CN108218429A - A kind of method that high purity graphite material is prepared using coal tar pitch as raw material - Google Patents
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material Download PDFInfo
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- CN108218429A CN108218429A CN201710932423.0A CN201710932423A CN108218429A CN 108218429 A CN108218429 A CN 108218429A CN 201710932423 A CN201710932423 A CN 201710932423A CN 108218429 A CN108218429 A CN 108218429A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
Abstract
The invention discloses a kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step is as follows：Prepare raw material；Calcination processing is carried out to petroleum coke and pitch coke respectively；By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, powder is made；Kneading processing；Cool material, takes the dish out of the pot；It crushes, powder is made；Sulfuric acid solution, stir process are added in, filtering is rinsed using pure water to neutrality, drying；It is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carries out isostatic pressing；Roasting；Impregnation；Roasting；It is graphitized.Graphite material purity prepared by the present invention is high, and has many advantages, such as that fine structure is fine and close, uniformity is good, mechanical property is good, applied widely, and using coal tar pitch as primary raw material, turn waste into wealth, realize the high added value processing of coal tar pitch, have a vast market prospect.
Description
Technical field
It is specifically a kind of to prepare high purity graphite material by raw material of coal tar pitch the present invention relates to graphite production technical field
The method of material.
Background technology
With the fast development of the industries such as Chinese metallurgy, chemical industry, machinery, medical instrument, nuclear energy, automobile, aerospace, this
A little demands of the industry to graphite and carbon product will constantly increase, and China's graphite and carbon product industry will keep quick and increase
It is long, therefore the production technology of graphite also becomes graphite and the research hotspot of carbon product industry.
During coal tar processing, the residue after distillation removes liquid distillate is referred to as coal tar pitch, coal tar pitch
It is the main component of coal tar, accounts for about the 50%-60% of total amount, it is considered that its main component is polycyclic, condensed-nuclei aromatics and its spreads out
Biology, particular compound composition is sufficiently complex, and the difference of raw coal coal and processing technology also results in the difference of ingredient, existing
Method be mainly to be distinguished according to the softening temperature that it shows, be broadly divided into coal tar pitch, medium temperature coal pitch, low
Warm coal tar pitch.Coal tar pitch carbon residue is high, and graphitization ingredient is more, handling ease, if can be using coal tar pitch as raw material system
Standby graphite, being equivalent to turns waste into wealth.But it is difficult to prepare high purity graphite by raw material of coal tar pitch in the prior art.
Invention content
The purpose of the present invention is to provide a kind of method that high purity graphite material is prepared using coal tar pitch as raw material, with solution
Certainly the problems mentioned above in the background art.
To achieve the above object, the present invention provides following technical solution.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：45-50 parts of coal tar pitch, oil
10-14 parts burnt, 15-18 parts of pitch coke.
2）Calcination processing is carried out at 1350-1400 DEG C to petroleum coke and pitch coke respectively, petroleum coke and forging after being forged
Pitch coke afterwards.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 2-3h, obtains mixture B.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 65-70 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, in 65-70 DEG C, the condition of 150-180r/min
Lower stir process 50-60min, filtering obtain mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 60-70 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body.
10）Green body is put into roaster, is roasted at 1150-1200 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Impregnate green body.
12）Dipping green body at 950-1000 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can.
As further embodiment of the present invention：The raw material is made of the component below according to parts by weight：Coal tar pitch
46-49 parts, 11-13 parts of petroleum coke, 16-17 parts of pitch coke.
As further scheme of the invention：The raw material is made of the component below according to parts by weight：High-temperature coal drips
48 parts green, 12 parts of petroleum coke, 17 parts of pitch coke.
As further scheme of the invention：Step 4）In, kneading treatment temperature is 170-180 DEG C.
As further scheme of the invention：Step 9）In, the pressure of isostatic pressing is 120-140Mpa.
As further scheme of the invention：Step 11）In, impregnating agent used is medium temperature coal pitch.
As further scheme of the invention：Step 13）In, graphitization temperature is 3000 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows.
Graphite material purity prepared by the present invention is high, and with that fine structure is fine and close, uniformity is good, mechanical property is good etc. is excellent
Point, it is applied widely, there is important market value and social value.Graphite material prepared by the present invention uses coal tar pitch
As primary raw material, turn waste into wealth, realize the high added value processing of coal tar pitch, have a vast market prospect.
Specific embodiment
Technical scheme of the present invention is described in more detail With reference to embodiment.
Embodiment 1.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：45 parts of coal tar pitch, petroleum coke 10
Part, 15 parts of pitch coke.
2）Calcination processing is carried out at 1350 DEG C to petroleum coke and pitch coke respectively, petroleum coke and pitch after forging after being forged
It is burnt.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 2h, obtains mixture B, wherein, at kneading
It is 170 DEG C to manage temperature.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 65 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 65 DEG C, 150r/min
50min is handled, filtering obtains mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 60 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body, wherein, the pressure of isostatic pressing is 120Mpa.
10）Green body is put into roaster, is roasted at 1150 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Green body is impregnated, impregnating agent used is medium temperature coal pitch.
12）Dipping green body at 950 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can, wherein, graphitization temperature 3000
℃。
Embodiment 2.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：46 parts of coal tar pitch, petroleum coke 13
Part, 16 parts of pitch coke.
2）Calcination processing is carried out at 1360 DEG C to petroleum coke and pitch coke respectively, petroleum coke and pitch after forging after being forged
It is burnt.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 2.5h, obtains mixture B, wherein, kneading
Treatment temperature is 172 DEG C.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 68 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 67 DEG C, 155r/min
53min is handled, filtering obtains mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 62 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body, wherein, the pressure of isostatic pressing is 123Mpa.
10）Green body is put into roaster, is roasted at 1160 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Green body is impregnated, impregnating agent used is medium temperature coal pitch.
12）Dipping green body at 960 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can, wherein, graphitization temperature 3000
℃。
Embodiment 3.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：48 parts of coal tar pitch, petroleum coke 12
Part, 17 parts of pitch coke.
2）Calcination processing is carried out at 1380 DEG C to petroleum coke and pitch coke respectively, petroleum coke and pitch after forging after being forged
It is burnt.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 2.5h, obtains mixture B, wherein, kneading
Treatment temperature is 175 DEG C.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 68 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 68 DEG C, 165r/min
55min is handled, filtering obtains mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 65 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body, wherein, the pressure of isostatic pressing is 130Mpa.
10）Green body is put into roaster, is roasted at 1180 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Green body is impregnated, impregnating agent used is medium temperature coal pitch.
12）Dipping green body at 980 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can, wherein, graphitization temperature 3000
℃。
Embodiment 4.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：49 parts of coal tar pitch, petroleum coke 11
Part, 17 parts of pitch coke.
2）Calcination processing is carried out at 1390 DEG C to petroleum coke and pitch coke respectively, petroleum coke and pitch after forging after being forged
It is burnt.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 2.5h, obtains mixture B, wherein, kneading
Treatment temperature is 178 DEG C.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 69 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 68 DEG C, 170r/min
56min is handled, filtering obtains mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 65 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body, wherein, the pressure of isostatic pressing is 135Mpa.
10）Green body is put into roaster, is roasted at 1190 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Green body is impregnated, impregnating agent used is medium temperature coal pitch.
12）Dipping green body at 990 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can, wherein, graphitization temperature 3000
℃。
Embodiment 5.
A kind of method that high purity graphite material is prepared using coal tar pitch as raw material, step are as follows.
1）Prepare raw material, the raw material is made of the component below according to parts by weight：50 parts of coal tar pitch, petroleum coke 14
Part, 18 parts of pitch coke.
2）Calcination processing is carried out at 1400 DEG C to petroleum coke and pitch coke respectively, petroleum coke and pitch after forging after being forged
It is burnt.
3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity is made
For 10-15 μm of powder, mixture A is obtained.
4）Mixture A is put into heated type kneading machine, after kneading processing 3h, obtains mixture B, wherein, at kneading
It is 180 DEG C to manage temperature.
5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 70 DEG C, takes the dish out of the pot, obtains mixture C.
6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D.
7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 70 DEG C, 180r/min
60min is handled, filtering obtains mixture E.
8）Mixture E is rinsed using pure water to neutrality, and dried at 70 DEG C, obtains mixture F.
9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, carry out isostatic pressed into
Type obtains green body, wherein, the pressure of isostatic pressing is 140Mpa.
10）Green body is put into roaster, is roasted at 1200 DEG C, obtains primary roasting green body.
11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, obtain
Green body is impregnated, impregnating agent used is medium temperature coal pitch.
12）Dipping green body at 1000 DEG C is roasted, obtains after baking green body.
13）After baking green body is put into graphitizing furnace and is graphitized, you can, wherein, graphitization temperature 3000
℃。
Graphite material purity prepared by the present invention is high, and with that fine structure is fine and close, uniformity is good, mechanical property is good etc. is excellent
Point, it is applied widely, there is important market value and social value.Graphite material prepared by the present invention uses coal tar pitch
As primary raw material, turn waste into wealth, realize the high added value processing of coal tar pitch, have a vast market prospect.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, can also be under the premise of present inventive concept not be departed from the knowledge that one skilled in the relevant art has
Various changes can be made.
Claims (7)
- A kind of 1. method that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that step is as follows：1）Prepare raw material, the raw material is made of the component below according to parts by weight：45-50 parts of coal tar pitch, petroleum coke 10- 14 parts, 15-18 parts of pitch coke；2）Calcination processing at 1350-1400 DEG C is carried out to petroleum coke and pitch coke respectively, is dripped after petroleum coke and forging after being forged It is green burnt；3）By pitch coke after petroleum coke after coal tar pitch, forging and forging after coarse crushing, put into roller mill, granularity, which is made, is 10-15 μm of powder obtains mixture A；4）Mixture A is put into heated type kneading machine, after kneading processing 2-3h, obtains mixture B；5）Mixture B is put into cool material is carried out in cool material pot, treats that temperature reaches 65-70 DEG C, takes the dish out of the pot, obtains mixture C；6）Mixture C is put into roller mill and is crushed, the powder that granularity is 20-30 μm is made, obtains mixture D；7）Sulfuric acid solution is added in into mixture D, is put into agitator, is stirred under conditions of 65-70 DEG C, 150-180r/min Processing 50-60min is mixed, filtering obtains mixture E；8）Mixture E is rinsed using pure water to neutrality, and dried at 60-70 DEG C, obtains mixture F；9）Mixture F is fitted into Rubber membrane cover, after high-frequency electromagnetic vibrating compacting and vacuumizing, isostatic pressing is carried out, obtains Obtain green body；10）Green body is put into roaster, is roasted at 1150-1200 DEG C, obtains primary roasting green body；11）To once roast green body it is preheated after, put into impregnating autoclave in, carry out impregnation under vacuum, impregnated Green body；12）Dipping green body at 950-1000 DEG C is roasted, obtains after baking green body；13）After baking green body is put into graphitizing furnace and is graphitized, you can.
- 2. the method according to claim 1 that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that The raw material is made of the component below according to parts by weight：46-49 parts of coal tar pitch, 11-13 parts of petroleum coke, pitch coke 16- 17 parts.
- 3. the method according to claim 2 that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that The raw material is made of the component below according to parts by weight：48 parts of coal tar pitch, 12 parts of petroleum coke, 17 parts of pitch coke.
- 4. the method that high purity graphite material is prepared using coal tar pitch as raw material according to claims 1 or 2 or 3, special Sign is, step 4）In, kneading treatment temperature is 170-180 DEG C.
- 5. the method according to claim 4 that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that Step 9）In, the pressure of isostatic pressing is 120-140Mpa.
- 6. the method according to claim 5 that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that Step 11）In, impregnating agent used is medium temperature coal pitch.
- 7. the method according to claim 6 that high purity graphite material is prepared using coal tar pitch as raw material, which is characterized in that Step 13）In, graphitization temperature is 3000 DEG C.
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| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
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| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN114804880A (en) * | 2022-04-06 | 2022-07-29 | 宝丰县洁石碳素材料有限公司 | Method for processing graphite by electric spark |
| CN115466121A (en) * | 2022-10-28 | 2022-12-13 | 万基控股集团石墨制品有限公司 | Preparation method of graphite electrode |
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| CN110642248A (en) * | 2019-11-19 | 2020-01-03 | 平顶山市天宝特种材料有限公司 | Production method of fine-structure high-purity graphite with changed molecular arrangement combination |
| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN114804880A (en) * | 2022-04-06 | 2022-07-29 | 宝丰县洁石碳素材料有限公司 | Method for processing graphite by electric spark |
| CN115466121A (en) * | 2022-10-28 | 2022-12-13 | 万基控股集团石墨制品有限公司 | Preparation method of graphite electrode |
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