CN102887516A - Production method of high-purity quartz sand - Google Patents
Production method of high-purity quartz sand Download PDFInfo
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- CN102887516A CN102887516A CN2012104162538A CN201210416253A CN102887516A CN 102887516 A CN102887516 A CN 102887516A CN 2012104162538 A CN2012104162538 A CN 2012104162538A CN 201210416253 A CN201210416253 A CN 201210416253A CN 102887516 A CN102887516 A CN 102887516A
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Abstract
The invention discloses a production method of high-purity quartz sand, which comprises the following steps of: carrying out secondary roasting, acid washing, flotation, drying and magnetic separation on quartz sand by adding auxiliary materials, and finally carrying out chloridizing roasting to obtain the high-purity quartz sand. According to the production method, the total quantity of impurities of the quartz sand can be controlled to be within 10ppm, the purity reaches above 99.999 percent, a roasting process of a chlorine furnace is increased, the purity is increased to 99.9995 percent, and the actual industrial production of the high-purity quartz sand is realized.
Description
Technical field
The present invention relates to the production technical field of quartz sand, specifically a kind of production method of glass sand.
Background technology
Along with scientific and technical progress, electric light source, electronic industry, optical communication, SiO
2thin-film material, extensive and super large-scale integration, laser, space flight, the especially high-tech industry fast development such as photovoltaic industry and LED lamp of military project, the demand of high grade quartz sand raw material obtains surprising growth, the SiO2 content requirement is greater than 99.99%, and even 99.9999%.Only have traditionally natural one-level crystal can reach this requirement.Yet the mineral crystal resource is increasingly exhausted, and particularly high grade mineral crystal resource is rare especially, and, in distributed pole imbalance all over the world, 95% crystal concentrates on Brazil and Madagascar, makes country in addition all strive to find substitute.Progressively exhausted due to Crystal Resances, from the seventies in last century, various countries start to explore with the ordinary silicon stone ore and replace crystal to prepare glass sand, the current U.S. level that is in a leading position
.the production technology of glass sand is monopolized by a few countries such as the U.S., Germany, Russia.Invent this technique and solved the deficiency that China produces the glass sand technology, met the quality requirements of downstream industry to glass sand.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of glass sand, by the quartz sand secondary is added to auxiliary material roasting and pickling, be controlled at quartz sand product total impurities in 10ppm, and purity reaches more than 99.999%.
The production method of a kind of glass sand of the present invention, its concrete technology step is as follows:
(1) thick broken: the bulk that quartz raw material is broken into to 50 ㎜ * 35 ㎜ sizes;
(2) roughly select: by the significantly impurity foreign matter removal of raw ore surface;
(3) pre-treatment: the ore of choosing is sent into to clear water in stone scrubber and rinse, clean surperficial silt impurity;
(4) calcining: the lump ore after cleaning is sent in calcining furnace and calcined, and setting furnace temperature one district is 880-900 ℃, bis-district 920-950 ℃, calcines discharging in 2 hours;
(5) shrend: the ore that will calcine is released after furnace in the mixing solutions of putting in time the oxalic acid that contains 3% and 3% acetic acid and is carried out shrend dry;
(6) pulverize the sub-sieve magnetic separation: shrend dried ore are sent into to thin jaw crusher in small, broken bits to 5-10 ㎜ globule size, enter Double roll crusher and pulverize thick magnetic separation after the quartz sand that minute is sieved to 60 orders-100 order, 100 orders-200 order granularity specification, remove ferromagnetism impurity and bring into when broken containing iron contaminants;
(7) pickling: through the quartz sand of magnetic separation, putting into pickling machine, the 1.5-2 that adds the quartz sand volume doubly and the purity ultrapure water that is 16-18 million; And then toward adding concentrated hydrochloric acid in pickling machine: nitric acid: the mixing acid that hydrofluoric acid is 6:3:1, the 25-30% that the add-on of mixing acid is the ultrapure water volume, setting and keeping the temperature of pickling machine temperature controller is 80 ℃-90 ℃, open pickling machine, intermittent rotary stirs 90-120 minute, precipitate after 3-5 minute the liquid in pickling machine is discharged, repeatedly add and the ultrapure water of equivalent for the first time, stirring and washing 9-12 time is until the discharging while reaching neutrality of pH value;
(8) drying: quartz sand is put into to whizzer and dewatered and send into roasting sand machine again, controlling drying temperature is the 880-950 degree, drop temperature 300-350 degree, and roasting sand machine continuous rotation discharging, be cooled to normal temperature;
(9) calcining: dried quartz sand is sent into to stirrer, add concentration is 0.2%, weight is quartz sand 1% SODIUMNITRATE and ammonium chloride solution, send into again after stirring in the quartz sand stoving oven and carry out roasting for the second time, setting furnace temperature is 950-980 ℃ of roasting discharging after 2 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(10) repeating step (7) and (8) pickling, drying process, and be cooled to normal temperature;
(11) calcining: again quartz sand is sent into to stirrer, the aluminum nitrate and the ammonium nitrate solution that add concentration to be 0.1%, weight are quartz sand 1%, send into again after stirring in the quartz sand stoving oven and carry out roasting for the third time, setting furnace temperature is 950-980 ℃ of calcining discharging after 2.5 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(12) pickling process of repeating step (7);
(13) flotation: by pickling, good quartz sand adds in flotation machine, by quartz sand and ultrapure water volume ratio, is that 1:3 adds ultrapure water, and the heating slurry temperature is 50~65 ℃; Add oleic acid to stir 5 minutes, with hydrochloric acid, be adjusted to pH value 4-5, stir 5 minutes; Add the palmitinic acid with the kerosene dilution, stir 5 minutes; Adding ammoniacal liquor to regulate slurry pH is 8~9, stirs flotation 30-50 minute; Repeat above whole floating operation once, finally by flotation good quartz sand with ultrapure water clean to pH value be neutral discharging afterwards; Wherein oleic acid and quartz sand mass ratio are 1:3000, and the mass ratio of palmitinic acid and quartz sand is 1:15000;
(14) drying magnetic-separation: by the quartz sand after flotation finally dewater, dry and be cooled to normal temperature and carry out again magnetic separator for the second time;
(15) chloridizing roasting: the quartz sand after magnetic separation is sent into to the chlorine stoving oven, and setting temperature in stove is the 1250-1300 degree, sends into chlorine, and the quartz sand fluidised form is by the continuous roasting of high temperature chlorine discharging, carries out the packing of product after naturally cooling to normal temperature.
Advantage of the present invention is: present method takes full advantage of the vein quartz resource of China's abundant, by the quartz sand secondary is added to auxiliary material roasting and pickling, quartz sand product total impurities is controlled in 10ppm, purity reaches more than 99.999%, increase chlorine stove sinter process, purity is brought up to 99.9995, realized glass sand suitability for industrialized production truly.
Embodiment
The following examples can illustrate in greater detail the present invention, but do not limit in any form the present invention.
Embodiment 1:(1) thick broken: the bulk that quartz raw material is broken into to 50 ㎜ * 35 ㎜ sizes;
(2) roughly select: by the significantly impurity foreign matter removal of raw ore surface;
(3) pre-treatment: the ore of choosing is sent into to clear water in stone scrubber and rinse, clean surperficial silt impurity;
(4) calcining: the lump ore after cleaning is sent in calcining furnace and calcined, and setting furnace temperature one district is 880-900 ℃, bis-district 920-950 ℃, calcines discharging in 2 hours;
(5) shrend: the ore that will calcine is released after furnace in the mixing solutions of putting in time the oxalic acid that contains 3% and 3% acetic acid and is carried out shrend dry;
(6) pulverize the sub-sieve magnetic separation: shrend dried ore are sent into to thin jaw crusher in small, broken bits to 5-10 ㎜ globule size, enter Double roll crusher and pulverize thick magnetic separation after the quartz sand that minute is sieved to 60 orders-100 order, 100 orders-200 order granularity specification, remove ferromagnetism impurity and bring into when broken containing iron contaminants;
(7) pickling: through the quartz sand of magnetic separation, putting into pickling machine, the 1.5-2 that adds the quartz sand volume doubly and the purity ultrapure water that is 16-18 million; And then toward adding concentrated hydrochloric acid in pickling machine: nitric acid: the mixing acid that hydrofluoric acid is 6:3:1, the 25-30% that the add-on of mixing acid is the ultrapure water volume, setting and keeping the temperature of pickling machine temperature controller is 80 ℃-90 ℃, open pickling machine, intermittent rotary stirs 90-120 minute, precipitate after 3-5 minute the liquid in pickling machine is discharged, repeatedly add and the ultrapure water of equivalent for the first time, stirring and washing 9-12 time is until the discharging while reaching neutrality of pH value;
(8) drying: quartz sand is put into to whizzer and dewatered and send into roasting sand machine again, controlling drying temperature is the 880-950 degree, drop temperature 300-350 degree, and roasting sand machine continuous rotation discharging, be cooled to normal temperature;
(9) calcining: dried quartz sand is sent into to stirrer, add concentration is 0.2%, weight is quartz sand 1% SODIUMNITRATE and ammonium chloride solution, send into again after stirring in the quartz sand stoving oven and carry out roasting for the second time, setting furnace temperature is 950-980 ℃ of roasting discharging after 2 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(10) repeating step (7) and (8) pickling, drying process, and be cooled to normal temperature;
(11) calcining: again quartz sand is sent into to stirrer, the aluminum nitrate and the ammonium nitrate solution that add concentration to be 0.1%, weight are quartz sand 1%, send into again after stirring in the quartz sand stoving oven and carry out roasting for the third time, setting furnace temperature is 950-980 ℃ of calcining discharging after 2.5 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(12) pickling process of repeating step (7);
(13) flotation: by pickling, good quartz sand adds in flotation machine, by quartz sand and ultrapure water volume ratio, is that 1:3 adds ultrapure water, and the heating slurry temperature is 50~65 ℃; Add oleic acid to stir 5 minutes, with hydrochloric acid, be adjusted to pH value 4-5, stir 5 minutes; Add the palmitinic acid with the kerosene dilution, stir 5 minutes; Adding ammoniacal liquor to regulate slurry pH is 8~9, stirs flotation 30-50 minute; Repeat above whole floating operation once, finally by flotation good quartz sand with ultrapure water clean to pH value be neutral discharging afterwards; Wherein oleic acid and quartz sand mass ratio are 1:3000, and the mass ratio of palmitinic acid and quartz sand is 1:15000;
(14) drying magnetic-separation: by the quartz sand after flotation finally dewater, dry and be cooled to normal temperature and carry out again magnetic separator for the second time;
(15) chloridizing roasting: the quartz sand after magnetic separation is sent into to the chlorine stoving oven, and setting temperature in stove is the 1250-1300 degree, sends into chlorine, and the quartz sand fluidised form is by the continuous roasting of high temperature chlorine discharging, carries out the packing of product after naturally cooling to normal temperature.
Claims (1)
1. the production method of a glass sand, is characterized in that, the concrete technology step is as follows:
(1) thick broken: the bulk that quartz raw material is broken into to 50 ㎜ * 35 ㎜ sizes;
(2) roughly select: by the significantly impurity foreign matter removal of raw ore surface;
(3) pre-treatment: the ore of choosing is sent into to clear water in stone scrubber and rinse, clean surperficial silt impurity;
(4) calcining: the lump ore after cleaning is sent in calcining furnace and calcined, and setting furnace temperature one district is 880-900 ℃, bis-district 920-950 ℃, calcines discharging in 2 hours;
(5) shrend: the ore that will calcine is released after furnace in the mixing solutions of putting in time the oxalic acid that contains 3% and 3% acetic acid and is carried out shrend dry;
(6) pulverize the sub-sieve magnetic separation: shrend dried ore are sent into to thin jaw crusher in small, broken bits to 5-10 ㎜ globule size, enter Double roll crusher and pulverize thick magnetic separation after the quartz sand that minute is sieved to 60 orders-100 order, 100 orders-200 order granularity specification, remove ferromagnetism impurity and bring into when broken containing iron contaminants;
(7) pickling: through the quartz sand of magnetic separation, putting into pickling machine, the 1.5-2 that adds the quartz sand volume doubly and the purity ultrapure water that is 16-18 million; And then toward adding concentrated hydrochloric acid in pickling machine: nitric acid: the mixing acid that hydrofluoric acid is 6:3:1, the 25-30% that the add-on of mixing acid is the ultrapure water volume, setting and keeping the temperature of pickling machine temperature controller is 80 ℃-90 ℃, open pickling machine, intermittent rotary stirs 90-120 minute, precipitate after 3-5 minute the liquid in pickling machine is discharged, repeatedly add and the ultrapure water of equivalent for the first time, stirring and washing 9-12 time is until the discharging while reaching neutrality of pH value;
(8) drying: quartz sand is put into to whizzer and dewatered and send into roasting sand machine again, controlling drying temperature is the 880-950 degree, drop temperature 300-350 degree, and roasting sand machine continuous rotation discharging, be cooled to normal temperature;
(9) calcining: dried quartz sand is sent into to stirrer, add concentration is 0.2%, weight is quartz sand 1% SODIUMNITRATE and ammonium chloride solution, send into again after stirring in the quartz sand stoving oven and carry out roasting for the second time, setting furnace temperature is 950-980 ℃ of roasting discharging after 2 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(10) repeating step (7) and (8) pickling, drying process, and be cooled to normal temperature;
(11) calcining: again quartz sand is sent into to stirrer, the aluminum nitrate and the ammonium nitrate solution that add concentration to be 0.1%, weight are quartz sand 1%, send into again after stirring in the quartz sand stoving oven and carry out roasting for the third time, setting furnace temperature is 950-980 ℃ of calcining discharging after 2.5 hours, puts in time in the mixing solutions of the oxalic acid that contains 3% and 3% acetic acid and carries out shrend;
(12) pickling process of repeating step (7);
(13) flotation: by pickling, good quartz sand adds in flotation machine, by quartz sand and ultrapure water volume ratio, is that 1:3 adds ultrapure water, and the heating slurry temperature is 50~65 ℃; Add oleic acid to stir 5 minutes, with hydrochloric acid, be adjusted to pH value 4-5, stir 5 minutes; Add the palmitinic acid with the kerosene dilution, stir 5 minutes; Adding ammoniacal liquor to regulate slurry pH is 8~9, stirs flotation 30-50 minute; Repeat above whole floating operation once, finally by flotation good quartz sand with ultrapure water clean to pH value be neutral discharging afterwards; Wherein oleic acid and quartz sand mass ratio are 1:3000, and the mass ratio of palmitinic acid and quartz sand is 1:15000;
(14) drying magnetic-separation: by the quartz sand after flotation finally dewater, dry and be cooled to normal temperature and carry out again magnetic separator for the second time;
(15) chloridizing roasting: the quartz sand after magnetic separation is sent into to the chlorine stoving oven, and setting temperature in stove is the 1250-1300 degree, sends into chlorine, and the quartz sand fluidised form is by the continuous roasting of high temperature chlorine discharging, carries out the packing of product after naturally cooling to normal temperature.
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