CN105018124A - Coal tar waste-residue extraction separation method - Google Patents
Coal tar waste-residue extraction separation method Download PDFInfo
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- CN105018124A CN105018124A CN201510414383.1A CN201510414383A CN105018124A CN 105018124 A CN105018124 A CN 105018124A CN 201510414383 A CN201510414383 A CN 201510414383A CN 105018124 A CN105018124 A CN 105018124A
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Abstract
The invention relates to a coal tar waste-residue extraction separation method. The invention aims to solve technical problems such as secondary environmental pollution, expensive extractant, high operation cost and complex process in an existing solvent extraction separation method of coal tar waste-residues. According to the technical scheme, at normal temperature and atmospheric pressure, a composite extractant composed of furaldehyde and an esters solvent is used to separate solid residues such as tar and coal dust, coke powder and the like in coal tar waste-residues through steps of extraction, separation, distillation, washing and the like. During the extraction process, use amount of the composite extractant is 1-3 times larger than mass of the coal tar waste-residues. The components of the composite extractant are cheap and easily available and are both low-toxic. The composite extractant has high separation efficiency. The whole extraction separation operational process is carried out under the condition of normal temperature and atmospheric pressure. The technological process is simple, and energy consumption and operational cost are low.
Description
Technical field
The present invention relates to a kind of coal tar waste residue extraction separating method, particularly one at normal temperatures and pressures, utilize the composite extractant of furfural and esters solvent composition, through steps such as extraction, separation, distillation and washings, by the method for coal-tar middle oil for the coal-tar residue a kind of coal tar waste residue extracting and separating be separated with the solid slag such as coal dust, coke powder.
Background technology
Coal tar waste residue is coal in gasification and coking, and the coal dust, solia particle etc. carried secretly when the high boiling point organic compound generated under the high temperature conditions is condensed and in coal gas are mixed in together and a kind of industrial residue of being formed.Containing a large amount of fixed carbon and organic volatile in coal tar waste residue, calorific value, at about 8000kcal/kg, is a kind of useful secondary energy.But current most enterprise fails recycle well a large amount of coal tar waste residue produced in production process and utilize, but it is arbitrarily stacked or abandon it.In the course of time, a large amount of coal tar waste residues not only takies a large amount of vacant lot and brings burden to enterprise, and coal tar waste residue also because of rainwash, can cause severe contamination to surrounding environment and underground water.In addition, in coal tar waste residue, the effusion of fugitive constituent also makes ambient air suffer severe contamination.Therefore, coal tar waste residue being carried out disposal and utilization effectively, make it to turn harm into good, turn waste into wealth, is the optimal path solving coal tar waste residue.
In recent years, particularly domestic scholars has carried out the research to coal tar Solid state fermentation technology both at home and abroad.Wherein, adopt solvent-extracted method can isolate coal tar and coal dust, coke powder etc. from coal tar waste residue, the maximum resourceization achieving coal tar waste residue utilizes, and is therefore one more promising coal tar waste residue utilization technique.
Publication number is that CN101629086A discloses one " coal-tar solvent extraction process ", and its technique composition comprises separation, extracting, distillation, and it is 45 ~ 55 DEG C that the method dissolves whipping temp, and distillation temperature is 140 ~ 150 DEG C.The extraction solvent taked is Coal Chemical Industry petroleum naphtha, and its composition comprises aromatic hydrocarbons, alkane, naphthalene, indenes, cumarone etc.The deficiency of the method is, because the aromatic hydrocarbons that contains in Coal Chemical Industry petroleum naphtha and polycyclic aromatic hydrocarbons are up to more than 47%, and sulphur content is higher, and smell is comparatively large, and thus extraction agent toxicity is high, and treatment process easily causes secondary environmental pollution.In addition, in the method extraction temperature and solvent distillation temperature all higher, add the consumption of energy and the complicacy of method.
Publication number is that CN103059894A discloses " a kind of method of the coal carbonaceous residues extracting and separating based on ionic liquid ".The method is for extraction agent with pyridine and ammonium class ionic liquid, under 20 ~ 120 DEG C and 1 ~ 50atm, through extraction and back-extraction two step, be separated the asphaltene class material in carbonaceous residues, preparing mesophase pitch for modification and then produce high performance carbon cellulosic material provides high quality raw material.The deficiency of the method is, the extraction agent adopted is pyridine or ammonium class ionic liquid, and its price is relatively costly, and this technology needs to carry out under certain temperature and pressure condition, processing cost is increased, complex technical process.
Publication number is that CN101817935A discloses a kind of reclaimed rubber plasticizer and preparation method, carbolineum is selected to be separated with coke powder by the coal tar in coke tar refuse as extraction agent in method, the coal tar obtained containing naphthalene is lower is prepared into reclaimed rubber plasticizer, for smelting iron use after the coke powder extrusion molding sintering of by-product.The deficiency of the method is, the extraction agent adopted is carbolineum, and its main constituent has the polycyclic aromatic hydrocarbons of the contour poison of anthracene, phenanthrene, fluorenes, acenaphthene, carbazole, have intense stimulus, and boiling range is higher, reaches 280 ~ 360 DEG C, if reclaim carbolineum, a large amount of energy will certainly be consumed.
In the above prior art, carry out to coal tar waste residue extraction agent ubiquity that extracting and separating adopts and that extraction solvent toxicity is large and/or boiling point is higher, recovered energy consumption is large and/or cost is higher.Therefore, find a kind of cheap, low toxicity and the simple extraction agent of lock out operation, and at normal temperatures and pressures extracting and separating is carried out to coal tar waste residue, it is that current coal chemical industry needs technical solution problem that the method realizing environment-friendly and green safety carries out effectively process to existing a large amount of coal tar waste residue.
Summary of the invention
The concrete technical problems that the present invention will solve seeks a kind of cheap, low toxicity and the simple extraction agent of lock out operation, and carry out extracting and separating to coal tar waste residue at normal temperatures and pressures, and then provide a kind of method of coal tar waste residue extracting and separating.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of coal tar waste residue extraction separating method, extraction separating method described in it carries out extracting and separating to coal tar waste residue at normal temperatures and pressures based on a kind of furfural ester class composite extractant;
Describedly follow these steps to carry out to the method that coal tar waste residue carries out extracting and separating at normal temperatures and pressures:
(1) at normal temperatures and pressures, the ratio being 1: 1 ~ 3 in mass ratio by coal tar waste residue and composite extractant is placed in extraction tank and mixes, and obtains mixture;
(2) at normal temperatures and pressures, the mixture in above-mentioned steps (1) is stirred, churning time 0.5 ~ 2.0h, rear standing 0.5 ~ 1.0h, then send into separating device and be separated, obtain mixing solutions and solid slag;
(3) mixing solutions obtained after above-mentioned steps (2) is separated is placed in retort, is heated to boiling and fractionation by distillation, obtains composite extractant and tar, and composite extractant is recycled, and tar sends into tar tank;
(4) be separated the solid slag obtained through above-mentioned steps (2), again carry out secondary by the composite extractant reclaimed in composite extractant or above-mentioned steps (3) and embathe, be separated, obtain mixing solutions and solid slag;
(5) repeat above-mentioned steps (4) secondary to three times, obtain tar and solid slag.
The composition of described furfural esters extractant and content thereof are furfural 5 ~ 20% by volume, esters solvent 80 ~ 95% mixes, and obtain composite extractant;
Further additional technical feature is as follows.
Composition and the content thereof of described furfural ester class composite extractant are furfural 12%, esters solvent 88% by volume further.
Described coal tar waste residue and extraction agent are 1: 3 in mass ratio further.
When the composition of described furfural esters extractant and content thereof are furfural 18%, esters solvent 82% by volume, coal tar waste residue and extraction agent are 1: 2.5 in mass ratio.
Esters solvent in described composite extractant is one or more the mixing in methyl acetate, ethyl acetate and isopropyl acetate.
Described coal tar waste residue is the coal tar waste residue of coke-oven plant's generation and/or the coal tar waste residue of coal gasification course generation.
Described acquisition tar and solid slag are respectively 20% ~ 50% and 30% ~ 65%.
Implement a kind of method of coal tar waste residue extracting and separating that the invention described above provides, compared with prior art, its advantage and positively effect as follows.
First, the solvent composition of preparation needed for composite extractant is cheap and easy to get, and all belongs to low toxicity, reduces the risk that secondary environmental pollution occurs; Secondly, whole extracting and separating operating process carries out under normal temperature and pressure conditions, and energy consumption is low, and technological process is simple, and operating process can realize continuous prodution, and overall operation cost is low.Finally, adopt the inventive method to coal tar waste residue separating treatment, separation efficiency can reach more than 99%.
The solvent toxicity that the method for existing solvent extraction and separation coal tar waste residue exists greatly, easily causes that secondary environmental pollution, extraction agent are expensive, running cost is high, the technical problem of complex technical process, the invention provides a kind of composite extractant of cheap, low toxicity, further provide the method for a kind of lock out operation simple coal tar waste residue extracting and separating, thus tar, coal dust or coke powder wherein can be reclaimed economical, efficiently.
Accompanying drawing explanation
Fig. 1 is the schema of extraction separating method of the present invention.
subordinate list explanation
Table 1 is the present invention's coal tar waste residue composition used.
Embodiment
And describe the present invention in detail below with reference to the accompanying drawings in conjunction with the embodiments.It should be noted that, when not conflicting, the feature in following examples and embodiment can combine mutually.
Implement a kind of coal tar waste residue extraction separating method, the composition of described coal tar waste residue and content thereof are as following table 1:
Table 1
Embodiment 1
At normal temperatures and pressures, furfural, methyl acetate are followed successively by 5% and 95% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue J1 this composite extractant and coke-oven plant produced is that 1:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 0.5h is stirred to above mixture, leave standstill 0.5h, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.6% of integrated solid slag weight.
Embodiment 2
At normal temperatures and pressures, furfural, ethyl acetate are followed successively by 12% and 88% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue J2 this composite extractant and coke-oven plant produced is that 2:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 40min is stirred to above mixture, leave standstill 0.5h, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.22% of integrated solid slag weight.
Embodiment 3
At normal temperatures and pressures, furfural, ethyl acetate and methyl acetate are followed successively by 12%, 58%, 30% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue Q1 this composite extractant and coal gasification course produced is that 2.5:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 50min is stirred to above mixture, leave standstill 1h, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.2% of integrated solid slag weight.
Embodiment 4
At normal temperatures and pressures, furfural, isopropyl acetate are followed successively by 18% and 82% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue Q1 this composite extractant and coal gasification course produced is that 2.5:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 30min is stirred to above mixture, leave standstill 1h, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.13% of integrated solid slag weight.
Embodiment 5
At normal temperatures and pressures, furfural, isopropyl acetate and ethyl acetate are followed successively by 18%, 50%, 32% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue J3 this composite extractant and coke-oven plant produced is that 2.5:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 30min is stirred to above mixture, leave standstill 1h, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.16% of integrated solid slag weight.
Embodiment 6
At normal temperatures and pressures, furfural, isopropyl acetate and methyl acetate are followed successively by 20%, 50%, 30% according to volume percent and are mixed with furfural ester class composite extractant, then the coal tar waste residue Q1 this composite extractant and coal gasification course produced is that 3:1 mixes in extraction tank according to mass ratio, obtains mixture; Under the condition of normal temperature and pressure, fully 50min is stirred to above mixture, leave standstill 40 min, then send into separating device and be separated, obtain mixing solutions and solid slag; Be placed in retort by being separated the mixing solutions obtained, be heated to boiling and fractionation by distillation, obtain composite extractant and tar, composite extractant is recycled, and tar sends into tar tank; Be separated the solid slag obtained, again carry out secondary by the composite extractant reclaimed in composite extractant or above step and embathe, be separated, obtain mixing solutions and solid slag; Isolated solid slag carries out third time extraction again.In solid slag after three extracting and separating, contained tar component accounts for 0.25% of integrated solid slag weight.
The above embodiment just better understands the present invention to enable those skilled in the art to; but be not that the present invention is imposed any restrictions; to those skilled in the art; the present invention can have various conversion and replacement; the any amendment made under all principles in embodiment described in the inventive method and spirit, equivalent replacement, improvement etc., all belong to protection scope of the present invention.
Claims (8)
1. a coal tar waste residue extraction separating method, is characterized in that:
Described extraction separating method carries out extracting and separating to coal tar waste residue at normal temperatures and pressures based on a kind of furfural ester class composite extractant;
Described coal tar waste residue is the coal tar waste residue of coke-oven plant's generation and the coal tar waste residue of coal gasification course generation, and its composition and content thereof are respectively as following table 1:
Table 1
Describedly follow these steps to carry out to the method that coal tar waste residue carries out extracting and separating at normal temperatures and pressures:
(1) at normal temperatures and pressures, the ratio being 1: 1 ~ 3 in mass ratio by coal tar waste residue and composite extractant is placed in extraction tank and mixes, and obtains mixture;
(2) at normal temperatures and pressures, the mixture in above-mentioned steps (1) is stirred, churning time 0.5 ~ 2.0h, rear standing 0.5 ~ 1.0h, then send into separating device and be separated, obtain mixing solutions and solid slag;
(3) mixing solutions obtained after above-mentioned steps (2) is separated is placed in retort, is heated to boiling and fractionation by distillation, obtains composite extractant and tar, and composite extractant is recycled, and tar sends into tar tank;
(4) be separated the solid slag obtained through above-mentioned steps (2), again carry out secondary by the composite extractant reclaimed in composite extractant or above-mentioned steps (3) and embathe, be separated, obtain mixing solutions and solid slag;
(5) repeat above-mentioned steps (4) secondary to three times, obtain tar and solid slag.
2. the composition of furfural esters extractant described in and content thereof are furfural 5 ~ 20% by volume, esters solvent 80 ~ 95% mixes, and obtain composite extractant.
3. method according to claim 1, the composition of furfural esters extractant described in it and content thereof are furfural 12%, esters solvent 88% by volume further.
4. method according to claim 1, coal tar waste residue and extraction agent described in it are 1: 3 in mass ratio further.
5. method according to claim 1 and 2, when the composition of furfural esters extractant described in it and content thereof are furfural 18%, esters solvent 82% by volume, coal tar waste residue and extraction agent are 1: 2.5 in mass ratio.
6. method according to claim 1, the esters solvent in composite extractant described in it is one or more the mixing in methyl acetate, ethyl acetate and isopropyl acetate.
7. method according to claim 1, coal tar waste residue described in it is the coal tar waste residue of coke-oven plant's generation and/or the coal tar waste residue of coal gasification course generation, and the composition of coal tar waste residue used sees attached list 1.
8. method according to claim 1, obtains tar described in it and solid slag is respectively 20% ~ 50% and 30% ~ 65%.
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| CN107854861A (en) * | 2017-12-04 | 2018-03-30 | 太原理工大学 | A kind of method of the extract and separate of organic matter in coal carbonaceous residues |
| CN110358564A (en) * | 2019-07-15 | 2019-10-22 | 延安大学 | A kind of coal-tar residue separator and separation method |
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| CN110358564A (en) * | 2019-07-15 | 2019-10-22 | 延安大学 | A kind of coal-tar residue separator and separation method |
| CN114032115A (en) * | 2021-02-03 | 2022-02-11 | 海通久卓环保科技有限公司 | Resource recovery method of waste coal tar |
| CN114032115B (en) * | 2021-02-03 | 2024-01-16 | 臧正军 | Recycling recovery method of waste coal tar |
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