CN103102165B - Method for intensively producing refractory material through coal tar pitch needle coke - Google Patents
Method for intensively producing refractory material through coal tar pitch needle coke Download PDFInfo
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Abstract
The invention discloses a method for intensively producing a refractory material through coal tar pitch needle coke. Unutilized QI1 residues of the prior art, coal tar, delayed coking tower side oil products, a modifier and a nickel, vanadium and cobalt removing agent are subjected to separation, sedimentation, purification and oxidization modification to produce a refractory material adhesion agent with high softening point; the refractory material adhesion agent has the performances of high slag resistance, oxidation resistance and thermal shock resistance, is mixed with active agents such as white carbon black, ammonium humate, polyvinyl alcohol, carboxymethyl cellulose and the like and dry pressed to obtain the refractory material for a steel refining furnace, and the refractory material is better than phenolic resin; and the refractory material, carbon black, dimethylbenzene, benzofuran, polyethylene glycol and the like are dissolved, mixed and dissolved so as to obtain a liquid spraying adhesion agent for repairing the steel refining furnace, and the repairing strength of the liquid spraying adhesion agent is better than the repairing strength of common medium temperature pitch. The service lives of equipment such as converters, electric furnaces, calcinators and the like can be prolonged.
Description
Technical field
The present invention relates to the method for the intensive production refractory materials of a kind of tar needle-shape coke, belong to the technical field of the preparation of pyrocarbon material and application.
Background technology
Softening temperature is one of main performance index of Coal-tar Pitch, especially for use in the Coal-tar Pitch used for refractory material on electric furnace, converter steelmaking and high-temperature calcination equipment, more require the softening temperature of coal-tar pitch up to 230～280 ℃, also require coal-tar pitch to there is higher slag resistance, oxidation-resistance, heat-shock resistance simultaneously, otherwise will directly have influence on the work-ing life of converter, electric furnace, this is that general middle temperature, coal tar pitch institute are inaccessiable.Existing Coal-tar Pitch, mostly by the oxidative polycondensation of mesophase pitch, utilize special technique and equipment produce, and to needle coke production technology at an isolated quinoline insolubles (QI with the impurity such as heavy metal, carbon residue
1) deep processing and utilization no longer.Its defect can make the production cost of tar needle-shape coke improve, and forms solid waste in production process.
Summary of the invention
The present invention aims to provide the method for the intensive production fire bond of a kind of tar needle-shape coke, and it is more reasonable that the method is produced than single needle coke, and cost is lower, and energy
obtain compared with high softening-pointcoal-tar Pitch used for refractory material.
The present invention realizes by following technical proposal: the method for the intensive production fire bond of a kind of tar needle-shape coke, is characterized in that comprising following each step:
A. get raw material by the formula of following mass percent:
Coal-tar pitch 30～50%
Modified coal-tar 40～50%
Conditioning agent 5.5～19.5%
Nickel, vanadium, cobalt remove agent 1.0～10.5%;
B. be 50～200 ℃ by the raw material of steps A in temperature, under the condition that speed is 10～50mm/min, separate, obtain bottom isolate and top isolate;
C. B step is separated to the top isolate obtaining through centrifugation, obtain the solvent oil product on upper strata, and middle level thing and lower floor's thing;
D. bottom isolate step B being obtained remains at 120～250 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.01～0.5, mixture is passed in the isolate of bottom, at 220～300 ℃ of temperature, react 3～8h, obtain softening temperature and reach the intermediates of 230～260 ℃, wherein mixture is following volume ratio: air: oxygen: carbolic oil=0.5～1.2: 0.25～1.2: 0.1;
E. be to carry out heat screening under 250～400 ℃, the sieve aperture condition that is 50～1000um by the intermediates of step D in temperature, obtain the screen overflow of particle diameter > 50～1000um, further pulverize screen overflow and obtain fire bond, and the screen underflow of particle diameter < 50～1000um is directly as fire bond.
Modified coal-tar in described steps A obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=30～50 ︰ 40～50, after the by-product oil of coal tar and needle coke delayed coking drums is mixed, by the amount of 0.20～1L/min, in mixing oil, pass into technical grade hydrogen, and be that 350～460 ℃, pressure are that 0.1～5Mpa, oil gas speed ratio are 0.1～3.0h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 3～15h, obtain modified coal-tar.
Conditioning agent in described steps A is the conditioning agent that aromatize degree BMCI is 30～75, for a kind of in following organism or by several composition the in following organism: crude benzol, toluene, heavy benzol, kerosene, diesel oil, ethylene glycol, propylene glycol, aromatic solvent naphtha, washing oil, carbolineum, de-aromatic solvent naphtha, wherein, described aromatize degree BMCI is calculated by following formula:
BMCI=?48640/Tb,m+473.6d-456.8
In formula, Tb, m is raw material boiling point mean value, unit is K;
D is the density of raw material in the time of 288.5K, and unit is kg/m
3.
The conditioning agent that conditioning agent preferred fragrance degree BMCI in described steps A is 55～70.
Coal-tar pitch in described steps A is mid-temperature pitch, is the lighting coal tar of coal needle coke delay coking process by-product.
It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that nickel in described steps A, vanadium, cobalt remove agent, the reference of the method is: Shanghai University Of Electric Power's journal, 2010(1), 61-65 page, by Liu Kejia, Li Xiaohua, " microwave method of alkyl imidazole ionic liquid is synthesized and is purified " that the people such as Wang Luochun deliver.
The separation of described step B completes in conventional settlement separator, the centrifugation of described C step completes on conventional three sections of centrifuge separators, or the separation of B, C step is to complete in the tripping device being combined into by settlement separate machine and three sections of centrifuge separators.
The heat screening condition of described step e, preferably 250～300 ℃ of temperature, sieve aperture is 300～600um preferably.
Described step e gained fire bond mixes with white carbon black, silicon carbide, white fused alumina by following mass ratio, that is: fire bond: white carbon black: silicon carbide: white fused alumina=1～5: 25～40: 30～50: 40～60, and be 1～5Mpa/m at pressure
2under, dry-pressing formed after, at 110～300 ℃, 300～550 ℃, 550～850 ℃, 850～1100 ℃, 1100～1500 ℃, 1500～2000 ℃, stage drying 3～15h, makes the refractory materials that calcining furnace is used respectively.
Described step e gained fire bond and white carbon black, ammonium humate (HA-NH
4), tween (TWEEN-85), silane-KH570, polyvinyl alcohol (PVA-1799), carboxymethyl cellulose (CMC) promoting agent, mix i.e.: fire bond: white carbon black: ammonium humate (HA-NH by following mass ratio
4): tween (TWEEN-85): silane-KH570: polyvinyl alcohol (PVA-1799): carboxymethyl cellulose (CMC) promoting agent=10～35:10～50: 5～20: 25～50: 25～50: 5～10: 5～15, and dissolve after mixing at 50～300 ℃ of temperature, make the refractory materials that steel melting furnace is used.
The middle level thing of described C step can be used as needle coke viscid bitumen raw material; Lower floor's thing can be used as carbon fiber raw material.
Advantage of the present invention and effect: adopt such scheme, the QI that prior art is not utilized
1residue, with coal tar, delayed coking drums by-product oil, conditioning agent and nickel, vanadium, cobalt remove agent together through separating, subsiding and purifying, oxidation modification, make the fire bond of high softening-point, wherein softening temperature reaches 210～260 ℃, heat-shock resistance R=2.0 × 104～2.6 × 104s, thermal expansivity a=1.0 × 10
-6～1.3 × 10
-6/ K, viscosity reaches 25200～149000/mPas
-1, not only softening temperature is high, and has higher slag resistance, oxidation-resistance, thermal shock resistance, mix with white carbon black, ammonium humate, polyvinyl alcohol, the agent of carboxymethyl cellulose isoreactivity, and after dry-pressing formed, making steel melting furnace refractory materials, performance is better than resol; Dissolve after mixed dissolution with carbon black, dimethylbenzene, cumarone, polyoxyethylene glycol etc., make again steel melting furnace and study for a second time courses one has flunked with liquid spray type binding agent, study for a second time courses one has flunked the common mid-temperature pitch of strength ratio high.Can effectively extend the work-ing life of the equipment such as converter, electric furnace, calcining furnace.The present invention had both guaranteed the cleaner production of needle coke, had reduced again production cost, and the feed composition that has solved tar needle-shape coke intensive production carbon fiber, fire bond separates and processing and utilization.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
A. get raw material by the formula of following mass percent:
Coal-tar pitch 50%
Modified coal-tar 40%
Conditioning agent 9.0%
Nickel, vanadium, cobalt remove agent 1.0%;
Wherein, modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=30 ︰ 45, after the by-product oil of coal tar and needle coke delayed coking drums is mixed, press the amount of 1L/min, in mixing oil, pass into technical grade hydrogen, and be that 460 ℃, pressure are that 0.1Mpa, oil gas speed ratio are 2.0h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 15h, obtain modified coal-tar; Conditioning agent is the conditioning agent that aromatize degree BMCI is 75, is made up of following organism: crude benzol, toluene, heavy benzol, diesel oil, ethylene glycol; Coal-tar pitch is mid-temperature pitch, is the lighting coal tar of coal needle coke delay coking process by-product; It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that nickel, vanadium, cobalt remove agent;
B. be 100 ℃ by the raw material of steps A in temperature, under the condition that speed is 50mm/min, in conventional settlement separator, separate, obtain bottom isolate and top isolate;
C. step B is separated to the top isolate obtaining and carry out centrifugation in conventional three sections of centrifuge separators, obtain the recycled solvent oil on upper strata, and middle level thing and lower floor's thing; Middle level thing can be used as needle coke viscid bitumen raw material; Lower floor's thing can be used as carbon fiber raw material;
D. bottom isolate step B being obtained remains at 120 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.3, mixture is passed in the isolate of bottom, at 300 ℃ of temperature, react 3h, obtain softening temperature and reach the intermediates of 250 ℃, wherein mixture is following volume ratio: air: oxygen: carbolic oil=1.2: 1.2: 0.1;
E. be to carry out heat screening under 300 ℃, the sieve aperture condition that is 50um by the intermediates of step D in temperature, obtain the screen overflow of particle diameter > 50um, further pulverize screen overflow and obtain fire bond, and the screen underflow of particle diameter < 50um is directly as fire bond.
Step e gained fire bond mixes with white carbon black, silicon carbide, white fused alumina by following mass ratio: 5: 25: 40: 60, and be 3Mpa/m at pressure
2under, dry-pressing formed after, at 110 ℃, 550 ℃, 650 ℃, 1100 ℃, 1300 ℃, 1500 ℃, stage drying 12h, makes calcining furnace refractory materials respectively.
Step e gained fire bond and white carbon black, ammonium humate (HA-NH
4), tween (TWEEN-85), silane-KH570, polyvinyl alcohol (PVA-1799), carboxymethyl cellulose (CMC) promoting agent, mix by following mass ratio: 35:40: 5: 25: 50: 8: 15, and dissolve after mixing at 300 ℃ of temperature, make steel melting furnace refractory materials.
Embodiment 2
A. get raw material by the formula of following mass percent:
Coal-tar pitch 30%
Modified coal-tar 45%
Conditioning agent 14.5%
Nickel, vanadium, cobalt remove agent 10.5%;
Wherein, modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=50 ︰ 40, after the by-product oil of coal tar and needle coke delayed coking drums is mixed, press the amount of 0.8L/min, in mixing oil, pass into technical grade hydrogen, and be that 400 ℃, pressure are that 5Mpa, oil gas speed ratio are 3.0h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 12h, obtain modified coal-tar; Conditioning agent is the conditioning agent that aromatize degree BMCI is 30, is made up of organism kerosene; Coal-tar pitch is mid-temperature pitch, is the lighting coal tar of coal needle coke delay coking process by-product; It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that nickel, vanadium, cobalt remove agent;
B. be 200 ℃ by the raw material of steps A in temperature, under the condition that speed is 10mm/min, in the tripping device being combined into three sections of centrifuge separators by settlement separate machine, separate, obtain bottom isolate and top isolate;
C. step B is separated in the tripping device that the top isolate that obtains is combined into via settlement separate machine and three sections of centrifuge separators and carry out centrifugation, obtain the recycled solvent oil on upper strata, and middle level thing and lower floor's thing; Middle level thing can be used as needle coke viscid bitumen raw material; Lower floor's thing can be used as carbon fiber raw material;
D. bottom isolate step B being obtained remains at 250 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.01, mixture is passed in the isolate of bottom, at 220 ℃ of temperature, react 8h, obtain softening temperature and reach the intermediates of 230 ℃, wherein mixture is following volume ratio: air: oxygen: carbolic oil=0.5: 0.25: 0.1;
E. be to carry out heat screening under 250 ℃, the sieve aperture condition that is 1000um by the intermediates of step D in temperature, obtain the screen overflow of particle diameter > 1000um, further pulverize screen overflow and obtain fire bond, and the screen underflow of particle diameter < 1000um is directly as fire bond.
Step e gained fire bond mixes with white carbon black, silicon carbide, white fused alumina by following mass ratio: 1:30: at pressure be 5Mpa/m at 50: 40
2under, dry-pressing formed after, at 300 ℃, 400 ℃, 850 ℃, 1000 ℃, 1500 ℃, 1800 ℃, stage drying 3h, makes calcining furnace refractory materials respectively.
Step e gained fire bond and white carbon black, ammonium humate (HA-NH
4), tween (TWEEN-85), silane-KH570, polyvinyl alcohol (PVA-1799), carboxymethyl cellulose (CMC) promoting agent, mix by following mass ratio: 10:10: 10: 50: 35: 10: 5, and dissolve after mixing at 200 ℃ of temperature, make steel melting furnace refractory materials.
Embodiment 3
A. get raw material by the formula of following mass percent:
Coal-tar pitch 35%
Modified coal-tar 40%
Conditioning agent 19.5%
Nickel, vanadium, cobalt remove agent 5.5%;
Wherein, modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=40 ︰ 50, after the by-product oil of coal tar and needle coke delayed coking drums is mixed, press the amount of 0.20L/min, in mixing oil, pass into technical grade hydrogen, and be that 350 ℃, pressure are that 3Mpa, oil gas speed ratio are 0.1h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 3h, obtain modified coal-tar; Conditioning agent is the conditioning agent that aromatize degree BMCI is 55, is made up of following organism: propylene glycol, aromatic solvent naphtha, washing oil, carbolineum, de-aromatic solvent naphtha; Coal-tar pitch is mid-temperature pitch, is the lighting coal tar of coal needle coke delay coking process by-product; It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that nickel, vanadium, cobalt remove agent;
B. be 50 ℃ by the raw material of steps A in temperature, under the condition that speed is 30mm/min, in conventional settlement separator, separate, obtain bottom isolate and top isolate;
C. step B is separated to the top isolate obtaining and carry out centrifugation in conventional three sections of centrifuge separators, obtain the recycled solvent oil on upper strata, and middle level thing and lower floor's thing; Middle level thing can be used as needle coke viscid bitumen raw material; Lower floor's thing can be used as carbon fiber raw material;
D. bottom isolate step B being obtained remains at 200 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.5, mixture is passed in the isolate of bottom, at 280 ℃ of temperature, react 5h, obtain softening temperature and reach the intermediates of 260 ℃, wherein mixture is following volume ratio: air: oxygen: carbolic oil=1.0: 1.0: 0.1;
E. be to carry out heat screening under 400 ℃, the sieve aperture condition that is 300um by the intermediates of step D in temperature, obtain the screen overflow of particle diameter > 300um, further pulverize screen overflow and obtain fire bond, and the screen underflow of particle diameter < 300um is directly as fire bond.
Step e gained fire bond mixes with white carbon black, silicon carbide, white fused alumina by following mass ratio: 3: 40: 30: 50, and be 1Mpa/m at pressure
2under, dry-pressing formed after, at 200 ℃, 300 ℃, 550 ℃, 850 ℃, 1100 ℃, 2000 ℃, stage drying 15h, makes calcining furnace refractory materials respectively.
Step e gained fire bond and white carbon black, ammonium humate (HA-NH
4), tween (TWEEN-85), silane-KH570, polyvinyl alcohol (PVA-1799), carboxymethyl cellulose (CMC) promoting agent, mix by following mass ratio: 25:50: 20: 35: 25: 5: 10, and dissolve after mixing at 50 ℃ of temperature, make steel melting furnace refractory materials.
Embodiment 4
A. get raw material by the formula of following mass percent:
Coal-tar pitch 30%
Modified coal-tar 50%
Conditioning agent 10.5%
Nickel, vanadium, cobalt remove agent 9.5%;
Wherein, modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=50 ︰ 50, after the by-product oil of coal tar and needle coke delayed coking drums is mixed, press the amount of 0.5L/min, in mixing oil, pass into technical grade hydrogen, and be that 360 ℃, pressure are that 4Mpa, oil gas speed ratio are 1h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 8h, obtain modified coal-tar; Conditioning agent is the conditioning agent that aromatize degree BMCI is 70, is made up of organism aromatic solvent naphtha; Coal-tar pitch is mid-temperature pitch, is the lighting coal tar of coal needle coke delay coking process by-product; It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that nickel, vanadium, cobalt remove agent;
B. be 130 ℃ by the raw material of steps A in temperature, under the condition that speed is 40mm/min, in the tripping device being combined into three sections of centrifuge separators by settlement separate machine, separate, obtain bottom isolate and top isolate;
C. step B is separated in the tripping device that the top isolate that obtains is combined into via settlement separate machine and three sections of centrifuge separators and carry out centrifugation, obtain the recycled solvent oil on upper strata, and middle level thing and lower floor's thing; Middle level thing can be used as needle coke viscid bitumen raw material; Lower floor's thing can be used as carbon fiber raw material;
D. bottom isolate step B being obtained remains at 160 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.4, mixture is passed in the isolate of bottom, at 290 ℃ of temperature, react 4h, obtain softening temperature and reach the intermediates of 240 ℃, wherein mixture is following volume ratio: air: oxygen: carbolic oil=1.2: 0.25: 0.1;
E. be to carry out heat screening under 280 ℃, the sieve aperture condition that is 600um by the intermediates of step D in temperature, obtain the screen overflow of particle diameter > 600um, further pulverize screen overflow and obtain fire bond, and the screen underflow of particle diameter < 600um is directly as fire bond.
Step e gained fire bond mixes with white carbon black, silicon carbide, white fused alumina by following mass ratio: 2: 40: 35: 45, and be 4Mpa/m at pressure
2under, dry-pressing formed after, at 110 ℃, 450 ℃, 750 ℃, 900 ℃, 1500 ℃, 1900 ℃, stage drying 13h, makes calcining furnace refractory materials respectively.
Step e gained fire bond and white carbon black, ammonium humate (HA-NH
4), tween (TWEEN-85), silane-KH570, polyvinyl alcohol (PVA-1799), carboxymethyl cellulose (CMC) promoting agent, mix by following mass ratio: 20:50: 15: 40: 25: 9: 13, and dissolve after mixing at 220 ℃ of temperature, make steel melting furnace refractory materials.
Claims (5)
1. the method for the intensive production refractory materials of tar needle-shape coke, it is characterized in that fire bond to mix with white carbon black, silicon carbide, white fused alumina by following mass ratio, that is: fire bond: white carbon black: silicon carbide: white fused alumina=1～5: 25～40: 30～50: 40～60, be 1～5MPa/m at pressure
2under, dry-pressing formed after, at 110～300 ℃, 300～550 ℃, 550～850 ℃, 850～1100 ℃, 1100～1500 ℃, 1500～2000 ℃, stage drying 3～15h, makes the refractory materials that calcining furnace is used respectively;
Wherein: fire bond makes through the following step:
A. get raw material by the formula of following mass percent:
Coal-tar pitch 30～50%
Modified coal-tar 40～50%
Conditioning agent 5.5～19.5%
Nickel, vanadium, cobalt remove agent 1.0～10.5%;
Described coal-tar pitch is the lighting coal tar of coal needle coke delay coking process by-product;
Described modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=30～50 ︰ 40～50, after being mixed with by-product oil, coal tar obtains mixing oil, by the amount of 0.20～1L/min, in mixing oil, pass into technical grade hydrogen, and be that 350～460 ℃, pressure are that 0.1～5MPa, oil gas speed ratio are 0.1～3.0h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 3～15h, obtain modified coal-tar;
Described conditioning agent is the conditioning agent that aromatize degree BMCI is 30～75, for a kind of in following organism or by several composition the in following organism: crude benzol, toluene, heavy benzol, kerosene, diesel oil, ethylene glycol, propylene glycol, washing oil, carbolineum, de-aromatic solvent naphtha, wherein, described aromatize degree BMCI is calculated by following formula:
BMCI=?48640/Tb,m+473.6d-456.8
In formula, Tb, m is raw material boiling point mean value, unit is K;
D is the density of raw material in the time of 288.5K, and unit is Kg/m
3;
It is to obtain according to " preparation method of N-Methylimidazole ionic liquid " that described nickel, vanadium, cobalt remove agent;
B. be 50～200 ℃ by the raw material of steps A in temperature, under the condition that speed is 10～50mm/min, separate, obtain bottom isolate and top isolate;
C. B step is separated to the top isolate obtaining through centrifugation, obtain the solvent oil product on upper strata, and middle level thing and lower floor's thing;
D. bottom isolate step B being obtained remains at 120～250 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.01～0.5, mixture is passed in the isolate of bottom, at 220～300 ℃ of temperature, react 3～8h, obtain softening temperature and reach the intermediates of 230～260 ℃, wherein the volume ratio of mixture is: air: oxygen: carbolic oil=0.5～1.2: 0.25～1.2: 0.1;
E. be that 250～400 ℃, sieve aperture are to carry out heat screening under the condition of 50～1000 μ m by the middle level thing of step D in temperature, obtain the screen overflow of particle diameter > 50～1000 μ m, further pulverize this screen overflow and obtain fire bond, and the screen underflow of particle diameter < 50～1000 μ m is directly as fire bond.
2. the method for the intensive production refractory materials of a kind of tar needle-shape coke according to claim 1, is characterized in that: the conditioning agent in described steps A is the conditioning agent that aromatize degree BMCI is 55～70.
3. the method for the intensive production refractory materials of a kind of tar needle-shape coke according to claim 1, it is characterized in that: the separation of described step B completes in conventional settlement separator, the centrifugation of described C step completes on conventional three sections of centrifuge separators, or the separation of B, C step is to complete in the tripping device being combined into by settlement separate machine and three sections of centrifuge separators.
4. the method for the intensive production refractory materials of a kind of tar needle-shape coke according to claim 1, is characterized in that: the heat screening condition of described step e, and temperature is 250～300 ℃, sieve aperture is 300～600 μ m.
5. a method for the intensive production refractory materials of tar needle-shape coke, is characterized in that fire bond and white carbon black, ammonium humate HA-NH
4, tween TWEEN-85, silane-KH570, PVAC polyvinylalcohol-1799, carboxyl methyl cellulose promoting agent, mix i.e.: fire bond: white carbon black: ammonium humate HA-NH by following mass ratio
4: tween TWEEN-85: silane-KH570: PVAC polyvinylalcohol-1799: carboxyl methyl cellulose promoting agent=10～35:10～50: 5～20: 25～50: 25～50: 5～10: 5～15, and dissolve after mixing at 50～300 ℃ of temperature, make the refractory materials that steel melting furnace is used;
Wherein, fire bond makes through the following step:
A. get raw material by the formula of following mass percent:
Coal-tar pitch 30～50%
Modified coal-tar 40～50%
Conditioning agent 5.5～19.5%
Nickel, vanadium, cobalt remove agent 1.0～10.5%;
Described coal-tar pitch is the lighting coal tar of coal needle coke delay coking process by-product;
Described modified coal-tar obtains through following method: the mass ratio of pressing Mei Jiao You ︰ by-product oil=30～50 ︰ 40～50, after being mixed with by-product oil, coal tar obtains mixing oil, by the amount of 0.20～1L/min, in mixing oil, pass into technical grade hydrogen, and be that 350～460 ℃, pressure are that 0.1～5MPa, oil gas speed ratio are 0.1～3.0h in temperature
-1, catalyzer is γ-Al
2o
3, ZSM-5 molecular sieve condition under, reaction 3～15h, obtain modified coal-tar;
Described conditioning agent is the conditioning agent that aromatize degree BMCI is 30～75, for a kind of in following organism or by several composition the in following organism: crude benzol, toluene, heavy benzol, kerosene, diesel oil, ethylene glycol, propylene glycol, washing oil, carbolineum, de-aromatic solvent naphtha, wherein, described aromatize degree BMCI is calculated by following formula: BMCI=48640/Tb, m+473.6d-456.8
In formula, Tb, m is raw material boiling point mean value, unit is K; D is the density of raw material in the time of 288.5K, and unit is Kg/m
3;
B. be 50～200 ℃ by the raw material of steps A in temperature, under the condition that speed is 10～50mm/min, separate, obtain bottom isolate and top isolate;
C. B step is separated to the top isolate obtaining through centrifugation, obtain the solvent oil product on upper strata, and middle level thing and lower floor's thing;
D. bottom isolate step B being obtained remains at 120～250 ℃, by the mass ratio of bottom Fen Li Wu ︰ mixture=1 ︰ 0.01～0.5, mixture is passed in the isolate of bottom, at 220～300 ℃ of temperature, react 3～8h, obtain softening temperature and reach the intermediates of 230～260 ℃, wherein the volume ratio of mixture is: air: oxygen: carbolic oil=0.5～1.2: 0.25～1.2: 0.1;
E. be that 250～400 ℃, sieve aperture are to carry out heat screening under the condition of 50～1000 μ m by the middle level thing of step D in temperature, obtain the screen overflow of particle diameter > 50～1000 μ m, further pulverize this screen overflow and obtain fire bond, and the screen underflow of particle diameter < 50～1000 μ m is directly as fire bond.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310067646.7A CN103102165B (en) | 2011-08-29 | 2011-08-29 | Method for intensively producing refractory material through coal tar pitch needle coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310067646.7A CN103102165B (en) | 2011-08-29 | 2011-08-29 | Method for intensively producing refractory material through coal tar pitch needle coke |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110250879 Division CN102432306B (en) | 2011-08-29 | 2011-08-29 | Method for intensively producing refractory material binder by coal tar pitch needle coke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103102165A CN103102165A (en) | 2013-05-15 |
| CN103102165B true CN103102165B (en) | 2014-06-04 |
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| CN106589991A (en) * | 2016-12-08 | 2017-04-26 | 苏州艾博迈尔新材料有限公司 | High-performance epoxy asphalt and preparation technology thereof |
| CN114146725B (en) * | 2021-12-10 | 2023-07-18 | 南宁师范大学 | Acidic cobalt-based composite material and preparation method thereof |
| CN115505417A (en) * | 2022-09-20 | 2022-12-23 | 西安交通大学 | Pretreatment solvent for medium and low temperature coal tar, and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302431A (en) * | 2008-06-30 | 2008-11-12 | 邯郸市鑫宝煤化工有限公司 | Preparation of asphalt for producing coal-based needle coke |
| CN101508903A (en) * | 2009-03-20 | 2009-08-19 | 上海宝钢化工有限公司 | Process for continuously removing quinoline insoluble substances in coal tar pitch |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
| CN101787298A (en) * | 2009-01-23 | 2010-07-28 | 北京石油化工学院 | Coal art pitch purification method |
| CN102051191A (en) * | 2009-11-03 | 2011-05-11 | 上海宝钢化工有限公司 | Production method and system of coal-based needle coke |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302431A (en) * | 2008-06-30 | 2008-11-12 | 邯郸市鑫宝煤化工有限公司 | Preparation of asphalt for producing coal-based needle coke |
| CN101787298A (en) * | 2009-01-23 | 2010-07-28 | 北京石油化工学院 | Coal art pitch purification method |
| CN101508903A (en) * | 2009-03-20 | 2009-08-19 | 上海宝钢化工有限公司 | Process for continuously removing quinoline insoluble substances in coal tar pitch |
| CN102051191A (en) * | 2009-11-03 | 2011-05-11 | 上海宝钢化工有限公司 | Production method and system of coal-based needle coke |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
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