CN100453621C - Method for producing high quality needle-type coke by improving coking process - Google Patents
Method for producing high quality needle-type coke by improving coking process Download PDFInfo
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- CN100453621C CN100453621C CNB200410082728XA CN200410082728A CN100453621C CN 100453621 C CN100453621 C CN 100453621C CN B200410082728X A CNB200410082728X A CN B200410082728XA CN 200410082728 A CN200410082728 A CN 200410082728A CN 100453621 C CN100453621 C CN 100453621C
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Abstract
The present invention relates to a method for preparing needle-shaped coke which has high quality by improving the coking technology. The present invention is characterized in that coal system raw materials or oil system raw materials are adopted; by any method for preprocessing raw materials, concentrated materials which have high purity are prepared as coking raw materials, the QI value needs to be less than 0.1%, and the materials are fed in a variable mode so that the generating capacity of oil steam is stabilized; the coking raw materials are firstly input, light oil is then input, and finally, superheated steam is input; through the three steps, a carbonization process and a solid phase drying process are completed; waste superheated steam is eliminated out of the system; after the oil steam is purified by a purifying device additionally arranged, the oil steam is fractionated. The high purity of the raw materials and circulation oil can be obtained. Therefore, needle-shaped coke which has high quality can be prepared, and the phenomenon of tower escape can be avoided.
Description
Technical field
The present invention relates to a kind of coking chemical technology, especially a kind of method of improving coking process production needle coke.
Background technology
Coal measures or oil are that the preparation method of needle coke is a lot, comprise that mostly raw material gives processing and coking processing etc.As the ZL86100675 patented technology, because solubilizing agent not adopts distillation upgrading method, technology is simpler, and raw material is wider, can obtain multiple joint product, and the quality of needle coke product has also improved, but only is secondary product (can only be used as the superpower electrode material); The ZL98114371.7 patented technology has been howed than ZL86100675 patented technology advanced person, raw material is given handling made many improvement, and coking process has also been made the innovation of " two-stage method operation ", and quality product is improved greatly.But also have some coking technology problems, have to be solved.Generally, in order to improve the quality of needle coke product, mostly be to improve raw material emphatically to give handling and produce the method for high purity fine fodder, and do not give due care coking process thereafter.If adopt general coking process, because technology is unreasonable, the impurity in the coking raw material is increased, influenced the needle coke quality product, also easily produce phenomenons such as string tower simultaneously.
Summary of the invention
In view of the problems referred to above that exist, the objective of the invention is in order to improve the quality of needle coke, further improve coking process, to guarantee that the impurity that raw material gives in the high purity fine fodder of handling the back acquisition no longer too increases, do not produce string tower phenomenon, can produce the up-to-standard needle coke of first grade (as the ultra-high power graphite electrode raw material).
In order to realize the object of the invention, the technical measures of taking are a kind of methods of improving coking process production needle coke of invention, adopting coal measures or oil is that raw material gives the high purity fine fodder that treatment process makes through any raw material, with it as coking raw material, after turning oil mixes, deliver to coking tower 2 with pump 11 heater vias 1 and carry out the coking processing, the needle coke that makes comes out under tower; The oily vapour that comes out on the tower enters separation column 4 through filter 5 and carries out fractionation, and the light oil that is fractionated into is gone out from tower top side line; The heavy oil that is fractionated into is gone out from tower middle part side line, through turning oil-self-cleaning oil interchanger 8 and self-cleaning oil heat exchange, sending into steam generator 7 again carries out after used heat utilizes, major part is back to separation column 4 middle parts, small portion is gone out through water cooler 9, some heavy oil is made turning oil and is mixed with coking raw material, and heater via 1 is delivered in the coking tower 2, proceeds coking and handles; The second coking tower 2B and the first coking tower 2A alternate operation; It is characterized in that:
1) weight percentage of quinoline insolubles in the coking raw material, promptly the QI value is not more than 0.1%;
2) on the oil steam pipe of coking tower 2 tops, be provided with automatic control flow instrument 13, in order to control oily vapour generating capacity, make coking raw material carry out the variable charging by the variable operating curve, at a tower in the cycle, when the raw material inlet amount begins by the upper limit amount charging of setting, progressively reduce then, before stopping charging 6-8 hour the time by the lower limit amount charging of setting, be stabilized to always and stop charging;
When 3) coking raw material enters coking tower 2 and carries out coking and handle, be that advanced coking raw material makes it the liquid phase charing; After raw material stops into, advance lightweight oil again, constant temperature 4-6 hour, make it to continue to finish carbonization process; Stop into lightweight oil, advance superheated vapour at last again, constant temperature or intensification 4-8 hour, make it to finish the solid phase drying process; Useless superheated vapour is taken away the impurity in the volatile matter outside tower is discharged to system;
4) in coking process, set up oily vapour refining plant: with in the separation column 4, the bottom is made as clean-up stage, coking raw material with purify after turning oil in mixing tank 3A, mix; Or between tower strainer 5 and separation column 4, establish a scavenging tower 3B, the bottom of separation column 4 is made as mixing section, coking raw material with purify after turning oil mix at this.
The tower top pressure of described coking tower 2 is 0-0.3mpa, and the liquid phase carbonization temperature is 450-510 ℃, and recycle ratio is 0.5-2.0.
The tower top temperature of described separation column 4 is 100-250 ℃, and pressure is 0-0.25mpa.
The tower top temperature of described scavenging tower 3 is 380-430 ℃.
Described self-cleaning oil adopts coking heavy oil or viscid bitumen or the mixing oil of the two.
The present invention improves the method that coking process is produced needle coke, its advantage following points: (1) because to the purity requirement height of coking raw material, and QI value＜0.1% (weight percentage) has so fundamentally guaranteed the quality of needle coke product.(2) in the prior art, because for preventing that scurrying tower squeezes into defoamer, has influenced the quality of coke.The present invention no longer adds defoamer, and coking raw material is to carry out the variable charging by the variable operating curve that oily vapour generating capacity is controlled, and has stablized oily steam flow amount, has prevented to scurry tower, has guaranteed the quality of needle coke product like this.(3) in the prior art, coking raw material carries out two-stage coking in coking tower, and advanced raw material makes it the liquid phase charing, and then advances lightweight oil, constant temperature or intensification 4-20 hour, makes it to continue to finish carbonization process and finish the solid phase drying process.Among the present invention, coking raw material carries out the segmentation coking in coking tower, advanced raw material makes it the liquid phase charing, advances lightweight oil again, constant temperature 4-6 hour, make it to continue to finish carbonization process, advance superheated vapo(u)r at last again, constant temperature or intensification 4-8 hour, make it to finish the solid phase drying process, useless superheated vapour outside the discharge system, is taken away the impurity in the volatile matter from tower, guaranteed quality product.(4) in the prior art, the a part of heavy oil that comes out from separation column reenters the coking tower coking as turning oil and coking raw material mixing, because burnt grain, coke powder impurity that oily vapour carries make the foreign matter content in the turning oil improve after the fractionation, influenced the purity of coking raw material so significantly.The present invention with in the separation column, the bottom is made as clean-up stage or sets up a scavenging tower before separation column, burnt grain, coke powder impurity that oily vapour is carried purify out, circulation heavy oil purity after the fractionation can be very high, in the composite mixing oil of coking raw material, the QI value reaches Schwellenwert, when sending into coking tower and carrying out coking and handle, just can guarantee to obtain the up-to-standard needle coke of first grade.
Description of drawings
Fig. 1 is embodiment 1 process flow sheet that the present invention " improves the method that coking process is produced needle coke ".
Fig. 2 is embodiment 2 process flow sheets that the present invention " improves the method that coking process is produced needle coke ".
In the accompanying drawing 1,1, well heater, 2A, first coking tower, 2B, second coking tower, 3A, mixing tank, 4, separation column (top fractionation section and bottom clean-up stage), 5, tower strainer, 6, self-cleaning oil-mixing oil interchanger, 7, steam generator, 8, turning oil-self-cleaning oil interchanger, 9, heavy oil water cooler, 10, purify oil pump, 11, mix oil pump, 12, circulating oil pump, 13, the automatic control flow instrument.
In the accompanying drawing 2,1, well heater, 2A, first coking tower, 2B, second coking tower, 3B, scavenging tower, 4, separation column (top fractionation section and bottom mixing section), 5, tower strainer, 6, self-cleaning oil-mixing oil interchanger, 7, steam generator, 8, turning oil-self-cleaning oil interchanger, 9, heavy oil water cooler, 10, purify oil pump, 11, mix oil pump, 12, circulating oil pump, 13, the automatic control flow instrument.
Embodiment
Embodiment 1
As shown in Figure 1, will with various give coal measures that treatment process makes or oil be the high purity fine fodder (QI value＜0.1 weight percentage〉as coking raw material, by automatic control flow instrument 13, variable operating curve charging by oily vapour generating capacity control, in mixing tank 3A, mix with turning oil, mixing oil is squeezed into self-cleaning oil-mixing oil interchanger 6 through pump 11, after the self-cleaning oil heat exchange, sending into coking tower 2 through well heater 1 again, is the upper limit amount charging to set during beginning, the variable operation, the lower limit amount charging to set 6-8 hour time the before stopping into, be stabilized to always and stop charging, guaranteed that the oily vapour generating capacity later stage can not the value of peaking, avoided scurrying tower.The tower top pressure of coking tower 2 is that 0-0.3mpa, recycle ratio are 0.5-2.5, and raw material carries out the liquid phase charing under 450-510 ℃ of temperature; After stopping into raw material, advance lightweight oil, constant temperature 4-6 hour, make material continue to finish carbonization process through pump 11, self-cleaning oil-mixing oil interchanger 6, well heater 1; After stopping into lightweight oil, enter superheated vapo(u)r again, constant temperature or intensification 6-8 hour, make material finish the solid phase drying process, useless superheated vapour outside the discharge system, is taken away the impurity in the volatile matter the qualified needle coke of tower bottom output quality from tower.Oily vapour on the tower is controlled the material feeding amount through automatic control flow instrument 13, removes big burnt grain through tower strainer 5, enter again separation column 4 in, the bottom clean-up stage, remove little burnt grain and coke powder impurity through purification.Oily vapour after the purification enters separation column 4 top fractionation sections again and carries out fractionation, its tower top temperature is 100-250 ℃, pressure is 0-0.25mpa, the light oil that fractionates out is discharged from tower top side line, heavy oil is discharged from tower middle part side line, squeeze into turning oil-self-cleaning oil interchanger 8 and self-cleaning oil heat exchange through pump 12, sending into steam generator 7 again carries out after used heat utilizes, major part is back to separation column 4 middle parts, small portion is gone out after water cooler 9 coolings, some heavy oil is in mixing tank 3A and after the coking raw material mixing, after self-cleaning oil-mixing oil interchanger 6 and self-cleaning oil heat exchange, heater via 1 enters coking tower 2 continuation coking again through pump 11.The second coking tower 2B and the first coking tower 2A alternate operation.
As shown in Figure 2, whole process flow is identical with embodiment 1, just sets up a scavenging tower 3B between tower strainer 5 and separation column 4, removes mixing tank 3A, and separation column 4 tops still are the fractionation section, and the bottom changes mixing section into.The oily vapour that coking tower 2 comes out above arrives first scavenging tower 3B and purifies behind automatic control flow instrument 13, tower strainer 5, carries out fractionation to the top fractionation section of separation column 4 again.Coking raw material be the bottom of separation column 4 mixing section with purify after turning oil mix.Its operating process is the same with embodiment 1 with principle, and only oily vapour purification is different with turning oil blended position with raw material.
Press operational condition and the technological process of embodiment 1, adopt viscid bitumen coal measures raw material, give facture through distillation and produce the high purity fine fodder as coking raw material, its QI value is 0, and softening temperature is 30 ℃ (ring and ball methods); Make QI value＜0.3% (weight percentage) of the mixing oil of coking raw material and turning oil; Self-cleaning oil adopts coking heavy oil and viscid bitumen; Produce out up-to-standard coal-based needle coke product as a trial, its performance index are:
Volatile matter V, (%) 0.56
Ash content A, (%) 0.06
Sulphur content S, (%) 0.18
True specific gravity, (g/ml) 2.2
Long-width ratio Km, 2.1
Thermal expansivity CTE, (* 10
-6/ ℃) 0.91 (100-600 ℃).
Claims (5)
1. one kind is improved the method that coking process is produced needle coke, adopting coal measures or oil is that raw material gives the high purity fine fodder that treatment process makes through any raw material, with it as coking raw material, after turning oil mixes, deliver to coking tower (2) with pump (11) heater via (1) and carry out the coking processing, the needle coke that makes comes out under tower; The oily vapour that comes out on the tower enters separation column (4) through filter (5) and carries out fractionation, and the light oil that is fractionated into is gone out from the top side line; The heavy oil that is fractionated into is gone out from tower middle part side line, through turning oil-self-cleaning oil interchanger (8) and self-cleaning oil heat exchange, sending into vapour generator (7) again carries out after used heat utilizes, major part is back to separation column (4) middle part, small portion is gone out through water cooler (9), some heavy oil is made turning oil and is mixed with coking raw material, and heater via (1) is delivered in the coking tower (2), proceeds coking and handles; Second coking tower (2B) and first coking tower (2A) alternate operation; It is characterized in that:
1) weight percentage of quinoline insolubles in the coking raw material, promptly the QI value is not more than 0.1%;
2) on the oil steam pipe of coking tower (2) top, be provided with automatic control flow instrument (13), in order to control oily vapour generating capacity, make coking raw material carry out the variable charging by the variable operating curve, at a tower in the cycle, when the raw material inlet amount begins by the upper limit amount charging of setting, progressively reduce then, before stopping charging 6-8 hour the time by the lower limit amount charging of setting, be stabilized to always and stop charging;
When 3) coking raw material enters coking tower (2) and carries out coking and handle, be that advanced coking raw material makes it the liquid phase charing; After raw material stops into, advance lightweight oil again, constant temperature 4-6 hour, make it to continue to finish carbonization process; After stopping into lightweight oil, advance superheated vapour at last again, constant temperature or intensification 4-8 hour, make it to finish the solid phase drying process; Useless superheated vapour is taken away the impurity in the volatile matter outside tower is discharged to system;
4) in coking process, set up oily vapour refining plant: with in the separation column (4), the bottom is made as clean-up stage, coking raw material with purify after turning oil in mixing tank (3A), mix; Or between tower strainer (5) and separation column (4), establish a scavenging tower (3B), the bottom of separation column (4) is made as mixing section, coking raw material with purify after turning oil mix at this.
2. improvement coking process according to claim 1 is produced the method for needle coke, and the tower top pressure that it is characterized in that coking tower (2) is 0-0.3mpa, and the liquid phase carbonization temperature is 450-510 ℃, and recycle ratio is 0.5-2.0.
3. improvement coking process according to claim 1 is produced the method for needle coke, and the tower top temperature that it is characterized in that separation column (4) is 100-250 ℃, and pressure is 0-0.25mpa.
4. improvement coking process according to claim 1 is produced the method for needle coke, and the tower top temperature that it is characterized in that scavenging tower (3B) is 380-430 ℃.
5. according to the method for claim 1 or 2 or 3 or 4 described improvement coking process production needle cokes, it is characterized in that self-cleaning oil adopts coking heavy oil or viscid bitumen or the mixing oil of the two.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410082728XA CN100453621C (en) | 2004-11-04 | 2004-11-04 | Method for producing high quality needle-type coke by improving coking process |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410082728XA CN100453621C (en) | 2004-11-04 | 2004-11-04 | Method for producing high quality needle-type coke by improving coking process |
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| CN1769373A CN1769373A (en) | 2006-05-10 |
| CN100453621C true CN100453621C (en) | 2009-01-21 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102436177B (en) * | 2011-10-24 | 2013-05-15 | 长春工业大学 | Automatic control device for multiple-effect water distillator |
| CN106635143B (en) * | 2015-11-02 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of method for preparing needle coke |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4104150A (en) * | 1974-07-17 | 1978-08-01 | Bergwerksverband Gmbh | Process for the production of coke from pitch |
| CN86100675A (en) * | 1986-01-20 | 1987-02-25 | 冶金部鞍山焦化耐火材料设计研究院 | A kind of novel preparation method of coal-based needle coke |
| CA1263848A (en) * | 1984-09-12 | 1989-12-12 | Tadashi Murakami | Process for the preparation of super needle coke |
-
2004
- 2004-11-04 CN CNB200410082728XA patent/CN100453621C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4104150A (en) * | 1974-07-17 | 1978-08-01 | Bergwerksverband Gmbh | Process for the production of coke from pitch |
| CA1263848A (en) * | 1984-09-12 | 1989-12-12 | Tadashi Murakami | Process for the preparation of super needle coke |
| CN86100675A (en) * | 1986-01-20 | 1987-02-25 | 冶金部鞍山焦化耐火材料设计研究院 | A kind of novel preparation method of coal-based needle coke |
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