CN102320602A - Purifying method of green silicon-carbide micropowder - Google Patents
Purifying method of green silicon-carbide micropowder Download PDFInfo
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- CN102320602A CN102320602A CN201110237784A CN201110237784A CN102320602A CN 102320602 A CN102320602 A CN 102320602A CN 201110237784 A CN201110237784 A CN 201110237784A CN 201110237784 A CN201110237784 A CN 201110237784A CN 102320602 A CN102320602 A CN 102320602A
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Abstract
The invention relates to a purifying method of green silicon-carbide micropowder, which belongs to the technical field of chemistry and comprises the following processing steps of: washing with water, washing with alkali, dipping with dilute acid, adjusting the acidity, dipping with severe acid, then adjusting the acidity, stirring, washing to be neutral, discharging, drying through grading and the like, wherein free carbon and graphite are removed through a water-washing step, free silicon and silicon dioxide on the surfaces of micropowder granules are removed through alkali washing, partial alumina can also be removed, metallic iron and iron oxide are removed through acid washing, and impurities, such as partial calcium oxide, magnesia, alumina and the like can also be removed. Finally, the purity of the green silicon-carbide micropowder reaches more than 99.9 percent.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind ofly produce that green silicon carbide powder is washed, the method for purification of alkali cleaning, pickling impurity removal.
Background technology
The high purity green silicon carbide powder is mainly used in solar energy grade opto-electronic conversion, thyrite, carborundum crystals information material, silit sealing member; Because it is stable to have hardness height, high temperature resistant, high thermal conductance, chemical property, is widely used in key areas such as national defence, Aeronautics and Astronautics, electronics, petroleum prospecting, optical storage.
Green silicon carbide is in smelting process; Because the influence of starting material content and Technology implementation effect; Can bring a certain amount of impurity into, secondly silit is unavoidably sneaked into impurity in the pulverizing and the course of processing, improve technologies such as silit SiC (purity) must wash, alkali cleaning, pickling.Washing process can be removed F.C and graphite; The purpose of alkali cleaning can be removed free silica, the silicon-dioxide on micro powder granule surface; The purpose that also can remove partial oxidation aluminium, pickling is to remove metallic iron and red stone, also can remove impurity such as a part of quicklime, Natural manganese dioxide, aluminum oxide.
Summary of the invention
The objective of the invention is the problem of unavoidably sneaking into impurity in the above-mentioned technological process, and it is high to have proposed a kind of green silicon carbide powder purification concentration, the green silicon carbide powder SiC method of purification that impurity is few in order to solve.
To above-mentioned technical problem, the green silicon carbide powder method of purification of the present invention's design comprises the steps:
(1) washing
Put into the slip that has stirred in the purification container, press pulp density and add 0.35kg trapping agent and 0.4kg silicate dispersant, add pressurized air again, uncombined carbon is floated in the slip foaming, take away uncombined carbon through rotary water current;
(2) alkali cleaning
Put into the slip of washing in the alkali cleaning container, by material: water: the mass ratio of NaOH piece=1: 5: 0.015, heat 70 ℃～80 ℃ through steam, insulated and stirred 4 hours is carried out batch cleaning then, should leave standstill 4 hours after changing water at every turn, is washed till neutrality again;
(3) pickling
Render to the slip that alkali cleaning is intact in the washing tank, add content 98% sulfuric acid, make the sulfuric acid concentration in the washing lotion keep 10%, through steam heating to 2 hour～2.5 hours; Water temperature remains on 70 ℃～80 ℃, carries out stirring and washing then 5～6 times, changes water static 4 hours at every turn, is washed till neutrality; PH value reaches 6～7, adds the hydrofluoric acid 15kg～20kg of concentration 40% again and heats, and begins to stir; Temperature reaches 70 ℃～80 ℃, is incubated 2 hours, adds water rinse 5～6 times; Leave standstill 4 hour after changing water at every turn, make in the material pH value reach neutral discharging water, pH value reaches 6～7;
(4) classification
Washed slip is pumped into weir tank, and after the adding dispersion agent disperseed on inspection, when pushing up slurry level to overflow weir 20cm with big flow, the adjustment flow utilized the buoyancy of water classification to go out the finished product material, and oven dry is until end.
About the oven dry in the described classification step 4, can adopt the hotblast stove oven dry, 150 ℃～180 ℃ of bake out temperatures, 8 hours time.In the described acid pickling step 3, on the basis of pickling, can adjust the excessive acidity pickling again: adding hydrofluoric acid 10kg in proportion, to add concentration be 86% nitric acid 15kg, adds sulfuric acid 30kg; Stir after 8 hours; Left standstill 6～8 hours, and added water rinse, make slip reach neutral.Described adjust acidity again after, just can carry out the severe pickling after the pickling for the second time, add concentrated hydrochloric acid 20kg and nitric acid 15kg, stir acidleach after 8 hours, left standstill 6 hours, add the ionized water agitator treating, repeats 6 times, rinsing is neutrality extremely.Water in the described classification step makes electrical conductivity of water reduce to 87us/cm by 256us/cm through outside normal purification, softening, and total hardness is reduced to 24.1mg/l by 37.2mg/l.
Beneficial effect: embathe through the washing in the above-mentioned technical scheme, alkali cleaning, diluted acid, adjustment acidity, the severe acidleach is washed; Adjust procedure of processings such as acidity agitator treating to neutrality, blowing, classification oven dry again; Removed F.C (uncombined carbon) and graphite through water-washing step, removed free silica, the silicon-dioxide on micro powder granule surface, also can remove partially oxidation aluminium through alkali cleaning; Remove metallic iron and red stone through pickling, also can remove impurity such as a part of quicklime, Natural manganese dioxide, aluminum oxide.The purity of green silicon carbide powder is reached more than 99.9%.
Description of drawings
Below in conjunction with description of drawings and embodiment the present invention is further specified.
Fig. 1 is a process flow sheet of the present invention
Embodiment
Embodiment 1
Acidity is embathed, adjusted to this method mainly through washing, alkali cleaning, diluted acid, and excessive pickling is adjusted acidity again and may further comprise the steps to filtration washing, dehydration, oven dry between the pH value 6～7:
1, washing: in the silicon carbide micro-powder section slip input purification container that has stirred; Press pulp density and add 0.35kg trapping agent and 0.4kg silicate dispersant; Trapping agent can comprise pine camphor oil; Add pressurized air again, uncombined carbon is floated in the slip foaming, take uncombined carbon out of through rotary water current.
2, alkali cleaning: put into the slip of having arranged carbon in the alkali cleaning container; By material: water: NaOH=1: 5: 0.015 (mass ratio) was through steam heating to 70 ℃～80 ℃ insulated and stirred 4 hours; Carry out batch cleaning then, change water at every turn and left standstill 4 hours, wash neutrality.
3, pickling:
(1) diluted acid embathes: put into the intact slip of alkali cleaning and add content 98% sulfuric acid in the washing tank, make that sulfuric acid concentration keeps 10% in the washing lotion, through steam-heated cal(l)andria 2～2.5 hours; Water temperature remains on 70 ℃～80 ℃, and the row stirring and washing is 5～6 times in the time of then, changes water static 4 hours at every turn; Be washed till neutrality (pH value reaches 6～7); Repeated hydrogenation fluoric acid (40%) 15kg～20kg also heats, and begins to stir, and temperature reaches 70 ℃～80 ℃; Be incubated 2 hours, add water rinse and change for 5～6 times to leave standstill behind the water at every turn and made in the slip pH value reach neutral (pH value 6～7) to get the slip chemical examination discharging water in 4 hours.
4, classification
Washed slip is pumped into weir tank, with big flow the slurry level top to apart from overflow weir 20cm the time, adjust flow and utilize the buoyancy of water classification to go out #1000, #1200, #1500 to be equal to not specification finished product material.
Examining report 1
Unit: %
| F.C | Fe2O3 | Fe | Si | Sio2 | Al2O3 | CaO | MgO | SiC |
| 0.2 | 0.15 | 0.03 | 0.02 | 0.15 | 0.02 | 0.01 | 0.02 | 99.40 |
Embodiment 2
Adjustment excessive acidity pickling: add hydrofluoric acid (40%) 10kg in proportion, nitric acid (density 1.42g/m
3) 15kg, add sulfuric acid (98%) 30kg and stirred 8 hours, left standstill 6～8 hours, add water rinse 5～6 times, make pH value reach neutral (6～7) and get the slip chemical examination.Oven dry in the classification step can be adopted hotblast stove oven dry, 150 ℃～180 ℃ of bake out temperatures, 8 hours time.Water in the classification step purifies, softens through normal, can also increase reverse osmosis water and handle, and makes electrical conductivity of water reduce to 87us/cm by 256us/cm, and total hardness is reduced to 24.1mg/l by 37.2mg/l.
Examining report 2
Unit: %
| F.C | Fe2O3 | Fe | Si | Sio2 | Al2O3 | CaO | MgO | SiC |
| 0.04 | 0.06 | 0.008 | 0.009 | 0.06 | 0.007 | 0.006 | 0.003 | 99.80 |
Implement 3
Adjust the excessive acidity pickling again: add concentrated hydrochloric acid (1.19g/mm
3Concentration 38%) 20kg and nitric acid (concentration 86%) 15kg stirs acidleach and left standstill after 6 hours 8 hours, adds deionized water 200kg and stirs, and repeats 4～5 times, and rinsing is got slip and chemically examined to neutral.
Examining report 3
| F.C | Fe2O3 | Fe | Si | Sio2 | Al2O3 | CaO | MgO | SiC |
| 0.03 | 0.04 | 0.006 | 0.006 | 0.004 | 0.006 | 0.005 | 0.002 | 99.90 |
Claims (5)
1. a green silicon carbide powder method of purification is characterized in that comprising the steps:
(1) washing
Put into the slip that has stirred in the purification container, press pulp density and add 0.35kg trapping agent and 0.4kg silicate dispersant, add pressurized air again, uncombined carbon is floated in the slip foaming, take away uncombined carbon through rotary water current;
(2) alkali cleaning
Put into the slip of washing in the alkali cleaning container, by material: water: the mass ratio of NaOH piece=1: 5: 0.015, heat 70 ℃～80 ℃ through steam, insulated and stirred 4 hours is carried out batch cleaning then, should leave standstill 4 hours after changing water at every turn, is washed till neutrality again;
(3) pickling
Render to the slip that alkali cleaning is intact in the washing tank, add content 98% sulfuric acid, make the sulfuric acid concentration in the washing lotion keep 10%, through steam heating to 2～2.5 hour; Water temperature remains on 70 ℃～80 ℃, carries out stirring and washing then 5～6 times, changes water static 4 hours at every turn, is washed till neutrality; PH value reaches 6～7, adds the hydrofluoric acid 15kg～20kg of concentration 40% again and heats, and begins to stir; Temperature reaches 70 ℃～80 ℃, is incubated 2 hours, adds water rinse 5～6 times; Leave standstill 4 hour after changing water at every turn, make in the material pH value reach neutral discharging water, pH value reaches 6～7;
(4) classification
Washed slip is pumped into weir tank, and after the adding dispersion agent disperseed on inspection, when pushing up slurry level to overflow weir 20cm with big flow, the adjustment flow utilized the buoyancy of water classification to go out the finished product material, and oven dry is until end.
2. a kind of green silicon carbide powder method of purification according to claim 1 is characterized in that, the oven dry in the described classification step can be adopted the hotblast stove oven dry, 150 ℃～180 ℃ of bake out temperatures, 8 hours time.
3. a kind of green silicon carbide powder method of purification according to claim 1 is characterized in that, in the described acid pickling step; Can adjust the excessive acidity pickling: adding hydrofluoric acid 10kg in proportion, to add concentration be 86% nitric acid 15kg; Add sulfuric acid 30kg, stir after 8 hours, left standstill 6～8 hours; Add water rinse, make slip reach neutral.
4. a kind of green silicon carbide powder method of purification according to claim 3 is characterized in that, described adjust acidity again after; Can carry out the severe pickling, add concentrated hydrochloric acid 20kg and nitric acid 15kg, stir acidleach after 6 hours; Left standstill 8 hours; Add the ionized water agitator treating, repeat 4～5 times, rinsing is to neutral.
5. a kind of green silicon carbide powder method of purification according to claim 1; It is characterized in that; Water in the described classification step purifies, softens through normal, makes electrical conductivity of water reduce to 87us/cm by 256us/cm, and total hardness is reduced to 24.1mg/l by 37.2mg/l.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668571A (en) * | 2016-04-01 | 2016-06-15 | 宝兴易达光伏刃料有限公司 | Acid washing and centrifugal dewatering technique of silicon carbide |
| CN106365167A (en) * | 2016-08-31 | 2017-02-01 | 福建省建瓯市富晶宝微粒有限公司 | Silicon carbide micropowder impurity clearing and removing technology and production equipment |
| CN106395827A (en) * | 2016-08-31 | 2017-02-15 | 福建省建瓯市富晶宝微粒有限公司 | Silicon carbide micro-powder purification grading production technology and production equipment thereof |
| CN113769658A (en) * | 2021-09-27 | 2021-12-10 | 郑州中南杰特超硬材料有限公司 | Method for manufacturing novel heating body for synthesizing polycrystalline diamond |
| CN114273022A (en) * | 2021-12-23 | 2022-04-05 | 连云港原发新材料科技有限公司 | Filtering and impurity removing equipment for conveying high-purity alumina and implementation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668571A (en) * | 2016-04-01 | 2016-06-15 | 宝兴易达光伏刃料有限公司 | Acid washing and centrifugal dewatering technique of silicon carbide |
| CN106365167A (en) * | 2016-08-31 | 2017-02-01 | 福建省建瓯市富晶宝微粒有限公司 | Silicon carbide micropowder impurity clearing and removing technology and production equipment |
| CN106395827A (en) * | 2016-08-31 | 2017-02-15 | 福建省建瓯市富晶宝微粒有限公司 | Silicon carbide micro-powder purification grading production technology and production equipment thereof |
| CN113769658A (en) * | 2021-09-27 | 2021-12-10 | 郑州中南杰特超硬材料有限公司 | Method for manufacturing novel heating body for synthesizing polycrystalline diamond |
| CN114273022A (en) * | 2021-12-23 | 2022-04-05 | 连云港原发新材料科技有限公司 | Filtering and impurity removing equipment for conveying high-purity alumina and implementation method thereof |
| CN114273022B (en) * | 2021-12-23 | 2023-06-16 | 江苏汇联铝业有限公司 | Filtering impurity-removing equipment for conveying high-purity alumina and implementation method thereof |
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Application publication date: 20120118 |