CN106290448A - A kind of method of quickly evaluating needle coke heat stability - Google Patents
A kind of method of quickly evaluating needle coke heat stability Download PDFInfo
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- CN106290448A CN106290448A CN201610553017.9A CN201610553017A CN106290448A CN 106290448 A CN106290448 A CN 106290448A CN 201610553017 A CN201610553017 A CN 201610553017A CN 106290448 A CN106290448 A CN 106290448A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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Abstract
A kind of method that the invention discloses quickly evaluating needle coke heat stability, to carrying out spot test after needle-shape coke raw material heat treatment, raw material heat stability is judged according to spot test grade, the method provided by the present invention, the heat stability of needle-shape coke raw material can be judged in the short period of time, it is thus possible to the feasibility of certain raw material production needle coke of Fast Evaluation, and the formulation for preprocessing method of raw materials provides reliable basis；This inventive method is few for raw material dosage to be evaluated, simple to operate, time saving and energy saving, it is not necessary to expensive instrument and full-time staff, and without numerous and diverse analysis process.
Description
Technical field
The present invention relates to needle coke production field, particularly relate to the side of a kind of quickly evaluating needle coke heat stability
Method.
Background technology
Needle coke is the high-quality Carbon Materials that 20 century 70s are greatly developed, owing to having degree of crystallinity height, graphitization
The advantages such as performance is good, mechanical strength is high, thermal coefficient of expansion is low, thus can serve as ultra high power graphite electrode in metallurgical industry
Raw material.The industrial raw material that can be used to produce needle coke mainly has catalytic cracking clarified oil, black petroleum products, ethylene bottom oil, coal tar
Oil etc., can be divided into oil system needle coke and coal-based needle coke needle coke according to the difference of raw material sources, but no matter which kind of needle coke,
It all has certain requirement to raw material.It is said that in general, the ingredient requirement of needle coke (must not comprise condensed ring to divide greatly by arene content height
Sub-aromatic hydrocarbons), hetero atom (S, N, O) content is low, tenor is low, ash is low, asphalt content is low.In addition, needle coke is former
Material requires have in higher heat stability, i.e. raw material the dormancy fast reaction constituent content by thermal excitation low, thus is conducive to
Raw material keeps carbonization speed that will not be too fast in thermal conversion processes, and then forms preferably threadiness mesophase structure.At present
In commercial production, above-mentioned every conventional index can be obtained by raw material being carried out a series of analysis test, but to raw material
Heat stability does not also have existing evaluation methodology, it is therefore necessary to invent a kind of simple and easy to do evaluation needle-shape coke raw material thermally-stabilised
The method of property.
Summary of the invention
A kind of method that the invention aims to provide quickly evaluating needle coke heat stability, passes through the method
Can quickly judge the heat stability of needle-shape coke raw material, time saving and energy saving.
In order to reach above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of method of quickly evaluating needle coke heat stability, to carrying out speckle examination after needle-shape coke raw material heat treatment
Testing, judge raw material heat stability according to spot test grade, this spot test refers to Standard Test Method for
Cleanliness and Compatibility of Residual Fuels by Spot Test。
In order to generate bigger mesophasespherule in thermal conversion processes, needle-shape coke raw material have to have higher
Mesophase Transformation temperature and wider Mesophase Transformation temperature range, needle coke requires in raw material quick by the dormancy of thermal excitation
Reactive component content is low, thus beneficially raw material keep in thermal conversion processes will not be too fast carbonization speed, and then formed
Preferably threadiness mesophase structure.Such as directly heated by the above-mentioned heat treatment to raw material, can make in raw material that may be present
Thermally labile component under in a dormant state is occurred rapid condensation to react by thermal excitation, is susceptible to phase separation, so
Phenomenon of phase separation is i.e. can determine whether afterwards, such that it is able to evaluate the heat stability situation of raw material by spot test.
A kind of method of quickly evaluating needle coke heat stability, specifically comprises the following steps that
1) being placed in container by needle-shape coke raw material sample to be evaluated, container is placed in consersion unit；
2) consersion unit is placed in there is time of heating setpoint in the firing equipment setting reaction temperature；
3) in step 2) complete after, by container take out, take out reacted fluid sample, carry out spot test, according to speckle
Experimental tests grade determines needle-shape coke raw material heat stability.
Further, described consersion unit is minisize reaction still, and the volume of minisize reaction still is 10～50mL, described heating
Equipment is heating furnace.
Further, described step 1) in needle-shape coke raw material to be evaluated be oil system raw material, coal measures raw material or the mixing of the two
Raw material；
Preferably, oil system raw material is catalytic cracked oil pulp, black petroleum products or ethylene bottom oil etc., and coal measures raw material is coal tar
Or coal tar asphalt, the quality of raw material to be evaluated chooses 5～10g.
Further, described step 1) in after container is placed in consersion unit, by inert gas replacement consersion unit
Air；
Preferably, noble gas is nitrogen.
Further, in described consersion unit, the pressure of noble gas is 0.5～5MPa.
Further, the reaction temperature of described firing equipment is 450～500 DEG C, in this range of reaction temperature, can make
In needle-shape coke raw material that may be present in a dormant state under thermally labile component within the shortest time by thermal excitation
And occur rapid condensation to react, thus follow-up spot test.
Further, in order to realize quickly measuring, described step 2) response time is 5～15min.
Further, described heating furnace is tin bath stove or sand bath stove.
Further, spot test is carried out with reference to ASTM D4740-04 (2014) standard, according to spot test grade
The judgment principle determining described needle-shape coke raw material heat stability is: in raw material spot test grade to be evaluated 1 grade, 2 grades, 3 grades, 4
Level, 5 grades of its heat stability the most corresponding are the best, preferable, general, poor, excessively poor.
The invention has the beneficial effects as follows:
The method provided by the present invention, it is possible to judge the heat stability of needle-shape coke raw material in the short period of time, from
And can the feasibility of certain raw material production needle coke of Fast Evaluation, and provide for the formulation of preprocessing method of raw materials and reliably depend on
According to；This inventive method is few for raw material dosage to be evaluated, simple to operate, time saving and energy saving, it is not necessary to expensive instrument and full-time staff, and
Without numerous and diverse analysis process.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is carried out clear, complete description.
Embodiment 1
350-500 DEG C of distillate of 5g catalytic cracked oil pulp is placed in glass bushing pipe, and this glass bushing pipe is placed in 25mL
Minisize reaction still in, with nitrogen displacement still in air, be then pressurized to 2MPa.Minisize reaction still kettle is partially disposed in 450
DEG C tin bath stove in react 15min.Take out reacted sample, carry out speckle examination with reference to ASTM D4740-04 (2014) standard
Testing, recording its spot test grade is 3 grades, shows that this raw material heat stability is general, for meeting requirement, needs to process it
To improve heat stability.
Embodiment 2
350-500 DEG C of distillate of 5g catalytic cracked oil pulp is placed in glass bushing pipe, and this glass bushing pipe is placed in 25mL
Minisize reaction still in, with nitrogen displacement still in air, be then pressurized to 2MPa.Minisize reaction still kettle is partially disposed in 480
DEG C tin bath stove in react 10min.Take out reacted sample, carry out speckle examination with reference to ASTM D4740-04 (2014) standard
Testing, recording its spot test grade is 3 grades, shows that this raw material heat stability is general, for meeting requirement, needs to process it
To improve heat stability.
Embodiment 3
350-500 DEG C of distillate of 5g catalytic cracked oil pulp is placed in glass bushing pipe, and this glass bushing pipe is placed in 25mL
Minisize reaction still in, with nitrogen displacement still in air, be then pressurized to 2MPa.Minisize reaction still kettle is partially disposed in 500
DEG C tin bath stove in react 5min.Take out reacted sample, carry out speckle examination with reference to ASTM D4740-04 (2014) standard
Testing, recording its spot test grade is 3 grades, shows that this raw material heat stability is general, for meeting requirement, needs to process it
To improve heat stability.
Embodiment 4
350-500 DEG C of distillate of above-mentioned catalytic cracked oil pulp after being processed by 5g is placed in glass bushing pipe, and by this glass
Bushing pipe is placed in the minisize reaction still of 25mL, with air in nitrogen displacement still, is then pressurized to 2MPa.By minisize reaction still kettle
It is partially disposed in the tin bath stove of 450 DEG C reaction 15min.Take out reacted sample, with reference to ASTM D4740-04 (2014) standard
Carrying out spot test, recording its spot test grade is 1 grade, shows that this raw material heat stability is the best, meets needle-shape coke raw material
Requirement to heat stability.
Embodiment 5
350-500 DEG C of distillate of above-mentioned catalytic cracked oil pulp after being processed by 5g is placed in glass bushing pipe, and by this glass
Bushing pipe is placed in the minisize reaction still of 25mL, with air in nitrogen displacement still, is then pressurized to 2MPa.By minisize reaction still kettle
It is partially disposed in the tin bath stove of 480 DEG C reaction 10min.Take out reacted sample, with reference to ASTM D4740-04 (2014) standard
Carrying out spot test, recording its spot test grade is 1 grade, shows that this raw material heat stability is the best, meets needle-shape coke raw material
Requirement to heat stability.
Embodiment 6
350-500 DEG C of distillate of above-mentioned catalytic cracked oil pulp after being processed by 5g is placed in glass bushing pipe, and by this glass
Bushing pipe is placed in the minisize reaction still of 25mL, with air in nitrogen displacement still, is then pressurized to 2MPa.By minisize reaction still kettle
It is partially disposed in the tin bath stove of 500 DEG C reaction 5min.Take out reacted sample, with reference to ASTM D4740-04 (2014) standard
Carrying out spot test, recording its spot test grade is 1 grade, shows that this raw material heat stability is the best, meets needle-shape coke raw material
Requirement to heat stability.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. the method for a quickly evaluating needle coke heat stability, it is characterised in that laggard to needle-shape coke raw material heat treatment
Row spot test, judges raw material heat stability according to spot test grade.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 1, it is characterised in that specifically walk
Rapid as follows:
1) being placed in container by needle-shape coke raw material sample to be evaluated, container is placed in consersion unit；
2) consersion unit is placed in there is time of heating setpoint in the firing equipment setting reaction temperature；
3) in step 2) complete after, by container take out, take out reacted sample, carry out spot test, according to spot test etc.
Level determines needle-shape coke raw material heat stability.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that described instead
Answering equipment is minisize reaction still, and described firing equipment is heating furnace.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that described step
Rapid 1) in, needle-shape coke raw material to be evaluated is oil system raw material, coal measures raw material or the mixing raw material of the two；
Preferably, oil system raw material is catalytic cracked oil pulp, black petroleum products or ethylene bottom oil etc., and coal measures raw material is coal tar or coal tar
Oil asphalt.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that described step
Rapid 1) after in, container is placed in consersion unit, by the air in inert gas replacement consersion unit；
Preferably, noble gas is nitrogen.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 5, it is characterised in that described instead
Answering the pressure of noble gas in equipment is 0.5～5MPa.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that described in add
The reaction temperature of hot equipment is 450～500 DEG C.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that described step
Rapid 2) response time is 5～15min.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 3, it is characterised in that described in add
Hot stove is tin bath stove or sand bath stove.
The method of a kind of quickly evaluating needle coke heat stability the most as claimed in claim 2, it is characterised in that according to
Spot test grade determines that the judgment principle of described needle-shape coke raw material heat stability is: in raw material spot test grade to be evaluated 1
Level, 2 grades, 3 grades, 4 grades, 5 grades respectively its heat stability corresponding the best, preferable, general, poor, excessively poor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610553017.9A CN106290448A (en) | 2016-07-13 | 2016-07-13 | A kind of method of quickly evaluating needle coke heat stability |
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| CN201610553017.9A CN106290448A (en) | 2016-07-13 | 2016-07-13 | A kind of method of quickly evaluating needle coke heat stability |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109253943A (en) * | 2018-08-23 | 2019-01-22 | 辽宁科技大学 | The monitoring method of oil nature is mixed in a kind of coal-based needle coke production process |
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| CN101463266A (en) * | 2007-12-21 | 2009-06-24 | 中国石油化工股份有限公司 | Viscosity breaking method |
| CN102504862A (en) * | 2011-11-18 | 2012-06-20 | 中国石油天然气股份有限公司 | Hydrogen-donating thermal cracking method |
| CN103760053B (en) * | 2014-01-15 | 2016-04-27 | 中钢集团鞍山热能研究院有限公司 | A kind of raw material evaluation method instructing needle coke coking production |
-
2016
- 2016-07-13 CN CN201610553017.9A patent/CN106290448A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101463266A (en) * | 2007-12-21 | 2009-06-24 | 中国石油化工股份有限公司 | Viscosity breaking method |
| CN102504862A (en) * | 2011-11-18 | 2012-06-20 | 中国石油天然气股份有限公司 | Hydrogen-donating thermal cracking method |
| CN103760053B (en) * | 2014-01-15 | 2016-04-27 | 中钢集团鞍山热能研究院有限公司 | A kind of raw material evaluation method instructing needle coke coking production |
Non-Patent Citations (2)
| Title |
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| 李凤绪: "委内瑞拉重油受热氢转移能力及供氢改质特性研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 王永刚，周国江主编: "《煤化工工艺学》", 30 September 2014, 中国矿业大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109253943A (en) * | 2018-08-23 | 2019-01-22 | 辽宁科技大学 | The monitoring method of oil nature is mixed in a kind of coal-based needle coke production process |
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