CN101372326B - Method for preparing carbon microsphere with ductile iron - Google Patents
Method for preparing carbon microsphere with ductile iron Download PDFInfo
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- CN101372326B CN101372326B CN2008100553822A CN200810055382A CN101372326B CN 101372326 B CN101372326 B CN 101372326B CN 2008100553822 A CN2008100553822 A CN 2008100553822A CN 200810055382 A CN200810055382 A CN 200810055382A CN 101372326 B CN101372326 B CN 101372326B
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Abstract
The invention relates to a method for preparing carbospheres by ductile cast iron. The ductile cast iron is taken as a raw material, a stainless steel ball is taken as a ball mill, anhydrous alcohol is taken as a ball milling medium, dilute hydrochloric acid is taken as a deferrization agent, deionized water is taken as a cleaning agent and a detergent, and argon is taken as a shielding gas for vacuum heat treatment and spheroidization. Black, spherical and granular carbosphere powder is obtained by raw material planning, ball milling with the ball mill, deferrization with the dilute hydrochloric acid, cleaning with the deionized water, filtration, drying, grinding, sieving and vacuum heat treatment and spheroidization. The method has the advantages of short technological process, fewer devices required, no environmental pollution; and the product has high purity which can reach 95%, an average grain size of 1mum, stable physical and chemical properties, and can be matched with a plurality of chemical substances to be made into products with high added values, thus the invention is an ideal method for extracting the carbospheres from the ductile cast iron.
Description
Technical field
The present invention relates to a kind of method, belong to the technical field that ferrous metal extracts carbon material and preparation carbosphere with preparing carbon microsphere with ductile iron.
Background technology
In ferrous metal, steel, iron is most widely used, most important metallic substance, the structure and composition of steel and iron has tangible difference, the iron that exists with the iron-carbon form, be called cast iron, cast iron is divided into white cast iron according to the existence form of carbon, grey cast iron and mottled cast iron, carbon in the white cast iron exists with the cementite form, carbon exists with the flake graphite form in the grey cast iron, carbon exists with cementite and two kinds of forms of graphite in the mottled cast iron, difference according to graphite shape, be divided into grey cast iron again, vermicular cast iron and spheroidal graphite cast iron, spheroidal graphite cast iron are to add nodulizing agent such as ferrosilicon etc. spheroidization of graphite, the globular graphite in the spheroidal graphite cast iron are present in the cast iron matrix in cast iron iron liquid, can improve its effect of isolating, the mechanical property of spheroidal graphite cast iron is improved greatly matrix.
Carbosphere has the performance of many excellences, for example self sintering, unreactiveness, high-bulk-density, good electrical and thermal conductivity and oilness etc. can be used as high strength carbon material, support of the catalyst, activated carbon with high specific surface area, lithium ion secondary electrode negative material, nano-device and energy storage etc.
Be that to extract carbosphere be a new scientific domain to raw material with spheroidal graphite cast iron, because the carbon in the nodular cast iron is fused in the iron liquid with the globular graphite form, the carbon that is fused to is wherein separated, make new product-carbosphere, this is a new technical field, in preparation, sepn process certain degree of difficulty is arranged, its product pattern, purity and production yield rate etc. all are to need to inquire into and study.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at the present situation of background technology and deficiency, with spheroidal graphite cast iron is raw material, by slicing, ball milling, pickling, washing, drying, grinding, vacuum heat treatment spheroidizing etc., finally make the micron order carbosphere, so that extracting carbosphere, the spheroidal graphite cast iron preparation becomes possibility.
Technical scheme
Raw chemical material required for the present invention is: spheroidal graphite cast iron piece, dehydrated alcohol, hydrochloric acid, deionized water, argon gas, Stainless Steel Ball, its consumption is as follows: with gram, milliliter, centimetre
3, the millimeter be measure unit
Spheroidal graphite cast iron piece: FeCSi 1000g ± 2g
Dehydrated alcohol: CH
3COOH 1000ml ± 10ml
Hydrochloric acid: HCl 800ml ± 10ml
Deionized water: H
2O 9000ml ± 20ml
Argon gas: Ar 100000cm
3± 100cm
3
Stainless Steel Ball: 6 of Cr18Ni8 Φ 20mm, 30 of Φ 10mm, 600 of Φ 6mm
The preparation method is as follows:
(1) selected raw chemical material
To carry out selectedly to preparing required raw chemical material, and carry out the control of purity, precision:
Spheroidal graphite cast iron piece: Fe content 93-94%
C content 3.5-4%
Si content 2-2.7%
Dehydrated alcohol: 99.5%
Hydrochloric acid: concentration 36-38%
Deionized water: 99.99%
Argon gas: 99.95%
Stainless Steel Ball: Φ 20mm, Φ 10mm, Φ 6mm, deviation from spherical form Δ S
Ph≤ 0.25 μ m, surface roughness Ra 0.02-0.04 μ m
(2) slicing spheroidal graphite cast iron piece
The spheroidal graphite cast iron piece of 1000g ± 2g is carried out mechanical slicing on planer, make the agglomerating cotton-shaped spheroidal graphite cast iron bits of spheroidal graphite cast iron piece;
(3) mechanical ball milling extracts graphite
In planetary ball mill, carry out;
1. clear up, clean ball grinder:
With dust and the objectionable impurities in the suction cleaner absorption ball grinder;
With deionized water 500ml ± 5ml lavation ball grinder, and scrub jar a mouthful edge, dry after the cleaning with hairbrush;
2. clean Stainless Steel Ball:
In stainless steel vessel, put Φ 20mm * 6, Φ 10mm * 30, Φ 6mm * 600 Stainless Steel Ball adds deionized water 500ml ± 5ml, rocks container, scrubs the Stainless Steel Ball surface with hairbrush, makes its cleaning, dries after the cleaning;
3. in ball grinder, add Stainless Steel Ball, spheroidal graphite cast iron bits and dehydrated alcohol
With cleaned stainless steel ball Φ 20mm * 6, Φ 10mm * 30, Φ 6mm * 600 place ball grinder; Consider spheroidal graphite cast iron to be worth doing 100g ± 2g and place ball grinder; 500ml ± 5ml pours in the ball grinder with the ball-milling medium dehydrated alcohol, and Stainless Steel Ball and spheroidal graphite cast iron bits mass ratio are 10: 1;
4. seal ball grinder
Stainless Steel Ball, spheroidal graphite cast iron are considered to be worth doing with having put, the ball grinder of dehydrated alcohol seals, with O RunddichtringO sealed can mouth;
5. ball milling spheroidal graphite cast iron is considered to be worth doing
Open ball mill, ball grinder rotates, velocity of rotation 400r/min, voltage 248V, electric current 2.6A;
The forward and reverse alternate intervals timing operation of ball grinder, each run time 60min ± 0.5min, pitch time, 30min ± 0.5min to reduce temperature in the ball grinder, moved ball milling time 1200min ± 10min;
20 * 6 of big steel ball Φ are used for broken spheroidal graphite cast iron filing, and 10 * 30 of middle steel ball Φ are used for fragmentation and grind the spheroidal graphite cast iron filing, and 6 * 600 of small ball Φ are used to grind the spheroidal graphite cast iron filing, make it become finely powdered;
6. cooling
Close ball mill behind the ball milling, make spheroidal graphite cast iron fine powder and large, medium and small steel ball and ball-milling medium dehydrated alcohol naturally cool to 20 ℃ ± 3 ℃ with ball grinder;
7. open jar and get liquid
The cooled Stainless Steel Ball of ball milling, spheroidal graphite cast iron ethanol solution are placed stainless steel vessel, separate Stainless Steel Ball and solution, with after the solution separating as in the stainless steel vessel;
Stainless Steel Ball is cleaned with dehydrated alcohol 500ml ± 5ml, after the cleaning scavenging solution is mixed with solution, take out Stainless Steel Ball and also independently deposit;
This solution is: spheroidal graphite cast iron graphite ethanol solution 1000ml ± 20ml
8. filtering graphite ethanol solution
1000ml ± 20ml places filter funnel with the graphite ethanol solution, filters with two-layer middling speed qualitative filter paper, and that retains on the filter paper is product: Graphite Cake;
9. oven dry
Graphite Cake after filtering is collected in the ceramic crucible, in drying baker, carries out drying, 70 ℃ ± 3 ℃ of drying temperatures, time of drying 600min ± 5min, after the drying be: powdered graphite;
(4) pickling deironing
Powdered graphite is placed beaker, add dilute hydrochloric acid 150ml ± 2ml, stir 30min with agitator under 20 ℃ ± 3 ℃ states, make its dissolving, ferro element in the powdered graphite and hydrochloric acid reaction generate FeCl
2Solution, carbon and hydrochloric acid do not react in the graphite, FeCl
2With the dilute hydrochloric acid mixing solutions carbon is separated, reaction formula is as follows:
In the formula:
FeCl
2: iron protochloride
C: carbon
Si: silicon
H
2: hydrogen
The pickling iron removal repeats three times;
With solution left standstill 1440min ± 10min, it is fully reacted after the pickling deironing three times;
(5) filter
The mixing solutions of the graphite after the pickling deironing, iron protochloride and dilute hydrochloric acid is placed filter funnel, filter, filter FeCl with two-layer middling speed qualitative filter paper
2With the mixing solutions of dilute hydrochloric acid, on filter paper, stay the product filter cake, that is: the carbon filter cake;
(6) washing, filtration ten times
The carbon filter cake is placed beaker, add deionized water 500ml ± 5ml, stir 30min, filter the FeCl that filtering is residual then with two-layer middling speed qualitative filter paper with agitator
2With the mixing solutions of dilute hydrochloric acid, on filter paper, stay product: the carbon filter cake;
Washing, filtration repeat ten times;
(7) drying
Place the inherent drying baker of crucible dry carbon filter cake after washing, filtering, 70 ℃ ± 3 ℃ of drying temperatures, time of drying, 600min ± 5min was a product after the drying: carbon dust;
(8) grind, sieve
Dried carbon dust is ground, sieves with agate mortar, pestle,, get product: carbosphere, product particle diameter≤0.038mm with 400 purpose screen filtrations;
(9) vacuum heat treatment spheroidizing
In vacuum sintering furnace, carry out;
1. the carbosphere powder is placed in the quartz crucible, and place on the interior product boat seat of vacuum heat treatment furnace;
2. close bell, extract furnace air, make the interior vacuum tightness of stove remain on 3 * 10 with vacuum pump
-3Pa;
3. open argon bottle, in stove, import argon gas, input speed 100cm
3/ min;
4. open electric control box, make in the stove and heat up, liquid crystal display shows temperature in the stove, and 25 ℃/min of temperature rise rate is warming up to 2000 ℃ ± 5 ℃, and heating-up time 80min ± 2min is at this temperature constant temperature, be incubated, leave standstill 60min ± 2min;
5. close the vacuum heat treatment furnace temperature regulator, make its cooling cooling, continue the input argon gas, input speed 100cm
3/ min makes furnace temperature reduce to 100 ℃ ± 4 ℃ gradually;
(10) secondary cooling
Close vacuum heat treatment furnace vacuum pump, argon bottle, product is naturally cooled to 20 ℃ ± 3 ℃ with body of heater, be final product after the cooling: carbosphere, carbosphere are black, spheroidal powder, median size 1 μ m;
(11) detect, analyze, characterize
To extracting the product carbosphere of preparation, carry out pattern, composition and purity check, sign;
With x-ray diffractometer product structure and composition are analyzed;
With transmission electron microscope microtexture is analyzed;
Carry out the surface topography analysis with scanning electron microscope;
(12) store
Carbosphere powder to preparation places water white Glass Containers, and clean environment wants waterproof, anti-oxidation, fire prevention, acid-proof alkali salt to corrode 20 ℃ ± 3 ℃ of storing temps, relative humidity≤20%.
Described method with preparing carbon microsphere with ductile iron is to be raw material with the spheroidal graphite cast iron piece, is ball-milling medium with the dehydrated alcohol; with the Stainless Steel Ball is the ball milling body; with dilute hydrochloric acid is iron removing reagent, is clean-out system, washing composition with the deionized water, is vacuum heat treatment spheroidizing shielding gas with the argon gas.
The ball milling of described spheroidal graphite cast iron, be in the ball grinder of ball mill, to carry out, storing Stainless Steel Ball Φ 20mm in the ball grinder of 1000ml * 6, Φ 10mm * 30, Φ 6mm * 600, the mass ratio of Stainless Steel Ball and spheroidal graphite cast iron bits is 10: 1, and the ball-milling medium dehydrated alcohol is 500ml ± 5ml.
The spheroidizing of described carbosphere is carried out in vacuum heat treatment furnace, in the bottom of vacuum heat treatment furnace body 12 is stove seat 13, top is bell 14, bell 14 is provided with pore 18, thermopair 19, in the body of heater 12 is furnace chamber 15, is provided with product boat seat 16, quartz crucible 17 in the furnace chamber 15, is carbosphere product 35 on the quartz crucible 17, in the furnace chamber 15 is argon gas 20, and the furnace wall of body of heater 12 is provided with resistance wire 34; Right part at body of heater 12 is provided with argon bottle 31, and is communicated with furnace chamber 15 by argon gas valve 32, tunger tube 33; Lower left quarter at body of heater 12 is provided with vacuum pump 28, and is communicated with furnace chamber 15 by vacuum valve 29, valve tube 30; Left part at body of heater 12 is provided with electric control box 21, and electric control box 21 is provided with liquid crystal display 22, modulator 23, pilot lamp 24, power switch 25, and electric control box 21 is connected with thermopair 19 by lead 26, is connected with resistance wire 34 on the body of heater 12 by lead 27.
Described carbosphere with the spheroidal graphite cast iron preparation, its product pattern is black, spheroidal, particulate state powder, product powder particle median size is 1 μ m.
Beneficial effect
The present invention compares with background technology has tangible advance; make the spheroidal graphite cast iron piece extract the preparation carbosphere and become possibility; it is to be raw material with the spheroidal graphite cast iron piece; with the Stainless Steel Ball is the ball milling body; with the dehydrated alcohol is ball-milling medium; with dilute hydrochloric acid is iron removing reagent; with the deionized water is clean-out system; washing composition; with the argon gas is vacuum heat treatment spheroidizing shielding gas, by the slicing of material; the ball mill ball milling; the hydrochloric acid deironing; deionized water wash; filter; dry; grind; sieve; the spheroidal carbosphere is finally made in the vacuum heat treatment spheroidizing; this preparation method's technical process is short; use equipment is few, and is free from environmental pollution, the product purity height; can reach 95%; the product physical and chemical performance is stable, can make high value added product with number of chemical material coupling, is the very good method with spheroidal graphite cast iron extraction carbosphere.
Description of drawings
Fig. 1 is preparation technology's schema
Fig. 2 is the state graph of spheroidal graphite cast iron ball milling
Fig. 3 is carbosphere vacuum heat treatment nodularization state graph
Fig. 4 is vacuum heat treatment spheroidization treatment temperature and time coordinate graph of a relation
Fig. 5 is carbosphere shape appearance figure before the spheroidizing
Fig. 6 is carbosphere shape appearance figure after the spheroidizing
Fig. 7 is a carbosphere X ray diffracting spectrum after the vacuum heat treatment spheroidizing
Shown in the figure, list of numerals is as follows:
1. ball grinder, 2. base, 3. cover, 4. jar chamber, 5. big steel ball, 6. in steel ball, 7. small ball, 8. dehydrated alcohol, 9. spheroidal graphite cast iron is considered to be worth doing, 10.O RunddichtringO, 11. standing bolts, 12. bodies of heater, 13. the stove seat, 14. bells, 15. furnace chambers, 16. product boat seats, 17. quartz crucible, 18. pores, 19. thermopairs, 20. argon gas, 21. electric control box, 22. liquid crystal display, 23. modulators, 24. pilot lamp, 25. power switches, 26. leads, 27. lead, 28. vacuum pumps, 29. vacuum valves, 30. valve tube, 31. argon bottles, 32. argon gas valves, 33. tunger tube, 34. resistance wires, 35. carbosphere products.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be preparation technology's schema, each parameter is wanted strict control, operation according to the order of sequence.
Preparing required chemical substance material is to draw by the magnitude calculation that sets in advance, with gram, milliliter, millimeter, centimetre 3 be measure unit, can kilogram when industrialization is produced, rise, millimeter, rice 3 be measure unit.
Want strict selected to preparing required spheroidal graphite cast iron piece, anhydrous ethanol medium, deionized water, dilute hydrochloric acid, argon gas, big steel ball, middle steel ball, small ball, and carry out purity, precision control, to guarantee preparation technology's accuracy.
Ball milling is to carry out in the ball grinder of 1000ml, big steel ball in the ball grinder is Φ 20mm * 6, middle steel ball Φ 10mm * 30, small ball Φ 6mm * 600, the mass ratio of its Stainless Steel Ball and spheroidal graphite cast iron bits is 10: 1, the ball-milling medium dehydrated alcohol is 500ml ± 5ml, want strict its ratio of control, make steel ball, spheroidal graphite cast iron bits that abundant space can be arranged, dehydrated alcohol is a ball-milling medium, make graphite behind the ball milling be dissolved in the ethanol and can reduce in the mechanical milling process jar in temperature, collect solution behind the ball milling and can extract carbon.
Ball grinder is the planetary rotation formula, available two, also available four, looks extracted amount and determines.
Want forward and reverse timing intermittently to carry out during ball milling, ball milling 60min, 30min intermittently, thus reduce the heat that produces in the mechanical milling process, to ensure safety.
Large, medium and small steel ball has complementary functions, and big steel ball is used for broken spheroidal graphite cast iron filing, and middle steel ball is used for fragmentation and grinds the spheroidal graphite cast iron filing, and small ball is used to grind the spheroidal graphite cast iron filing makes it become finely powdered.
The dilute hydrochloric acid deironing is with iron in the graphite ethanol solution and hydrochloric acid reaction after-filtration, thereby stays carbon.
The vacuum heat treatment spheroidizing is carried out for the product precision, the nodularization degree that improve carbosphere, can make the circularity of carbosphere better, homogenizing more, and the chemical physics performance is more stable.
It is clean that the ball grinder container that uses in the preparation, filter flask, filter paper, screen cloth, grinding vessel, vacuum heat treatment furnace, crucible etc. will keep, and must not have impurity to get involved, in order to avoid produce by product.
Shown in Figure 2, be ball grinder ball milling view, ball grinder 1 bottom is a base 2, top is cover 3, O RunddichtringO 10, inside is a jar chamber 4,4 built-in amplification steel balls 5, middle steel ball 6, small ball 7, dehydrated alcohol 8, spheroidal graphite cast iron bits 9 in the jar chamber, and base 2 places on the ball mill, can be driven by transmission mechanism, cover 3 tops are reinforced by standing bolt 11.
Shown in Figure 3, be vacuum heat treatment spheroidizing state graph, to clear up furnace chamber 15 earlier during spheroidizing, make its cleaning, add bell 14 sealings then, vacuumize earlier, make vacuum tightness remain on 3 * 10
-3Pa feeds argon gas then, and it is sufficient that the amount of the argon gas 20 in the furnace chamber 15 is wanted, must not be intermittently, and input rate 100cm
3/ min, furnace chamber temperature rises to 2000 ℃ by 20 ℃, and temperature rise rate is 25 ℃/min, and constant temperature insulation 60min makes the abundant nodularization of carbosphere again, cooling cooling then.
Shown in Figure 4, be vacuum heat treatment spheroidization treatment temperature and time coordinate graph of a relation, as seen from the figure: heating up since 20 ℃ is the A point, rise to the B point with 25 ℃/min speed, 60min, i.e. B-C section are left standstill in the constant temperature insulation during to 2000 ℃, be cooled to 100 ℃ then, i.e. the D point.
Shown in Figure 5, for carbosphere product before the spheroidizing amplifies 500 times of shape appearance figures, as seen from the figure: carbosphere is black, spheroidal, particulate state powder, irregular alignment, and median size is 10 μ m, ruler units is 10 μ m.
Shown in Figure 6, for carbosphere product after the spheroidizing amplifies 10000 times of shape appearance figures, as seen from the figure: after vacuum heat treatment, carbosphere product sphericity is homogenizing more, particle diameter obviously diminishes, and median size is 1 μ m, and vacuum heat treatment can obviously promote the degree of graphitization and the nodularization degree of carbosphere, and can make carbosphere particle diameter homogenizing more, ruler units is 1 μ m.
Shown in Figure 7, be carbosphere product diffracted intensity collection of illustrative plates after the vacuum heat treatment spheroidizing, X-coordinate is diffraction angle 2 θ, ordinate zou is the diffracted intensity index, as seen from the figure: the carbosphere degree of graphitization is very high in the vacuum heat treatment after product, corresponding 2 θ=26.5 ° of diffraction peaks of locating to (002) crystal face of carbon, intensity height and peak shape are sharp-pointed, simultaneously bag SiC and Fe in the carbosphere
3C, the diffraction peaks of corresponding SiC (102), (110), (202) crystal face respectively, 2 θ=45.2 ° corresponding Fe are located in 2 θ=35.5 °, 59.9 °, 71.6 °
3The diffraction peak of C (031) crystal face, SiC and Fe
3C is that Si and Fe at high temperature form with the carbon reaction respectively, and the two plays the effect of catalyzer, promotes the nodularization of carbosphere.
Claims (4)
1. method with preparing carbon microsphere with ductile iron, it is characterized in that: required raw chemical material is: spheroidal graphite cast iron piece, dehydrated alcohol, hydrochloric acid, deionized water, argon gas, Stainless Steel Ball, its consumption is as follows: with gram, milliliter, centimetre 3, millimeter is measure unit
Spheroidal graphite cast iron piece: FeCSi 1000g ± 2g
Dehydrated alcohol: CH
3COOH 1000ml ± 10ml
Hydrochloric acid: HCl 800ml ± 10ml
Deionized water: H
2O 9000ml ± 20ml
Argon gas: Ar 100000cm
3± 100cm
3
Stainless Steel Ball: 6 of Cr18Ni8 Φ 20mm, 30 of Φ 10mm, 600 of Φ 6mm
The preparation method is as follows:
(1) selected raw chemical material
To carry out selectedly to preparing required raw chemical material, and carry out the control of purity, precision:
Spheroidal graphite cast iron piece: Fe content 93-94%
C content 3.5-4%
Si content 2-2.7%
Dehydrated alcohol: 99.5%
Hydrochloric acid: concentration 36-38%
Deionized water: 99.99%
Argon gas: 99.95%
Stainless Steel Ball: Φ 20mm, Φ 10mm, Φ 6mm, deviation from spherical form Δ S
Ph≤ 0.25 μ m, surface roughness Ra 0.02-0.04 μ m
(2) slicing spheroidal graphite cast iron piece
The spheroidal graphite cast iron piece of 1000g ± 2g is carried out mechanical slicing on planer, make the agglomerating cotton-shaped spheroidal graphite cast iron bits of spheroidal graphite cast iron piece;
(3) mechanical ball milling extracts graphite
In planetary ball mill, carry out;
1. clear up, clean ball grinder:
With dust and the objectionable impurities in the suction cleaner absorption ball grinder;
With deionized water 500ml ± 5ml lavation ball grinder, and scrub jar a mouthful edge, dry after the cleaning with hairbrush;
2. clean Stainless Steel Ball:
In stainless steel vessel, put Φ 20mm * 6, Φ 10mm * 30, Φ 6mm * 600 Stainless Steel Ball adds deionized water 500ml ± 5ml, rocks container, scrubs steel ball surface with hairbrush, makes its cleaning, dries after the cleaning;
3. in ball grinder, add Stainless Steel Ball, spheroidal graphite cast iron bits and dehydrated alcohol
With cleaned stainless steel ball Φ 20mm * 6, Φ 10mm * 30, Φ 6mm * 600 place ball grinder; Consider spheroidal graphite cast iron to be worth doing 100g ± 2g and place ball grinder; 500ml ± 2ml pours in the ball grinder with the ball-milling medium dehydrated alcohol, and Stainless Steel Ball and spheroidal graphite cast iron bits mass ratio are 10: 1;
4. seal ball grinder
The ball grinder of having put steel ball, iron filings, dehydrated alcohol is sealed, with O RunddichtringO sealed can mouth;
5. ball milling spheroidal graphite cast iron is considered to be worth doing
Open ball mill, ball grinder rotates, velocity of rotation 400r/min, voltage 248V, electric current 2.6A;
The forward and reverse alternate intervals timing operation of ball grinder, each run time 60min ± 0.5min, pitch time, 30min ± 0.5min to reduce temperature in the ball grinder, moved ball milling time 1200min ± 10min;
20 * 6 of big steel ball Φ are used for broken spheroidal graphite cast iron filing, and 10 * 30 of middle steel ball Φ are used for fragmentation and grind the spheroidal graphite cast iron filing, and 6 * 600 of small ball Φ are used to grind the spheroidal graphite cast iron filing, make it become finely powdered;
6. cooling
Close ball mill behind the ball milling, make spheroidal graphite cast iron fine powder and large, medium and small steel ball and ball-milling medium dehydrated alcohol naturally cool to 20 ℃ ± 3 ℃ with ball grinder;
7. open jar and get liquid
The cooled Stainless Steel Ball of ball milling, spheroidal graphite cast iron ethanol solution are placed stainless steel vessel, separate Stainless Steel Ball and solution, with after the solution separating as in the stainless steel vessel;
Stainless Steel Ball is cleaned with dehydrated alcohol 500ml ± 5ml, after the cleaning scavenging solution is mixed with solution, take out Stainless Steel Ball and also independently deposit;
This solution is: spheroidal graphite cast iron graphite ethanol solution 1000ml ± 20ml
8. filtering graphite ethanol solution
1000ml ± 20ml places filter funnel with the graphite ethanol solution, filters with two-layer middling speed qualitative filter paper, and that retains on the filter paper is product: Graphite Cake;
9. oven dry
Graphite Cake after filtering is collected in the ceramic crucible, in drying baker, carries out drying, 70 ℃ ± 3 ℃ of drying temperatures, time of drying 600min ± 5min, after the drying be: powdered graphite;
(4) pickling deironing
Powdered graphite is placed beaker, add dilute hydrochloric acid 150ml ± 2ml, stir 30min with agitator under 20 ℃ ± 3 ℃ states, make its dissolving, ferro element in the powdered graphite and hydrochloric acid reaction generate FeCl
2Solution, carbon and hydrochloric acid do not react in the graphite, FeCl
2With the dilute hydrochloric acid mixing solutions carbon is separated, reaction formula is as follows:
In the formula:
FeCl
2: iron protochloride
C: carbon
Si: silicon
H
2: hydrogen
The pickling iron removal repeats three times;
With solution left standstill 1440min ± 10min, it is fully reacted after the pickling deironing three times;
(5) filter
The mixing solutions of the graphite after the pickling deironing, iron protochloride and dilute hydrochloric acid is placed filter funnel, filter, filter FeCl with two-layer middling speed qualitative filter paper
2With the mixing solutions of dilute hydrochloric acid, on filter paper, stay the product filter cake, that is: the carbon filter cake;
(6) washing, filtration ten times
The carbon filter cake is placed beaker, add deionized water 500ml ± 5ml, stir 30min, filter the FeCl that filtering is residual then with two-layer middling speed qualitative filter paper with agitator
2With the mixing solutions of dilute hydrochloric acid, on filter paper, stay product: the carbon filter cake;
Washing, filtration repeat ten times;
(7) drying
Place the inherent drying baker of crucible dry carbon filter cake after washing, filtering, 70 ℃ ± 3 ℃ of drying temperatures, time of drying, 600min ± 5min was a product after the drying: carbon dust;
(8) grind, sieve
Dried carbon dust is ground, sieves with agate mortar, pestle,, get product: carbosphere, product particle diameter≤0.038mm with 400 purpose screen filtrations;
(9) vacuum heat treatment spheroidizing
In vacuum sintering furnace, carry out;
1. the carbosphere powder is placed in the quartz crucible, and place on the interior intermediate product base of vacuum heat treatment furnace;
2. close bell, extract furnace air, make the interior vacuum tightness of stove remain on 3 * 10 with vacuum pump
-3Pa;
3. open argon bottle, in stove, import argon gas, input speed 100cm
3/ min;
4. open electric control box, make in the stove and heat up, liquid crystal display shows temperature in the stove, and 25 ℃/min of temperature rise rate is warming up to 2000 ℃ ± 5 ℃, and heating-up time 80min ± 2min is at this temperature constant temperature, be incubated, leave standstill 60min ± 2min;
5. close the vacuum heat treatment furnace temperature regulator, make its cooling cooling, continue the input argon gas, input speed 100cm
3/ min makes furnace temperature reduce to 100 ℃ ± 4 ℃ gradually;
(10) secondary cooling
Close vacuum heat treatment furnace, vacuum pump, argon bottle, product is naturally cooled to 20 ℃ ± 3 ℃ with body of heater, be final product after the cooling: carbosphere, carbosphere are black, spheroidal powder, median size 1 μ m;
(11) detect, analyze, characterize
To extracting the product carbosphere of preparation, carry out pattern, composition and purity check, sign;
With x-ray diffractometer product structure and composition are analyzed;
With transmission electron microscope microtexture is analyzed;
Carry out the surface topography analysis with scanning electron microscope;
(12) store
Carbosphere powder to preparation places water white Glass Containers, and clean environment wants waterproof, anti-oxidation, fire prevention, acid-proof alkali salt to corrode 20 ℃ ± 3 ℃ of storing temps, relative humidity≤20%.
2. a kind of method according to claim 1 with preparing carbon microsphere with ductile iron, it is characterized in that: the ball milling of described spheroidal graphite cast iron, be in the ball grinder of ball mill, to carry out, storing Stainless Steel Ball Φ 20mm in the ball grinder of 1000ml * 6, Φ 10mm * 30, Φ 6mm * 600, the mass ratio of Stainless Steel Ball and spheroidal graphite cast iron bits is 10: 1, the ball-milling medium dehydrated alcohol is 500ml ± 5ml.
3. a kind of method according to claim 1 with preparing carbon microsphere with ductile iron, it is characterized in that: the spheroidizing of described carbosphere is carried out in vacuum heat treatment furnace, in the bottom of vacuum heat treatment furnace body (12) is stove seat (13), top is bell (14), bell (14) is provided with pore (18), thermopair (19), in the body of heater (12) is furnace chamber (15), be provided with product boat seat (16) in the furnace chamber 15, quartz crucible (17), quartz crucible (17) is gone up and is carbosphere product (35), in the furnace chamber (15) is argon gas (20), and the furnace wall of body of heater (12) is provided with resistance wire (34); Right part at body of heater (12) is provided with argon bottle (31), and is communicated with furnace chamber (15) by argon gas valve (32), tunger tube (33); Lower left quarter at body of heater (12) is provided with vacuum pump (28), and is communicated with furnace chamber (15) by vacuum valve (29), valve tube (30); Left part at body of heater (12) is provided with electric control box (21), electric control box (21) is provided with liquid crystal display (22), modulator (23), pilot lamp (24), power switch (25), electric control box (21) is connected with thermopair (19) by lead (26), is connected with resistance wire (34) on the body of heater (12) by lead (27).
4. a kind of method with preparing carbon microsphere with ductile iron according to claim 1 is characterized in that: described carbosphere with the spheroidal graphite cast iron preparation, and its product pattern is black, spheroidal, particulate state powder, product powder particle median size is 1 μ m.
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| CN102211005B (en) * | 2011-04-28 | 2013-06-12 | 山东大学 | Method for preparing magnetic graphite microspheres |
| CN105869922A (en) * | 2016-04-11 | 2016-08-17 | 太原理工大学 | Rapid preparation method of manganese oxide/carbon sphere composite material for three-dimensional (3D) printing |
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