CN105018124B - A kind of coal tar waste residue extraction separating method - Google Patents
A kind of coal tar waste residue extraction separating method Download PDFInfo
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- CN105018124B CN105018124B CN201510414383.1A CN201510414383A CN105018124B CN 105018124 B CN105018124 B CN 105018124B CN 201510414383 A CN201510414383 A CN 201510414383A CN 105018124 B CN105018124 B CN 105018124B
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- waste residue
- coal tar
- composite extractant
- solid slag
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Abstract
The present invention relates to a kind of method of coal tar waste residue extract and separate.Present invention aim to address being easily caused present in the method for existing solvent extraction and separation coal tar waste residue, secondary environmental pollution, extractant are expensive, operating cost is high, complex technical process technical problem.The technical solution adopted by the present invention is, at normal temperatures and pressures, utilize the composite extractant being made up of furfural and esters solvent, by steps such as extraction, separation, distillation and washings, by the separation of the solid slags such as the tar and coal dust in coal tar waste residue, coke powder, in extraction process, the consumption of the composite extractant is 1~3 times of the quality of the coal tar waste residue.Composite extractant composition of the present invention is cheap and easy to get, and low toxicity, and separative efficiency is high, and whole extract and separate operating process is carried out under normal temperature and pressure conditionses, and technical process is simple, and energy consumption and operating cost are low.
Description
Technical field
The present invention relates to a kind of coal tar waste residue extraction separating method, particularly one kind at normal temperatures and pressures, utilizes furfural
The composite extractant constituted with esters solvent, by steps such as extraction, separation, distillation and washings, by tar in coal-tar residue and
A kind of method of coal tar waste residue extract and separate of the solid slags such as coal dust, coke powder separation.
Background technology
Coal tar waste residue be coal in gasification and coking, the higher boiling organic compound quilt generated under the high temperature conditions
A kind of industrial residue formed by coal dust, the solia particle carried secretly during condensation and in coal gas etc. is mixed in together.Coal tar waste residue
In contain substantial amounts of fixed carbon and organic volatile, calorific capacity, in 8000kcal/kg or so, is a kind of useful secondary energy sources.
However, majority enterprise fails to carry out recycling well and profit to the substantial amounts of coal tar waste residue produced in production process at present
With, but it is arbitrarily stacked or abandons it.In the course of time, substantial amounts of coal tar waste residue not only takes substantial amounts of vacant lot and gives enterprise's band
To bear, and coal tar waste residue can also cause severe contamination because of rainwash to surrounding environment and underground water.In addition, coal
The effusion of fugitive constituent also makes surrounding air suffer severe contamination in coke tar waste slag.Therefore, coal tar waste residue is effectively located in
Reason and utilization, are allowed to turn harm into good, turn waste into wealth, and are the optimal paths for solving coal tar waste residue.
In recent years, particularly domestic scholars have carried out the research to coal tar Solid state fermentation technology both at home and abroad.Wherein, use
Solvent-extracted method can isolate coal tar and coal dust, coke powder etc. from coal tar waste residue, realize coal tar waste residue most
Large resourceization is utilized, therefore is a kind of more promising coal tar waste residue utilization technique.
Publication No. CN101629086A is disclosed a kind of " coal-tar solvent extraction process ", and its technique composition includes dividing
From, extracting, distillation, this method dissolving whipping temp be 45~55 DEG C, vapo(u)rizing temperature be 140~150 DEG C.The extraction taken is molten
Agent is coal chemical industry naphtha, and its composition includes aromatic hydrocarbons, alkane, naphthalene, indenes, benzofuran etc..The deficiency of this method is, due to coalification
The aromatic hydrocarbons and polycyclic aromatic hydrocarbon contained in work naphtha is up to more than 47%, and sulfur content is higher, and smell is larger, thus extractant poison
Property it is high, handling process easily causes secondary environmental pollution.In addition, extraction temperature and solvent vapo(u)rizing temperature are higher in this method, increase
The consumption of energy and the complexity of method are added.
Publication No. CN103059894A discloses a kind of " side of the coal carbonaceous residues extract and separate based on ionic liquid
Method ".This method is using pyridine and ammonium class ionic liquid as extractant, under 20 ~ 120 DEG C and 1 ~ 50atm, through extracting and being stripped two
Pitch alkenes material in step, separation carbonaceous residues, is carried to be modified to prepare mesophase pitch and then produce high performance carbon cellulosic material
For quality raw materials.The deficiency of this method be the extractant used for pyridine or ammonium class ionic liquid, its price is relatively expensive,
And the technology needs to carry out under the conditions of certain temperature and pressure so that processing cost increase, complex technical process.
Publication No. CN101817935A, which is disclosed, selects carbolineum in a kind of reclaimed rubber plasticizer and preparation method, method
The coal tar in tar slag and coke blacking are separated as extractant, the lower coal tar containing naphthalene is obtained and is prepared into reclaimed rubber increasing
Agent is moulded, the coke powder extrusion forming of by-product is used after sintering for ironmaking.The deficiency of this method is the extractant used for anthracene
Oil, its main constituent has the polycyclic aromatic hydrocarbon of the high poisons such as anthracene, phenanthrene, fluorenes, acenaphthene, carbazole, there is intense irritation, and boiling range is higher, reaches
280 ~ 360 DEG C, if being reclaimed to carbolineum, substantial amounts of energy will certainly be consumed.
In the above prior art, extraction to the extractant generally existing that coal tar waste residue progress extract and separate is used
Solvent toxicity is big and/or boiling point is higher, and the consumption that recovers energy is big and/or cost is higher.Therefore, find a kind of cheap, low
Poison and the simple extractant of lock out operation, and extract and separate is carried out to coal tar waste residue at normal temperatures and pressures, realize environment-friendly and green
It is that current coal chemical industry needs to solve technical problem that the method for safety is effectively treated to existing substantial amounts of coal tar waste residue.
The content of the invention
The invention solves the problems that concrete technical problems be to seek a kind of cheap, low toxicity and lock out operation is simply extracted
Agent, and extract and separate is carried out to coal tar waste residue at normal temperatures and pressures, and then a kind of side of coal tar waste residue extract and separate is provided
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of coal tar waste residue extraction separating method, its described extraction separating method is based on a kind of compound extraction of furfural esters
Agent is taken to carry out extract and separate to coal tar waste residue at normal temperatures and pressures；
It is described the method that coal tar waste residue carries out extract and separate to be followed these steps to carry out at normal temperatures and pressures：
（1）At normal temperatures and pressures, coal tar waste residue and composite extractant are placed in extraction for 1: 1 ~ 3 ratio in mass ratio
Mixed in groove, obtain mixture；
（2）At normal temperatures and pressures, to above-mentioned steps（1）In mixture be stirred, 0.5~2.0h of mixing time, after
0.5~1.0h is stood, separation equipment is then fed into and is separated, mixed solution and solid slag is obtained；
（3）Through above-mentioned steps（2）The mixed solution obtained after separation is placed in alembic, is heated to seething with excitement and is distilled point
From acquisition composite extractant and tar, composite extractant are recycled, tar feeding tar tank；
（4）Through above-mentioned steps（2）The solid slag obtained is separated, again by composite extractant or above-mentioned steps（3）In return
The composite extractant progress of receipts is secondary to embathe, and separates, obtains mixed solution and solid slag；
（5）Repeat the above steps（4）Secondary to three times, obtain tar and solid slag.
The composition and its content of the furfural esters extractant are furfural 5~20%, esters solvent 80~95% by volume
Mixed, obtain composite extractant；
Further additional technical feature is as follows.
The composition and its content of the furfural esters composite extractant are further furfural 12%, esters solvent by volume
88%。
The coal tar waste residue is further 1: 3 in mass ratio with extractant.
When the composition and its content of the furfural esters extractant are furfural 18%, esters solvent 82% by volume, coal tar
Oily waste residue is 1: 2.5 in mass ratio with extractant.
Esters solvent in the composite extractant is one kind or many in methyl acetate, ethyl acetate and isopropyl acetate
The mixing planted.
The coal tar waste residue is that the coal tar that the coal tar waste residue and/or coal gasification course that coke-oven plant is produced are produced gives up
Slag.
The acquisition tar and solid slag are respectively 20% ~ 50% and 30% ~ 65%.
Implement a kind of method for coal tar waste residue extract and separate that the invention described above is provided, compared with prior art, its
Advantage is as follows with good effect.
First, the solvent composition needed for preparing composite extractant is cheap and easy to get, and belongs to low toxicity, reduces two secondary rings of generation
The risk of border pollution；Secondly, whole extract and separate operating process is carried out under normal temperature and pressure conditionses, and energy consumption is low, technical process
Simply, operating process can realize continuous production, and overall operation cost is low.Finally, using the inventive method to coal tar waste residue
Separating treatment, separative efficiency is up to more than 99%.
Solvent toxicity that the method for existing solvent extraction and separation coal tar waste residue is present is big, easily cause secondary environmental pollution,
Extractant is expensive, operating cost is high, complex technical process technical problem, and the invention provides one kind is cheap, low
A kind of composite extractant of poison, it is further provided method of the simple coal tar waste residue extract and separate of lock out operation, so as to
It is economical, efficiently reclaim tar therein, coal dust or coke powder.
Brief description of the drawings
Fig. 1 is the flow chart of extraction separating method of the present invention.
Subordinate list explanation
Table 1 is that coal tar waste residue used in the present invention is constituted.
Embodiment
Below with reference to the accompanying drawings the present invention is described in detail and in conjunction with the embodiments.It should be noted that in situation about not conflicting
Under, the feature in following examples and embodiment can be mutually combined.
Implement a kind of coal tar waste residue extraction separating method, the composition and its content such as table 1 below of the coal tar waste residue：
Table 1
Embodiment 1
At normal temperatures and pressures, furfural, methyl acetate are followed successively by 5% and 95% according to percent by volume and are configured to furfural esters
Composite extractant, the coal tar waste residue J1 for then producing the composite extractant and coke-oven plant is 1 according to mass ratio:1 in extraction
Mixed in groove, obtain mixture；Under conditions of normal temperature and pressure, thing mixed above is carried out to be sufficiently stirred for 0.5h, 0.5h is stood,
It is then fed into separation equipment to be separated, obtains mixed solution and solid slag；The mixed solution for separating acquisition is placed in alembic
In, boiling and separated are heated to, composite extractant and tar is obtained, composite extractant is recycled, tar feeding tar
Storage tank；The solid slag obtained is separated, the composite extractant reclaimed again in composite extractant or above step carries out secondary
Embathe, separate, obtain mixed solution and solid slag；The solid slag isolated carries out third time extraction again.After three extract and separates
Solid slag in contained tar component account for the 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 percent by volume and are configured to furfural ester
Class composite extractant, the coal tar waste residue J2 for then producing the composite extractant and coke-oven plant is 2 according to mass ratio:1 in extraction
Take in groove and mix, obtain mixture；Under conditions of normal temperature and pressure, thing mixed above is carried out to be sufficiently stirred for 40min, stood
0.5h, is then fed into separation equipment and is separated, and obtains mixed solution and solid slag；The mixed solution for separating acquisition is placed in steaming
Evaporate in tank, be heated to boiling and separated, obtain composite extractant and tar, composite extractant is recycled, tar feeding
Tar tank；The solid slag obtained is separated, the composite extractant reclaimed again in composite extractant or above step is carried out
Secondary to embathe, separation obtains mixed solution and solid slag；The solid slag isolated carries out third time extraction again.Three extractions point
Contained tar component accounts for the 0.22% of integrated solid slag weight in solid slag from after.
Embodiment 3
At normal temperatures and pressures, furfural, ethyl acetate and methyl acetate are followed successively by 12%, 58%, 30% according to percent by volume
Be configured to furfural esters composite extractant, the coal tar waste residue Q1 for then producing the composite extractant and coal gasification course according to
Mass ratio is 2.5:1 mixes in extraction tank, obtains mixture；Under conditions of normal temperature and pressure, thing mixed above is filled
Divide stirring 50min, stand 1h, be then fed into separation equipment and separated, obtain mixed solution and solid slag；It will separate what is obtained
Mixed solution is placed in alembic, is heated to boiling and separated, obtains composite extractant and tar, and composite extractant is reclaimed
Utilize, tar feeding tar tank；The solid slag obtained is separated, that is reclaimed again in composite extractant or above step answers
Conjunction extractant progress is secondary to embathe, and separates, obtains mixed solution and solid slag；The solid slag isolated carries out third time extraction again
Take.Contained tar component accounts for the 0.2% of integrated solid slag weight in solid slag after three extract and separates.
Embodiment 4
At normal temperatures and pressures, furfural, isopropyl acetate are followed successively by 18% and 82% according to percent by volume and are configured to furfural
Esters composite extractant, the coal tar waste residue Q1 for then producing the composite extractant with coal gasification course is according to mass ratio
2.5:1 mixes in extraction tank, obtains mixture；Under conditions of normal temperature and pressure, thing mixed above is sufficiently stirred for
30min, stands 1h, is then fed into separation equipment and is separated, and obtains mixed solution and solid slag；The mixing for separating acquisition is molten
Liquid is placed in alembic, is heated to boiling and separated, obtains composite extractant and tar, and composite extractant is recycled,
Tar sends into tar tank；Separate the solid slag obtained, the compound extraction reclaimed again in composite extractant or above step
Take agent progress is secondary to embathe, separate, obtain mixed solution and solid slag；The solid slag isolated carries out third time extraction again.Three
Contained tar component accounts for the 0.13% of integrated solid slag weight in solid slag after secondary extract and separate.
Embodiment 5
At normal temperatures and pressures, furfural, isopropyl acetate and ethyl acetate are followed successively by 18% according to percent by volume, 50%,
32% is configured to furfural esters composite extractant, the coal tar waste residue J3 for then producing the composite extractant and coke-oven plant according to
Mass ratio is 2.5:1 mixes in extraction tank, obtains mixture；Under conditions of normal temperature and pressure, thing mixed above is filled
Divide stirring 30min, stand 1h, be then fed into separation equipment and separated, obtain mixed solution and solid slag；It will separate what is obtained
Mixed solution is placed in alembic, is heated to boiling and separated, obtains composite extractant and tar, and composite extractant is reclaimed
Utilize, tar feeding tar tank；The solid slag obtained is separated, that is reclaimed again in composite extractant or above step answers
Conjunction extractant progress is secondary to embathe, and separates, obtains mixed solution and solid slag；The solid slag isolated carries out third time extraction again
Take.Contained tar component accounts for the 0.16% of integrated solid slag weight in solid slag after three extract and separates.
Embodiment 6
At normal temperatures and pressures, furfural, isopropyl acetate and methyl acetate are followed successively by 20% according to percent by volume, 50%,
30% is configured to furfural esters composite extractant, the coal tar waste residue Q1 for then producing the composite extractant and coal gasification course
It is 3 according to mass ratio:1 mixes in extraction tank, obtains mixture；Under conditions of normal temperature and pressure, thing mixed above is carried out
50min is sufficiently stirred for, 40 min is stood, is then fed into separation equipment and is separated, mixed solution and solid slag is obtained；Will separation
The mixed solution of acquisition is placed in alembic, is heated to boiling and separated, obtains composite extractant and tar, compound extracting
Agent is recycled, tar feeding tar tank；The solid slag obtained is separated, is returned again in composite extractant or above step
The composite extractant progress of receipts is secondary to embathe, and separates, obtains mixed solution and solid slag；The solid slag isolated carries out the 3rd again
Secondary extraction.Contained tar component accounts for the 0.25% of integrated solid slag weight in solid slag after three extract and separates.
Embodiment described above is intended merely to enable those skilled in the art to be better understood from the present invention, but is not
The present invention is imposed any restrictions, to those skilled in the art, the present invention can have various conversion and replacement, all in this hair
Any modification, equivalent substitution and improvements done under the principle and spirit of embodiment described in bright method etc., belong to the guarantor of the present invention
Protect scope.
Claims (2)
1. a kind of coal tar waste residue extraction separating method, it is characterised in that：
The extraction separating method is that coal tar waste residue is carried out at normal temperatures and pressures based on a kind of furfural esters composite extractant
Extract and separate；
The coal tar waste residue is selected from any of coal tar waste residue J1, J2 and J3 that coke-oven plant is produced, or coal gasification course
The coal tar waste residue Q1 of generation, wherein：
J1 oil content is 44.82%, and moisture content is 6.30%, and solid slag content is 48.88%；
J2 oil content is 24.52%, and moisture content is 11.50%, and solid slag content is 63.98%；
J3 oil content is 49.82%, and moisture content is 17.50%, and solid slag content is 32.68%；
Q1 oil content is 28.23%, and moisture content is 16.30%, and solid slag content is 55.47%；
It is described the method that coal tar waste residue carries out extract and separate to be followed these steps to carry out at normal temperatures and pressures：
（1）At normal temperatures and pressures, coal tar waste residue and composite extractant are placed in extraction tank for 1: 1-3 ratio in mass ratio
Mixed, obtain mixture；
（2）At normal temperatures and pressures, to above-mentioned steps（1）In mixture be stirred, 0.5~2.0h of mixing time is rear to stand
0.5~1.0h, is then fed into separation equipment and is separated, and obtains mixed solution and solid slag；
（3）Through above-mentioned steps（2）The mixed solution obtained after separation is placed in alembic, is heated to boiling and separated, is obtained
Composite extractant and tar are obtained, composite extractant is recycled, tar feeding tar tank；
（4）Through above-mentioned steps（2）The solid slag obtained is separated, again by composite extractant or above-mentioned steps（3）Middle recovery
Composite extractant progress is secondary to embathe, and separates, and obtains mixed solution and solid slag；
（5）By above-mentioned steps（4）The solid slag that separation is obtained carries out third time extraction again；
The composition and its content of the furfural esters composite extractant are furfural 5~20%, esters solvent 80~95% by volume.
2. according to the method described in claim 1, the esters solvent in its described composite extractant is methyl acetate, ethyl acetate
With one or more mixing in isopropyl acetate.
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| CN105602596B (en) * | 2016-03-03 | 2018-08-03 | 西北大学 | A method of coal tar is detached based on selective reaction-solvent step |
| CN105668567B (en) * | 2016-04-15 | 2018-08-21 | 太原理工大学 | A kind of method that gasification of coal coke tar waste slag prepares Magnaglo activated carbon |
| CN106978203B (en) * | 2017-04-12 | 2019-06-04 | 西北大学 | A kind of coal tar takes off slag and fraction seperation technique and device |
| 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 |
| CN110395857A (en) * | 2018-04-19 | 2019-11-01 | 北京中科国通环保工程技术股份有限公司 | The method and apparatus for handling oil-containing hydrous matter |
| CN110358564B (en) * | 2019-07-15 | 2020-09-29 | 延安大学 | Coal tar residue separation device and separation method |
| CN114032115B (en) * | 2021-02-03 | 2024-01-16 | 臧正军 | Recycling recovery method of waste coal tar |
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| US4567464A (en) * | 1983-01-28 | 1986-01-28 | International Business Machines Corporation | Fixed rate constrained channel code generating and recovery method and means having spectral nulls for pilot signal insertion |
| CN101525284A (en) * | 2008-03-03 | 2009-09-09 | 艾博特(厦门)设备工程有限公司 | Method for reclaiming aliphatic carboxylic acid |
| CN101619230A (en) * | 2008-07-01 | 2010-01-06 | 汉能科技有限公司 | Method for recycling organic compounds from caustic sludge generated in coal tar oil light end alkali cleaning |
| CN101629086B (en) * | 2008-07-14 | 2013-03-20 | 中煤龙化哈尔滨煤制油有限公司 | Solvent extraction process for coal tar slag |
| CN101580729B (en) * | 2009-06-11 | 2012-12-05 | 煤炭科学研究总院 | Method for preparing mesophase asphalt by coal liquefaction residue |
| CN101885976B (en) * | 2010-07-02 | 2013-07-24 | 神华集团有限责任公司 | Method for extracting heavy liquefaction oil and intermediate-phase bitumen matter from coal liquefaction residuals and application thereof |
| CN104447238B (en) * | 2013-09-24 | 2016-06-08 | 中国石油化工股份有限公司 | The method purifying polyoxymethylene dimethyl ethers |
| CN104447283A (en) * | 2014-11-24 | 2015-03-25 | 太仓运通生物化工有限公司 | Preparation method for dextro-flurbiprofen |
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