizing agent, the aim is to adjust the pH value of the waste residue to 7 to 8, and the neutralizing agent consists of alkali liquor, carbonate, a heavy metal catching agent and a stabilizing agent; wherein the heavy metal scavenger is ethyl sulfur nitrogen (C) 2 H 5 ) 2 NCSSNa·3H 2 O), the addition amount of the catalyst accounts for 0.1 to 1.5 wt% of the neutralizer; wherein the stabilizer is organic rare earth, and the addition amount of the stabilizer accounts for 0.1wt% of the neutralizer.
Further, the alkali liquor is 50 to 70wt% of NaOH +30 to 50wt% of NH 4 OH; composition of the carbonate: 5g of Na 2 CO 3 +15g (NH 4 ) 2 CO 3 +15g NH 4 HCO 3 。
Further, the flotation agent in the step (2) is composed of the following raw materials in percentage by mass: 30 to 60 percent of xanthate or xanthate derivative, 30 to 60 percent of oxalic acid, 1 to 3 percent of sodium dodecyl benzene sulfonate, 0.5 to 1 percent of other metal collecting agents, and the sum of the total mass fraction is 100 percent.
Further, in the step (3), the mass ratio of the KH570 coupling agent to the precipitate A is 1.
Further, the step (4) is specifically to obtain 2000-mesh silicon dioxide after supersonic speed crushing and classification; then cyclone dust removal is carried out to obtain 5000-mesh functional silicon dioxide; and collecting the dust generated after cloth bag dust removal through a pipeline dust remover and a trap to synthesize the nanoscale functional ultra-pure silicon micropowder.
The flotation agent has the advantages of high flotation speed, less and fine foam, simple formula and low price. The sediment after flotation can be used for purifying silica sand, and the liquid can further use synthetic fluorite.
The basic principle is as follows:
H 2 SiF 6 →SiF 4 +HF
SiF 4 + H 2 O ↔ SiO 2 + 4HF
HF+OH - →Na + +F - +H 2 O
HF+NH 4 OH→NH 4 + +F - +H 2 O
SiF 4 +Na 2 CO 3 2- →Na + +F - +Si 2 (CO 3 ) 4 ↓
Si 2 (CO 3 ) 4 +CH 3 CCH 2 -OO(CH 2 ) 3 Si(OCH 3 ) 3 →SiO 2 ↓+CO 2 +H 2 O
wherein the selection and operation of the flotation reagent are the most important steps of the flow. The flotation agent which is independently researched and developed by the invention is prepared according to different slag sources, so that the flotation effect is good, the consumption is low, and the pollution is small. And washing with tap water or ultrapure water after flotation.
Further, the drying in the step (3): drying the centrifuged material by high-temperature heating and microwave heating to remove CO 2 And collecting CO 2 。
The invention has the following remarkable advantages:
(1) The invention fully and comprehensively utilizes the fluorine-containing silicon slag tailing resources, lightens the dependence on natural silicon ore, and has multiple benefits of reducing environmental pollution, obtaining ultra-pure functional nano silicon dioxide and relieving the pressure of fluorite resources.
(2) In the process of the invention, the wastewater, the dust and the solid waste are all recycled.
(3) The process can recover ultrapure SiO with different meshes 2 No need of special equipment, siO 2 The recovery rate can reach more than 99%.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 SEM image of the product of example 3.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
In the embodiment, the neutralizing agent is a self-made neutralizing agent, the aim is to adjust the pH value of waste residues to 7 to 8, and the neutralizing agent consists of alkali liquor, carbonate, a heavy metal catching agent and a stabilizing agent; wherein the heavy metal scavenger is ethionamide (C) 2 H 5 ) 2 NCSSNa·3H 2 O), the addition amount of the catalyst accounts for 0.1 to 1.5 wt% of the neutralizer; wherein the stabilizer is organic rare earth, and the addition amount of the stabilizer accounts for 0.1wt% of the neutralizer.
Further, the alkali liquor is 50-70wt% of NaOH + 30-50wt% of NH 4 OH; composition of the carbonate: 5g of Na 2 CO 3 +15g (NH 4 ) 2 CO 3 +15g NH 4 HCO 3 。
The flotation agent in the embodiment consists of the following raw materials in percentage by mass: 30 to 60 percent of xanthate or xanthate derivative, 30 to 60 percent of oxalic acid, 1 to 3 percent of sodium dodecyl benzene sulfonate, 0.5 to 1 percent of other metal collecting agents, and the total mass percentage sum is 100 percent.
Example 1 (product 1)
(1) Taking 100 g of fluorine-containing silicon silicate slag (with the water content of 35 percent), adding 300mL of recycled wastewater, heating in a batching tank at the constant temperature of 80 ℃, adding a neutralizer (with the speed of 100mL per hour), and stirring for 2 hours to obtain a batching A with the pH value of 8-9; .
(2) Taking the ingredient A, stirring and adding a flotation agent at the temperature of 70-80 ℃ until the pH value is 7, filtering, cleaning precipitates with ultrapure water, dehydrating, and drying at 120 ℃ to obtain precipitates A;
(3) Adding a KH570 coupling agent at room temperature, wherein the mass percentage of the coupling agent to the precipitate A is 1;
(4) Passing through air to carry out supersonic speed grinding and classification to obtain 51.63 g of 2000-mesh silicon dioxide, siO 2 The recovery rate can reach more than 99.29 percent, and the content of silicon dioxide is 99.95 percent.
Example 2 (product 2)
(1) Taking 100 g of fluorine-containing silicic acid silica residue (with the water content of 35 percent), adding 300mL of reuse wastewater, heating in a batching tank at the constant temperature of 80 ℃, adding a neutralizing agent (at the speed of 100mL per hour), and stirring for 2 hours to obtain a batching A with the pH value of 8-9; .
(2) Taking the ingredient A, stirring at 70-80 ℃, adding a flotation agent while stirring until the pH value is 7, filtering, cleaning precipitates with ultrapure water, dehydrating, and drying at 120 ℃ to obtain precipitates A;
(3) Adding a KH570 coupling agent at room temperature, wherein the mass percentage of the coupling agent to the precipitate A is 1;
(4) After supersonic speed crushing classification and cyclone dust removal, 51.70 g of silicon dioxide, siO, with 5000 meshes is obtained 2 The recovery rate can reach more than 99.42 percent, and the obtained sample is SiO calculated by elements 2 The purity was 99.9953%.
Example 3 (product 3)
(1) Taking 100 g of fluorine-containing silicic acid silica residue (with the water content of 35%), adding 300mL of reuse wastewater, heating in a batching tank at the constant temperature of 80 ℃, adding a neutralizing agent (at the speed of 100mL per hour), and stirring for 2 hours to obtain a batching A with the pH value of 8-9; .
(2) Taking the ingredient A, stirring and adding a flotation agent at the temperature of 70-80 ℃ until the pH value is 7, filtering, cleaning precipitates with ultrapure water, dehydrating, and drying at 120 ℃ to obtain precipitates A;
(3) Adding a KH570 coupling agent at room temperature, wherein the mass percentage of the coupling agent to the precipitate A is 1;
(4) Collecting the dust generated by air-passing supersonic speed pulverizing and grading, cyclone dust removal and cloth bag dust removal by a pipeline dust collector and a trap to synthesize 51.78 g of nano-scale functional ultra-pure silicon micropowder, siO 2 The recovery rate can reach more than 99.58 percent, and the sample is SiO calculated by elements 2 The purity was 99.9974%.
The treatment of wastewater, dust and solid waste of the invention:
1. waste water
The waste water produced by the invention is mainly used for preparing water for a proportioning tank, ultrapure water, raw material flotation and cleaning water and office water. Water for the batching tank is partially recycled after being precipitated by the precipitation tank, and the rest part is discharged into a factory sewage collection tank for pretreatment; the preparation of ultrapure water, the flotation of raw materials and the water for cleaning are discharged into a factory sewage collection pool for pretreatment (the main process of the sewage collection pool is an adjusting pool, a primary sedimentation pool, a reaction pool, a secondary sedimentation pool and a clean water pool). The sewage is pretreated in a factory and reaches the B-level standard in Table 1 of the Standard for Water quality of Sewage discharged into urban sewer (GB/T31962-2015); domestic sewage generated by the project reaches a third-level standard in Integrated wastewater discharge Standard (GB 8978-1996) after being treated by the oil separation tank and the third-level septic tank.
2. Dust
The fluorite powder is the wet powder output and does not have the raise dust problem. In addition, the purity of a high-end product of the silicon-based new material is more than 99.9 percent, and the product quality is about to be damaged due to slight mixing of environmental dust, so the technical process is totally closed, and all pollution of external dust to the product is refused; the dust generated in the process of the invention is high-purity silicon micropowder with economic priceThe value is very high, most of the technological process adopts wet process operation (the previous steps 1,2 and 3 are all in solution state, and only the 4 th step of air supersonic classification, cyclone dust collection and bag dust collection of the dried substance is carried out in dry state, and the water vapor and CO are removed 2 ) No dust will fly away, and each link generating dust is provided with a dust remover and a collector. The generated dust is collected by a dust remover and a collector through a pipeline to form ultra-pure silicon micro powder which is sold to customers as a high-value product; not only can prevent dust pollution, but also can improve the product benefit. The dust dissipated into the atmosphere is very little and cannot influence the air environment.
3. Solid waste
The solid waste produced by the invention is waste residue produced in the flotation process and precipitate produced in the sewage treatment process, is a high-quality raw material for producing gypsum for cement enterprises, and can be directly sold to gypsum enterprises.
The silicon powder inspection sample developed by the invention has the inspection result that the sample in example 3 is SiO calculated by elements 2 The purity was 99.9974%, and the sample of example 2 was SiO in terms of element 2 The purity was 99.9953%. The product index is close to the index of the Unimine company.
The following table specifically shows:
concrete inspection index table (Unit: PPm)
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. A production process for preparing and recovering functional ultra-pure nano silicon dioxide from low-grade fluorine-containing silicon-containing waste slag by a dry method is characterized by comprising the following steps of: the method specifically comprises the following steps:
(1) Adding the recycled wastewater and a neutralizing agent into the fluorine-containing silicon silicate slag, adjusting the pH, and heating and stirring the mixture for 2 hours at a constant temperature of 80 ℃ in a batching tank to obtain a batching A with the pH value of 8-9;
(2) Taking the ingredient A, stirring and adding a flotation agent at the temperature of 70-80 ℃ until the pH value is 7, filtering, cleaning precipitates with ultrapure water, dehydrating, and drying at 120 ℃ to obtain precipitates A;
(3) Adding a KH570 coupling agent at room temperature, further performing flotation, filtration, cleaning and dehydration on the precipitate A, and then drying and cooling;
(4) Obtaining ultra-pure silicon micro powder with different mesh numbers after supersonic speed crushing and grading, cyclone dust removal or cloth bag dust removal;
the neutralizing agent in the step (1) is a self-made neutralizing agent, the purpose is to adjust the pH value of the waste residue to 7 to 8, and the neutralizing agent consists of alkali liquor, carbonate, a heavy metal catching agent and a stabilizing agent; wherein the heavy metal scavenger is ethyl sulfur nitrogen (C) 2 H 5 ) 2 NCSSNa·3H 2 O, the addition amount of which accounts for 0.1 to 1.5 wt percent of the neutralizer; wherein the stabilizer is a rare earth citric acid complex, and the addition amount of the stabilizer accounts for 0.1wt% of the neutralizer;
wherein the alkali liquor is 50 to 70wt% of NaOH +30 to 50wt% of NH 4 OH; composition of the carbonate: 5g of Na 2 CO 3 +15g (NH 4 ) 2 CO 3 +15g NH 4 HCO 3 ；
The flotation agent in the step (2) is composed of the following raw materials in percentage by mass: 30 to 60 percent of xanthate or xanthate derivative, 30 to 60 percent of oxalic acid, 1 to 3 percent of sodium dodecyl benzene sulfonate, 0.5 to 1 percent of other metal collecting agents, and the total mass percentage sum is 100 percent;
and (3) the mass ratio of the KH570 coupling agent to the precipitate A is 1 to 8-1.
2. The production process for preparing and recovering functional ultra-pure nano silicon dioxide by using the low-grade fluorine-containing silicon-containing waste slag through the dry method according to claim 1, which is characterized in that: the fluorine-containing silicic acid silica slag comprises the following raw material components in percentage by mass: 35% by weight of water, F - Content 6.5wt%, si 4+ The content is 52wt%, and other impurities are 6.5wt%.
3. The dry preparation and recovery function of the low-grade waste slag containing fluorine and silicon according to claim 2The production process of ultrapure nanometer silicon dioxide is characterized by comprising the following steps: wherein F - Is H 2 SiF 6 、SiF 4 Or in the presence of HF; si 4+ Is SiO 2 、H 2 SiF 6 Or SiF 4 Are present.
4. The production process for preparing and recovering functional ultra-pure nano silicon dioxide by using the low-grade waste slag containing fluorine and silicon according to the claim 1 by the dry method is characterized by comprising the following steps: the step (4) is to obtain 2000-mesh silicon dioxide after supersonic speed crushing and grading; then cyclone dust removal is carried out to obtain 5000-mesh functional silicon dioxide;
and collecting the dust generated after cloth bag dust removal through a pipeline dust remover and a trap to synthesize the nanoscale functional ultra-pure silicon micropowder.
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