CN102602942B - Method for preparing high-purity quartz sand - Google Patents
Method for preparing high-purity quartz sand Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity quartz sands, belongs to the technical field of efficiently preparing quartz sands and relates to a method for preparing high purity quartz sands by using natural and common silica. Aiming at different mineral resources, the method selects reasonable preparation conditions, breaks various impurity inclosures and changes the crystalline form of silica, in particular improves the water quenching process during preparation of high-purity quartz sands and obtains the high-purity quartz sands with the total quantity of impurities controlled within 10ppm and the purity greater than 99.998%. According to the invention, as the method is adopted, the deficiencies of high cost and environmental pollution by using strong acids, such as sulfuric acid, hydrochloric acid, nitric acid or hydrofluoric acid and the like in the prior art are avoided; and the water quenching solution of ammonium nitrate and ammonium acetate has the advantages of low cost, easily accessibility and no pollution on environment.
Description
Technical field
The invention belongs to the efficient preparing technical field of quartz sand, relate to a kind of method for preparing glass sand, especially a kind of method for preparing glass sand that is applicable to adopt natural common silica.
Background technology
As everyone knows, quartzy as a kind of important industrial raw material, extensive application in a lot of fields, as glass, plastics, rubber, paint etc.A lot of high-technology fields need glass sand to make raw material, and glass sand generally refers to SiO2, and content, higher than 99.99% silica powder, has fabulous chemical stability, high dielectric voltage withstand ability and extremely low volume coefficient.Be the indispensable important raw and processed materials of new high-tech industry such as electronics core devices, optical communications material, solar cell, its expensive goods is widely used in the industries such as large-scale integrated circuit, solar cell, optical fiber, laser, space flight, military affairs.As electronic material, optical-fibre communications, SiO2 thin-film material etc.In above-mentioned industry, the content of the purity of quartz sand and impurity element directly affects the quality of prepared product.
All select mineral crystal to make raw material at present, both at home and abroad, through pulverizing, classification, purification, make standard compliant quartz sand.The level for preparing glass sand as Unimin Corp. (US) of the U.S. is higher, and its foreign matter content is in 20ppm, but its complex process, and cost is very expensive.At present the preparation technology of conventional quartz sand is: roughly select → fragmentation → roasting → water is broken → and pulverizing → deironing → operations such as acid soak → flotation, finally make 80～100 purpose products.This production and purifying technique are simpler, can not effectively remove some impurity that exist in quartzy parcel impurity, surface impurity and production process, make purity not high, the boron that particularly inside has a significant impact polysilicon and phosphorus etc., and removal effect is poorer.In prior art, as application number is that 200710132668.1 publication numbers are CN101391871, denomination of invention is " a kind of method for preparing glass sand ", be about to dried quartz sand in sulfuric acid, hydrochloric acid, nitric acid or the hydrofluoric acid of (concentration of acid is 5%～20%) of high density by acid leaching process, under the condition of higher temperature (30～100 ℃), remove trace metal and nonmetallic impurity in the quartz sand fine powder, use the high-intensity acid such as sulfuric acid, hydrochloric acid, nitric acid or hydrofluoric acid, not only increased cost, also environment has been caused to huge pollution.Application number is that 201010284139.5 publication numbers are that the CN101948235A denomination of invention is also so for " method for preparing glass sand ", has used concentrated hydrochloric acid or hydrochloric acid and hydrofluoric acid.
There is lack of raw materials for mineral crystal, and expensive.Progressively exhaustion along with Crystal Resances, from the seventies in last century, various countries start exploration and replace crystal to prepare glass sand with the ordinary silicon stone ore, at present U.S.'s level that is in a leading position, be characterized in that industrialization output is large, preparation is specialized, level of automation is high, detection level is high, the existing glass sand of constant product quality is monopolized by a few countries such as the U.S., Germany, Russia.Thereby, utilize natural ordinary silicon masonry raw material, substitute crystal high purity quartz sand and there is realistic meaning.But, because of the difference of geologic media, the quality of each department silica also is not quite similar, silica is when crystalline growth, and the various reasons owing to becoming ore deposit, can cause defect and the hole of crystal structure, thereby can form the impurity inclusion of all size volume.Domestic in China, the existing a kind of method that does not also have content that can from silica mine, prepare silicon-dioxide to be greater than 99.99% glass sand.Therefore in the urgent need to developing the method for the natural ordinary silicon glass sand for high purity, low impurity content made of stones.
Summary of the invention
The present invention is in order to solve above-mentioned the deficiencies in the prior art, a kind of method for preparing glass sand is proposed, for different mineral resources, select rational preparation condition, crack various impurity inclusions and change the silica crystalline form, especially improved preparing water quenching technology in the glass sand process, then obtain total impurities and be controlled in 10ppm, the glass sand that purity is greater than 99.998%.
A kind of method for preparing glass sand; According to following step, carry out:
(1) roughly select: the obvious impurity in all kinds of silica raw materials and foreign matter are removed,
(2) roasting: pour the silica silica granule into the roasting kiln roasting 4 hours,
(3) shrend:
The silica that roasting is rubescent is released with kick-off arm, and putting into mass concentration is shrend 3-5min in 1%-5% ammonium chloride or aqueous ammonium nitrate solution; , silica is taken out and pours drainage in the grid case in time, after drying, enter between crushing vehicle;
(4) crushing and classification:
By roasting shrend dried silica, be crushed to the 8-10mm globule size through jaw crusher, enter the quartzy sand grains that pair roller mill is crushed to 0.04-0.1mm; Pulverized material is divided into a plurality of granularity specifications such as 20 orders are above, 20 orders-50 order, 50 orders-100 order, 100 orders-160 order, 160 orders-200 order, and through thick magnetic separation, it is standby that packing is transported to the flotation workshop after weighing;
(5) flotation:
At first dropping into silica powder that magnetic separation is good to flotation machine, is 1: 3 by silica powder and deionized water volume ratio, and the heating slurry temperature is 70～85 ℃; The mixed solution that adds ammoniacal liquor and ore pulp collecting agent, adjust ore pulp ph value to 8～9; After stirring 10min, then add isooctyl alcohol flotation 30min; The silica powder that flotation is good is extremely neutral with ethanol and washed with de-ionized water;
(6) washed with de-ionized water:
By flotation, good quartz sand is put in cleaning machine and is cleaned 4-5 time, control sand volume of water ratio=1: 3, and wash temperature is the 70-80 degree, each washing time is 1-1.5h, when the ionic concn of washing water outlet reaches the control index, cleans complete after testing;
(7) roasting sand drying:
By cleaning qualified quartz sand, enter continuously in roasting sand machine, controlling drying temperature is the 980-1100 degree, drop temperature 200-250 degree, mass flow 200kg/h; Quartz sand is cooling through secondary, enters secondary magnetic separation and finished product packing after reaching normal temperature.
The obvious impurity in all kinds of silica raw materials and foreign matter are removed described in step (1) wherein, refer at first silica is arranged and divides the bulk of electing size 30mm*30mm size as, according to transparent, translucent and White-opalescent, be divided into successively for one-level, secondary, three grades, select foreign matter content more be waste product; The ore of choosing is put into to the grid case, then insert clear water immersion high pressure water washing in service sink, the independent removal of impurities of needs that surperficial matter is many; Cleaning is rinsed well, with surperficial visual inspection, without obvious impurity, is as the criterion, and drainage is treated the subsequent processing processing.
Wherein roasting described in step (2) refers to the silica of clean drying is poured in the stoving oven feed hopper, the stoving oven furnace temperature is set to 860 ℃, 2nd district, one 900 ℃, district, starting lift when furnace temperature reaches set(ting)value pours silica in stove into, set the process furnace rotational time, rotating distance and push rod discharging time and inlet amount, feed space interval, during discharging, so that the silica roasting is rubescent, be as the criterion.
The shrend solution described in step (3) wherein, the ammonium nitrate that preferred mass concentration is 2% and ammonium acetate compound aqueous solution, in compound aqueous solution, the mass ratio of ammonium chloride and ammonium nitrate is 1: 1, the shrend time is 5min.
The add-on that is wherein 0.5: 100 according to the mass ratio according to ammoniacal liquor and silica powder in step (5), add ammoniacal liquor, regulates slurry pH; The add-on that is 1: 100 according to the mass ratio of ore pulp collecting agent and silica powder, add and adjust the ore pulp collecting agent; The middle kerosene of ore pulp collecting agent: oleic acid: plam oil=2: 1: 1 (mass ratio); Mass ratio according to isooctyl alcohol and silica powder is that 1.5: 100 add-ons add isooctyl alcohol to carry out floating operation.Beneficial effect of the present invention: it is mainly by product purity and deviating from the method for impurity element that the present invention is compared with the prior art; In water quenching technology, pass through to select rational shrend solution, and the shrend operational condition such as double salt kind and concentration and shrend time in shrend solution, finally can make the total impurities of quartz sand be controlled in 10ppm, content is greater than 99.998%.The cost of having avoided using in the prior art strong acid such as sulfuric acid, hydrochloric acid, nitric acid or hydrofluoric acid to exist is high, the deficiency of contaminate environment; The shrend solution of ammonium nitrate and ammonium acetate has advantages of that cost is low, is easy to get, environmentally safe.
Embodiment
Embodiment
A kind of each embodiment for preparing the method for glass sand of the present invention; According to following step, carry out:
(1) roughly select: the obvious impurity in all kinds of silica raw materials and foreign matter are removed; At first silica is arranged to the bulk of minute electing size 30mm * 30mm size as, transparent and translucent and White-opalescent is followed successively by one-level, secondary, three grades, select foreign matter content more be waste product; The ore of choosing is put into to the grid case, then insert clear water immersion high pressure water washing in service sink, the independent removal of impurities of needs that surperficial matter is many; Cleaning is rinsed well, with surperficial visual inspection, without obvious impurity, is as the criterion, and drainage is treated the subsequent processing processing.
(2) roasting: by the roasting 4 hours under the condition of 850-900 ℃ of silica silica granule;
Because of the difference of geologic media, the quality of each department silica also is not quite similar, and silica is when crystalline growth, and the various reasons owing to becoming ore deposit, can cause defect and the hole of crystal structure, thereby can form the impurity inclusion of all size volume.So, for different mineral resources, select rational roasting condition, be the effective way that cracks various impurity inclusions and change the silica crystalline form, it goes deimpurity impact very large on the shrend operation.Through large batch of production pilot scale and various analysis contrast, for the East Sea silica roasting condition that we establish at present: maturing temperature 850-900 ℃; Roasting time 4h, both solved quartz sand crystalline form transfer problem, more solved impurity inclusion and crack problem, for the impurity that the shrend operational orientation is removed in quartz sand has been set up basis.
The concrete operations condition is: clean dry silica is poured in the stoving oven feed hopper, the stoving oven furnace temperature is set to 860 ℃, 2nd district, one 900 ℃, district, starting lift when furnace temperature reaches set(ting)value pours silica in stove into, set the process furnace rotational time, rotating distance and push rod discharging time and inlet amount, feed space interval, during discharging, so that the silica roasting is rubescent, be as the criterion.
(3) shrend: the silica that roasting is rubescent is released with discharging rod, in the compound aqueous solution that directly to put into mass concentration be 2%-5% ammonium chloride and ammonium nitrate, and shrend 3-5min; After, silica is taken out and pours drainage in the grid case in time, after drying, enter between crushing vehicle.
The impurity comparative analysis of testing by shrend, the variation of single salt concn and choose reasonable composite salt, removal that can be directed or reduce the content's index of a certain class impurity element, used the effect of composite salt to be greater than the effect of single salt; When the concentration of salt is selected to be greater than 5%, the content's index of removing or reduce impurity element is not had to too large variation.The variation of shrend time in single salts solution, to the content's index of impurity element reduce change little, and in composite salt solution suitable prolongation shrend time or control the shrend time, the content's index of impurity element is reduced and alters a great deal.
In the production process of glass sand, in the situation that other controlling of production process are constant, the shrend operational conditions such as the double salt that we are 2% ammonium nitrate and ammonium acetate by selection concentration and 5 minutes shrend time, finally can make the total impurities of quartz sand be controlled in 10ppm, content is greater than 99.998%.Detailed results is in Table 1-13.
(4) crushing and classification:
By roasting shrend and dried silica, be crushed to the 8-10mm globule size through jaw crusher, enter the sand grains (quartz sand) that pair roller mill is crushed to 0.04-0.1mm.Pulverized material is divided into a plurality of granularity specifications such as 20 orders are above, 20 orders-50 order, 50 orders-100 order, 100 orders-160 order, 160 orders-200 order, and through thick magnetic separation, it is standby that packing is transported to the chlorination workshop after weighing.
(5) flotation:
At first drop into silica powder that the 350kg magnetic separation is good to flotation machine, add again ionized water 900-1000L, controlling volume ratio is 1: 3, the heating ore pulp when temperature when reaching 70～85 ℃, add ammoniacal liquor 1.75kg and 3.5kg ore pulp collecting agent mixture (kerosene that the ore pulp collecting agent is 2: 1: 1 by mass ratio: oleic acid: plam oil forms), adjust slurry pH to 8～9; After stirring 10min, then add isooctyl alcohol 5.25kg flotation 30min; , finally by flotation, good silica powder uses ethanol and washed with de-ionized water to neutral.(6) washed with de-ionized water:
By flotation, good neutral quartz sand is put in cleaning machine and is continued to clean 4-5 time, control sand volume of water ratio=1: 3, wash temperature is the 70-80 degree, each washing time is 1-1.5h, when the ionic concn of washing water outlet reaches the control index, clean complete after testing.
(7) roasting sand drying:
By cleaning qualified quartz sand, enter continuously in roasting sand machine, controlling drying temperature is the 980-1100 degree, drop temperature 200-250 degree, mass flow 200kg/h; Quartz sand is cooling through secondary, enters secondary magnetic separation and finished product packing after reaching normal temperature.
Shrend solution composition and concentration (mass concentration) in the different embodiment of table 1
Experiment 1: test shrend solution and the concentration comparative analysis to the removal effect of impurity element in product before and after shrend in different embodiment
Test conditions: go-on-go material 300kg order is counted 80-160 shrend liquor capacity 1m
23 minutes shrend time
Analyze foundation: JY-T015-1996 " inductively coupled plasma atomic emission spectrum method general rule "
Table 2 utilizes the comparative analysis of deionized water shrend impurity element
The comparative analysis of the single salts solution shrend of table 3 1% impurity element
Single salt is chosen as: ammonium chloride
The comparative analysis of the single salts solution shrend of table 4 2% impurity element
Single salt is chosen as: ammonium nitrate
The comparative analysis of the single salts solution shrend of table 5 5% impurity element
Single salt is chosen as: ammonium chloride
The comparative analysis of table 6 2% complex salt solution shrend impurity element
Composite salt is chosen as: ammonium nitrate: ammonium acetate=1: 1
The comparative analysis of table 7 5% complex salt solution shrend impurity element
Composite salt is chosen as: ammonium nitrate: ammonium acetate=1: 1
By above-mentioned test, can find out, from the impurity element comparative analysis, the variation of single salt concn and choose reasonable composite salt, removal that can be directed or reduce the content's index of a certain class impurity element, used the effect of composite salt to be greater than the effect of single salt; When the concentration of salt is selected to be greater than 5%, the content's index of removing or reduce impurity element is not had to large variation.
The shrend time in the different embodiment of table 8
| Example number | The shrend time | The analytical results of impurity element in product before and after shrend |
| Embodiment 6 | 2% single salts solution shrend 3 minutes | In Table 9 |
| Embodiment 7 | 2% single salts solution shrend 5 minutes | In Table 10 |
| Embodiment 8 | 2% complex salt solution shrend 3 minutes | In Table 11 |
| Embodiment 9 | 2% complex salt solution shrend 5 minutes | In Table 12 |
Experiment 2: the contrast of test implementation different shrend time of example to the removal effect of impurity element in product before and after shrend
Analyze
Operational condition: go-on-go material 300kg order is counted 80-160 shrend liquor capacity 1m
2
Analyze foundation: JY-T015-1996 " inductively coupled plasma atomic emission spectrum method general rule "
The comparative analysis of 3 minutes impurity elements of the single salts solution shrend of table 9 2%
Single salt is chosen as: ammonium nitrate
The comparative analysis of 5 minutes impurity elements of the single salts solution shrend of table 10 2%
Single salt is chosen as: ammonium chloride
The comparative analysis of 3 minutes impurity elements of table 11 2% complex salt solution shrend
Composite salt is chosen as: ammonium nitrate: ammonium acetate=1:1
The comparative analysis of 5 minutes impurity elements of table 12 2% complex salt solution shrend
Composite salt is chosen as: ammonium nitrate: ammonium acetate=1: 1
Comparative analysis by above-mentioned impurity element, the variation of shrend time in single salts solution, to the content's index of impurity element reduce change little, and in composite salt solution suitable prolongation shrend time or control the shrend time, the content's index of impurity element is reduced and alters a great deal.
In the production process of glass sand, in the situation that other controlling of production process are constant, the shrend operational conditions such as the double salt that we are 2% ammonium nitrate and ammonium acetate by selection concentration and 5 minutes shrend time, finally can make the total impurities of quartz sand be controlled in 10ppm, content is greater than 99.998%.
Check analysis the results are shown in Table 13.
Analyze foundation: JY-T015-1996 " inductively coupled plasma atomic emission spectrum method general rule "
The comparative analysis of the impurity element of quartz sand in table 13 the finished product
Claims (4)
1. a method for preparing glass sand; It is characterized in that carrying out according to following step:
(1) roughly select: the obvious impurity in all kinds of silica raw materials and foreign matter are removed,
(2) roasting: pour silica granule into the roasting kiln roasting 4 hours,
(3) shrend:
The silica that roasting is rubescent is released with kick-off arm, and putting into mass concentration is shrend 3-5min in 1%-5% ammonium chloride or aqueous ammonium nitrate solution; Silica is taken out and pours drainage in the grid case in time, enter after drying between crushing vehicle;
(4) crushing and classification:
By roasting shrend dried silica, be crushed to the 8-10mm globule size through jaw crusher, enter the quartzy sand grains that pair roller mill is crushed to 0.04-0.1mm; Pulverized material is divided into that 20 orders are above, 20 orders-50 order, 50 orders-100 order, 100 orders-160 order, a plurality of granularity specifications of 160 orders-200 order, and through thick magnetic separation, it is standby that packing is transported to the flotation workshop after weighing;
(5) flotation:
At first dropping into silica powder that magnetic separation is good to flotation machine, is 1:3 by silica powder and deionized water volume ratio, and the heating slurry temperature is 70～85 ℃; The mixed solution that adds ammoniacal liquor and ore pulp collecting agent, ore pulp is adjusted pH value to 8～9; After stirring 10min, then add isooctyl alcohol flotation 30--60min; Finally by flotation, good silica powder uses ethanol and washed with de-ionized water to neutral;
(6) washed with de-ionized water:
By flotation, good quartz sand is put in cleaning machine and is cleaned 4-5 time, controls sand volume of water ratio=1:3, and wash temperature is the 70-80 degree, and each washing time is 1-1.5h, when the ionic concn of washing water outlet reaches the control index, cleans complete after testing;
(7) roasting sand drying:
By cleaning qualified quartz sand, enter continuously in roasting sand machine, controlling drying temperature is the 980-1100 degree, drop temperature 200-250 degree, mass flow 200kg/h; Quartz sand is cooling through secondary, enters secondary magnetic separation and finished product packing after reaching normal temperature.
2. a kind of method for preparing glass sand according to claim 1; It is characterized in that wherein the obvious impurity in all kinds of silica raw materials and foreign matter are removed described in step (1), refer at first silica is arranged and divides the bulk of electing size 30mm*30mm size as, according to transparent, translucent and White-opalescent, be divided into successively for one-level, secondary, three grades, select foreign matter content more be waste product; The ore of choosing is put into to the grid case, then insert clear water immersion high pressure water washing in service sink, the independent removal of impurities of needs that surperficial matter is many; Cleaning is rinsed well, with surperficial visual inspection, without obvious impurity, is as the criterion, and drainage is treated the subsequent processing processing.
3. a kind of method for preparing glass sand according to claim 1; It is characterized in that wherein roasting described in step (2) refers to pours the silica of clean drying in the stoving oven feed hopper into, the stoving oven furnace temperature is set to 860 ℃, 2nd district, one 900 ℃, district, starting lift when furnace temperature reaches set(ting)value pours silica in stove into, set the process furnace rotational time, rotating distance and push rod discharging time and inlet amount, feed space interval, during discharging, so that the silica roasting is rubescent, be as the criterion.
4. a kind of method for preparing glass sand according to claim 1; It is characterized in that in step (5) wherein that the add-on that the mass ratio according to ammoniacal liquor and silica powder is 0.5:100 adds ammoniacal liquor, regulates slurry pH; The add-on that is 1:100 according to the mass ratio of ore pulp collecting agent and silica powder, add and adjust the ore pulp collecting agent; The middle kerosene of ore pulp collecting agent: oleic acid: plam oil is 2:1:1 by quality ratio; Mass ratio according to isooctyl alcohol and silica powder is that the 1.5:100 add-on adds isooctyl alcohol to carry out floating operation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102897993A (en) * | 2012-10-25 | 2013-01-30 | 中国地质大学（北京） | Method for preparing high-purity quartz sands by using natural vein quartz ores |
| CN102887516B (en) * | 2012-10-26 | 2014-04-02 | 蔡雅纯 | Production method of high-purity quartz sand |
| CN103113014B (en) * | 2013-03-18 | 2015-07-08 | 连云港华源石英制品有限公司 | Sand baking device for quartz sand |
| CN104098101B (en) * | 2013-04-15 | 2015-11-11 | 沭阳县浩源石英制品厂 | Glass sand production technique |
| CN103449455B (en) * | 2013-08-30 | 2015-04-29 | 连云港市弘扬石英制品有限公司 | Method for producing high-quality quartz sand by taking low-grade quartz mines as raw materials |
| CN103964444B (en) * | 2014-05-05 | 2016-08-24 | 临沂晟泉矿业有限公司 | A kind of production method of glass sand |
| CN106186667B (en) * | 2014-06-14 | 2019-12-31 | 东莞东阳光科研发有限公司 | Method for removing impurities in high-purity quartz sand |
| CN104402276A (en) * | 2014-09-30 | 2015-03-11 | 仁新实业发展（信阳）有限公司 | Preparation technology of quartz sand used for synthetic quartzite |
| CN104817265A (en) * | 2015-05-09 | 2015-08-05 | 蚌埠玻璃工业设计研究院 | Method of producing super-white sand through marine-deposition-type natural quartz sand narrow granular class sorting |
| CN105271247B (en) * | 2015-10-09 | 2017-08-01 | 本益新材料股份公司 | High-performance quartz sand and preparation method thereof |
| CN105668574B (en) * | 2015-12-02 | 2018-06-12 | 南京中燊硅基新材料科技有限公司 | A kind of high-purity communicate-type porous oxide raw powder's production technology |
| CN107661810A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of method that arkose quartzite prepares glass sand |
| CN110092384A (en) * | 2019-04-16 | 2019-08-06 | 开鲁县昌达矽砂有限公司 | A kind of production method of natural high-purity quartz sand |
| CN110817886A (en) * | 2019-12-02 | 2020-02-21 | 凯盛石英材料（太湖）有限公司 | Quartz sand flotation and pesticide removal method |
| CN111874913B (en) * | 2020-07-24 | 2022-11-01 | 武汉理工大学 | Method for purifying quartz by chloridizing roasting |
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