CN108977210A - A kind of preparation method of semi-coke - Google Patents
A kind of preparation method of semi-coke Download PDFInfo
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- CN108977210A CN108977210A CN201810865662.3A CN201810865662A CN108977210A CN 108977210 A CN108977210 A CN 108977210A CN 201810865662 A CN201810865662 A CN 201810865662A CN 108977210 A CN108977210 A CN 108977210A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
- C10B55/02—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material with solid materials
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention provides a kind of preparation methods of semi-coke.This method comprises: directly liquefying coal into oil residue used and clean fine coal are mixed, mixture is obtained；Mixture is subjected to pyrolytic reaction, obtains semi-coke.This method is to be prepared for semi-coke using directly liquefying coal into oil residue used and clean fine coal as raw material.By preparing semi-coke together with clean fine coal, harmless treatment can be carried out to directly liquefying coal into oil residue used, and make full use of the products characteristics of its high heating value, floorboard with high oil content.It, can industrially large-scale application moreover, semi-coke preparation method provided by the invention is easy to operate.
Description
Technical field
The present invention relates to the preparation fields of semi-coke, more particularly, to a kind of preparation method of semi-coke.
Background technique
Direct coal liquefaction technology is by high temperature, high pressure and to add hydrogen, is under the action of catalyst directly translated into solid coal
A kind of advanced clean coal technology of the clean liquid fuel that is readily transported and can be used or industrial chemicals.It is direct in coal
In liquefaction process, other than obtaining the liquid such as required gasoline, diesel oil, also creates and account for feed coal weight 20%-30%'s
Main By product directly liquefying coal into oil residue used.
Contain 50% unconverted coal, minerals in coal and catalyst for coal liquefaction, 20% weight in directly liquefying coal into oil residue used
Oil and 30% asphaltene, preasphaltene, total 0.2% or more arene content, calorific value is up to 7000 kilocalories or more.2015,
Directly liquefying coal into oil residue used is put into hazardous solid waste register, and transfer and disposition need to meet relevant law requirement.DCL/Direct coal liquefaction
The common treating method of the dregs of fat is blended with thermal coal, is used as heat power plant boiler fuel, ton product price generally exists
It is 240 yuan or so, low in economic efficiency.
Currently, the country has made some research work successively in the use aspects of directly liquefying coal into oil residue used.
CN200610012547.9, which is disclosed, makees road asphalt modifier and its application method with directly liquefying coal into oil residue used.This
The application method of kind of road asphalt modifier be directly liquefying coal into oil residue used is crushed to 100 mesh hereinafter, and pitch at 100-250 DEG C
Under by directly liquefying coal into oil residue used account for the weight ratio of modified pitch for 5-30% be uniformly mixed.
CN200510047800.X discloses one kind using directly liquefying coal into oil residue used as raw material, is prepared using arc-plasma
The method of nano carbon fiber material.This method is that the directly liquefying coal into oil residue used without any processing is placed in direct current-arc plasma
It is heat-treated in body torch, nitrogen is as electric arc working gas, under normal pressure, after 120~175 seconds, a nanometer Carbon fiber can be obtained
Material is tieed up, preparation process is without adding any catalyst.
Although both the above method thinking is preferable, large-scale industrialization to apply and wanted there are also many basic works
It does.How research carries out harmless treatment to the direct coal liquefaction dregs of fat, and makes full use of the product of its high heating value, floorboard with high oil content special
Point becomes a technical problem.
Summary of the invention
The main purpose of the present invention is to provide a kind of preparation methods of semi-coke, to solve DCL/Direct coal liquefaction in the prior art
The harmless treatment of slag can not industrialize the problem of large-scale application.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of preparation method of semi-coke, including will
Directly liquefying coal into oil residue used and clean fine coal mixing, obtain mixture, mixture are carried out pyrolytic reaction, obtains semi-coke.
Further, in mixture, the weight percent that directly liquefying coal into oil residue used accounts for mixture is greater than 0, is less than or equal to
30%.
Further, in mixture, the weight percent that directly liquefying coal into oil residue used accounts for mixture is 10~20%.
Further, the Ge-Jin Jiao type of clean fine coal is A type.
Further, partial size≤3mm of directly liquefying coal into oil residue used.
Further, partial size≤3mm of clean fine coal.
Further, pyrolysis reaction temperature is 800~900 DEG C, and the reaction time is 4~6h.
It further, further include that cooling absorb to obtain semi-coke is carried out to the product that reaction obtains after carrying out pyrolytic reaction
The step of；Preferably, burnt oil and gas has been obtained simultaneously during cooling absorption, after cooling the step of absorbing, also wrapped
Include the step of being separated the cooling product absorbed to obtain semi-coke, tar and coal gas.
Further, the cold source used during cooling absorption is coal gas.
Further, coal gas carries out foring heating gas after cooling absorb, and heating gas is back to pyrolytic reaction process
It is middle to be used as heat source for reaction.
Further, the 30~50% of coal gas participate in cooling absorption process as cold source.
Using the preparation method of semi-coke of the invention, this method is prepared using directly liquefying coal into oil residue used and clean fine coal as raw material
Semi-coke.By preparing semi-coke together with clean fine coal, harmless treatment can be carried out to directly liquefying coal into oil residue used, and make full use of
The products characteristics of its high heating value, floorboard with high oil content.Moreover, semi-coke preparation method provided by the invention is easy to operate, it can be in industry
Upper large-scale application.
Liquefaction heavy oil, the asphaltene, preceding pitch generated in directly liquefying coal into oil residue used containing a large amount of DCL/Direct coal liquefaction process
Alkene, and the heavy oil that liquefies, asphaltene, preasphaltene show high caking property in pyrolytic process, directly liquefying coal into oil residue used is viscous
It ties index and is up to 90 or more, thus mix refining directly liquefying coal into oil residue used in pyrolytic process to play the role of substituting coking coal.Especially
It is it should be noted that will participate in together pyrolytic reaction after directly liquefying coal into oil residue used and clean fine coal mixing in the present invention, in addition to energy
It enough efficiently uses other than the calorific value and oil in directly liquefying coal into oil residue used, cooperation clean fine coal, which also helps, prevents coal direct liquefaction oil
Slag is individually pyrolyzed the coking difficulty easily led to and the low problem of semi-coke quality.This is because, clean fine coal volatile matter is higher, ash content compared with
It is low, sulfur content is lower, and calorific value is higher, no adhesion, and cooperation directly liquefying coal into oil residue used carries out pyrolytic reaction, can reduce high temperature
The mobility and product ash content of lower directly liquefying coal into oil residue used, and then the semi-coke that can promote coking, and obtain has good product
Matter.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the process schematic representation of the preparation method of semi-coke according to an embodiment of the present invention.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
As described in background technology part, how research carries out harmless treatment to the direct coal liquefaction dregs of fat, and fills
Dividing becomes a technical problem using the products characteristics of its high heating value, floorboard with high oil content.
In order to solve this technical problem, the present invention provides a kind of preparation methods of semi-coke, as shown in Figure 1, this method
Include: to mix directly liquefying coal into oil residue used and clean fine coal, obtains mixture；Mixture is subjected to pyrolytic reaction, obtains semi-coke.Benefit
With the preparation method of semi-coke of the invention, harmless treatment can be carried out to directly liquefying coal into oil residue used.Contain in directly liquefying coal into oil residue used
Liquefaction heavy oil, the asphaltene, preasphaltene for thering is a large amount of DCL/Direct coal liquefaction process to generate, and the heavy oil that liquefies, asphaltene, preceding pitch
Alkene shows high caking property in pyrolytic process, and directly liquefying coal into oil residue used caking index is up to 90 or more, thus is being pyrolyzed
Mixing refining directly liquefying coal into oil residue used in the process can play the role of substituting coking coal.
Clean fine coal volatile matter is higher, ash content is lower, sulfur content is lower, and calorific value is higher, and softening temperature is higher, soap-free emulsion polymeization
Property, thus refining part clean fine coal is mixed in directly liquefying coal into oil residue used process of coking, directly liquefying coal into oil residue used under high temperature can be reduced
Mobility and product ash content.
In a preferred embodiment, in mixture, the weight percent that directly liquefying coal into oil residue used accounts for mixture is big
In 0, be less than or equal to 30%, it is preferable that in mixture, directly liquefying coal into oil residue used account for the weight percent of mixture be 10~
20%.Within the above range by the weight ratio control of directly liquefying coal into oil residue used in mixture, mixed material can be further decreased
Mobility at high temperature, it might even be possible to reach the state of no mobility, leaks to be beneficial to prevent raw material in pyrolytic process, into
One step improves production security.
In a preferred embodiment, the Ge-Jin Jiao type of clean fine coal is A type.A type clean fine coal volatile matter is higher, grey
It is point lower, sulfur content is lower, and calorific value is higher, no adhesion, using the type clean fine coal and directly liquefying coal into oil residue used into
Row pyrolytic reaction can further increase the quality of semi-coke.Directly liquefying coal into oil residue used under high temperature can also be further decreased simultaneously
Mobility, further to promote coking, and improve production security.
In order to further increase the efficiency of pyrolytic reaction, in a preferred embodiment, directly liquefying coal into oil residue used
Partial size≤3mm.Preferably, partial size≤3mm of clean fine coal.By the size controlling of directly liquefying coal into oil residue used and clean fine coal in above-mentioned model
In enclosing, the component of mixture can be made to disperse more uniform, and pyrolysis is more efficient, can further improve production efficiency.
In a preferred embodiment, pyrolysis reaction temperature is 800~900 DEG C, and the reaction time is 4~6h.At this
Pyrolytic reaction is more thorough under reaction condition.
It in a preferred embodiment, further include that the product obtained to reaction cools down after carrying out pyrolytic reaction
The step of absorbing to obtain semi-coke；Preferably, burnt oil and gas has been obtained simultaneously during cooling absorption, in cooling absorption
After step, further include the steps that separating to obtain semi-coke, tar and coal gas the cooling product absorbed.DCL/Direct coal liquefaction
A large amount of liquefaction heavy oil, the asphaltene, preasphaltene contained in the dregs of fat can be in high temperature pyrolysis reaction during high-temperature-coked
A large amount of coal gas and tar are released in the process.The processing step can make the separation and recovery coal gas generated during pyrolytic reaction and
On the one hand the harmless treatment degree of directly liquefying coal into oil residue used can be improved in tar product, on the other hand, coal gas and tar are also
The important source material of downstream chemical products production.
In a preferred embodiment, the cold source used during cooling absorption is coal gas.Preferably, such as Fig. 1
Shown, coal gas carries out foring heating gas after cooling absorb, and heating gas is back to during pyrolytic reaction and is used as reaction heat
Source uses, it is preferable that as shown in Figure 1, the 30~50% of coal gas participate in cooling absorption process as cold source.Such technique realizes
Heat sufficiently recycles, and greatly reduces production cost, while it is self-sufficient to realize technical process fuel.
Hereinafter beneficial effects of the present invention will be further illustrated by embodiment:
Directly liquefying coal into oil residue used property is shown in Table 1, and clean fine coal property is shown in Table 2.
1 directly liquefying coal into oil residue used property of table
2 clean fine coal property of table
Embodiment 1
(1) directly liquefying coal into oil residue used and clean fine coal are individually crushed and is sieved respectively, the powder that partial size is less than or equal to 3mm is made
End, it is spare.
(2) directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 15:85, mixing is equal
It is even, mixed raw material powder is made.
(3) mixed raw material powder is placed in rotary kiln, raw material is heated, be warming up to rotary kiln coke oven entrance temperature
Degree is 850 DEG C, and holding 5 hours to carry out pyrolytic reaction.
(4) after completion of the reaction, to reaction obtain liquid, gaseous products by cool down absorption technique obtain semi-coke, tar
And coal gas.
(5) the 40% of generated coal gas is used for as cold source the cooling absorption process of reaction product in step (4), coal
Gas forms heating gas after absorbing through supercooling, heating gas is back to during pyrolytic reaction, heat source is used as to use.
Table 3 to table 5 is the quality index of the pyrolysis product prepared in the present embodiment.
3 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 9.1 | 0.56 | 2.28 | 88.36 |
4 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.27 | 11.7 | 9.24 | 12.26 | 1.12 |
5 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 52.1 | 13.01 | 17.81 | 7.01 | 0.78 | 2.5 |
Embodiment 2
Preparation process is same as Example 1, the difference is that:
Directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 20:80 in step 2.
In step 3 to raw material carry out heat-treatment process in, rotary kiln coke oven inlet temperature be 800 DEG C, keep 6 hours with
Carry out pyrolytic reaction.
Table 6 to table 8 is the quality index of the pyrolysis product prepared in the present embodiment.
6 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 9.3 | 0.59 | 2.30 | 88.39 |
7 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.29 | 11.7 | 9.24 | 13.12 | 1.14 |
8 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 52.5 | 13.15 | 17.78 | 7.05 | 0.75 | 2.5 |
Embodiment 3
Preparation process is same as Example 1, the difference is that:
Directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 10:90 in step 2.
In step 3 to raw material carry out heat-treatment process in, rotary kiln coke oven inlet temperature be 900 DEG C, keep 4 hours with
Carry out pyrolytic reaction.
Table 9 to table 11 is the quality index of the pyrolysis product prepared in the present embodiment.
9 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 8.3 | 0.47 | 2.24 | 89.02 |
10 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.25 | 11.9 | 9.27 | 12.16 | 1.09 |
11 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 52.1 | 13.24 | 17.88 | 7.07 | 0.75 | 2.4 |
Embodiment 4
Preparation process is same as Example 1, the difference is that:
Directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 1:99 in step 2.
Table 12 to table 14 is the quality index of the pyrolysis product prepared in the present embodiment.
12 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 4.69 | 0.38 | 1.86 | 82.6 |
13 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.16 | 13.6 | 9.05 | 13.13 | 1.11 |
14 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 53.6 | 12.59 | 17.68 | 7.05 | 0.78 | 2.38 |
Embodiment 5
Preparation process is same as Example 1, the difference is that:
Directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 30:70 in step 2.
Table 15 to table 17 is the quality index of the pyrolysis product prepared in the present embodiment.
15 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 11.5 | 0.85 | 1.86 | 80.26 |
16 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.25 | 12.68 | 9.25 | 13.56 | 1.26 |
17 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 50.56 | 12.85 | 16.32 | 7.26 | 0.65 | 2.6 |
Embodiment 6
Preparation process is same as Example 1, the difference is that:
Directly liquefying coal into oil residue used powder and clean fine coal powder are mixed according to weight ratio 35:65 in step 2.
Table 18 to table 20 is the quality index of the pyrolysis product prepared in the present embodiment.
18 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 12.1 | 0.91 | 1.85 | 80.05 |
19 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.25 | 12.53 | 9.16 | 13.56 | 1.24 |
20 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 50.53 | 12.56 | 16.38 | 7.07 | 0.74 | 2.6 |
Comparative example 1
(1) powder that partial size is less than or equal to 3mm is made in clean fine coal, is placed in rotary kiln and is heated, is warming up to
Rotary kiln inlet temperature is 850 DEG C, and holding 5 hours to carry out pyrolytic reaction.
(2) after completion of the reaction, to reaction obtain liquid, gaseous products by cool down absorption technique obtain semi-coke, tar
And coal gas.
(3) the 40% of generated coal gas is used for as cold source the cooling absorption process of reaction product in step (2), coal
Gas forms heating gas after absorbing through supercooling, heating gas is back to during pyrolytic reaction, heat source is used as to use.
Table 21 to table 23 is the quality index of the pyrolysis product prepared in this comparative example.
21 coke quality index of table
Unit, % (mass fraction)
| Title | Ash content | Sulfur content | Volatile matter | Fixed carbon |
| Semi-coke | 4.65 | 0.35 | 1.86 | 82.8 |
22 quality of coke tar index of table
Unit, % (mass fraction)
| Title | Ash content | Naphthalene | Moisture | Toluene insolubles | Density |
| Tar | 0.16 | 13.6 | 9.05 | 13.13 | 1.11 |
23 gas quality index of table
Unit, % (mass fraction)
| Title | H2 | CO | CH4 | N2 | O2 | Hydro carbons |
| Coal gas | 53.6 | 12.59 | 17.68 | 7.05 | 0.78 | 2.38 |
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: in the present invention
It is mixed with semi-coke using directly liquefying coal into oil residue used and clean fine coal, harmless treatment, pyrolysis can be carried out to directly liquefying coal into oil residue used
The liquid that generates in reaction process, gaseous products are all recycled through supercooling absorption technique, fully meet coal direct liquefaction oil
The harmless treatment of slag.Meanwhile such technique realizes the abundant recycling of heat, the production cost substantially reduced realizes work
Fuel is self-sufficient during skill.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of semi-coke, which is characterized in that the preparation method comprises the following steps:
Directly liquefying coal into oil residue used and clean fine coal are mixed, mixture is obtained；
The mixture is subjected to pyrolytic reaction, obtains the semi-coke.
2. the method according to claim 1, wherein the directly liquefying coal into oil residue used accounts in the mixture
The weight percent of the mixture is greater than 0, is less than or equal to 30%.
3. according to the method described in claim 2, it is characterized in that, the directly liquefying coal into oil residue used accounts in the mixture
The weight percent of the mixture is 10~20%.
4. according to the method in any one of claims 1 to 3, which is characterized in that the Ge-Jin Jiao type of the clean fine coal is A
Type.
5. method according to claim 1 to 4, which is characterized in that the partial size of the directly liquefying coal into oil residue used
≤3mm；Preferably, partial size≤3mm of the clean fine coal.
6. according to the method described in claim 5, it is characterized in that, the pyrolysis reaction temperature is 800~900 DEG C, when reaction
Between be 4~6h.
7. according to the method described in claim 6, it is characterized in that, the method also includes right after carrying out the pyrolytic reaction
It reacts obtained product and carries out cooling the step of absorbing to obtain the semi-coke；
Preferably, burnt oil and gas has been obtained simultaneously during the cooling absorption, after described cooling the step of absorbing,
The method also includes being separated the cooling product absorbed to obtain the semi-coke, the tar and the coal gas
Step.
8. the method according to the description of claim 7 is characterized in that the cold source used during the cooling absorption is described
Coal gas.
9. according to the method described in claim 8, it is characterized in that, the coal gas carries out cooling absorb forms heat later
Coal gas, the method also includes: the heating gas is back to during the pyrolytic reaction, heat source for reaction is used as to use.
10. according to the method described in claim 8, it is characterized in that, the 30~50% of the coal gas are joined as the cold source
With the cooling absorption process.
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|---|---|---|---|---|
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| CN101514291A (en) * | 2009-02-27 | 2009-08-26 | 西安建筑科技大学 | Method for coke dry quenching by coal internal heat smouldering |
| CN102533373A (en) * | 2012-01-12 | 2012-07-04 | 锡林郭勒盟创源煤化工有限公司 | Method for using residue generated by directly liquefying coal |
| CN107189800A (en) * | 2017-07-03 | 2017-09-22 | 内蒙古广纳煤业（集团）有限责任公司 | A kind of coking process and products thereof and application |
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Application publication date: 20181211 |