CN105013800A - Method for recovering composite extracting agent in extraction and separation process of coal tar waste residues - Google Patents
Method for recovering composite extracting agent in extraction and separation process of coal tar waste residues Download PDFInfo
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- CN105013800A CN105013800A CN201510414355.XA CN201510414355A CN105013800A CN 105013800 A CN105013800 A CN 105013800A CN 201510414355 A CN201510414355 A CN 201510414355A CN 105013800 A CN105013800 A CN 105013800A
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Abstract
The invention discloses a method for recovering a composite extracting agent in the extraction and separation process of coal tar waste residues. The method includes the steps that a mixed solution which includes the composite extracting agent and coal tar and is obtained after the coal tar waste residues are extracted and separated is fed into a distillation retort, and then water is added and heated to be boiled; the azeotrope formed by the composite extracting agent and the water is volatilized out from the mixed solution; distillate is recycled in a condensation mode so that an oil-water mixture can be obtained; the composite extracting agent and the water are obtained by standing and layering and then are returned to the system to be recycled. The method has the characteristics that the recovered temperature of a furfural and ester composite extracting agent is low, operation is safe and reliable, the handling capacity is large, solvent loss is small, and the water content of tar is lower than 3%.
Description
Technical field
The present invention relates to a kind of recovery method of extractant, specifically a kind of recovery method for composite extractant in coal tar waste residue extraction separation process.
Background technology
Coal tar waste residue is coal in gasification and coking, and the coal dust, solia particle etc. carried secretly when the higher boiling 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 capacity is at about 8000kcal/kg, and therefore, coal tar waste residue is a kind of useful resource.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 surrounding air suffer severe contamination.Therefore, coal tar waste residue is carried out disposal and utilization effectively, the method use simply, be suitable for processes and reclaims natural resources and energy resources wherein, makes it to turn harm into good, turn waste into wealth, and 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, solvent extraction can isolate coal tar and coal dust, coke powder etc. efficiently from coal tar waste residue, is therefore a kind of very promising coal tar Solid state fermentation technique.The bottleneck problem that solvent extraction develops at present is the selection of extractant and the optimization of technique, and especially the recycling of extractant is most important.This seminar has carried out the research utilizing solvent extraction to carry out the method for coal tar waste residue extract and separate early stage, through many experiments, find that the composite extractant be made up of furfural and esters solvent is that a kind of separative efficiency is high, the extractant of function admirable, adopt the coal tar waste residue extract and separate operating process of this composite extractant can carry out under normal temperature and pressure conditions, technical process is simple, energy consumption and operating cost low, but the extraction dosage that consumes of this process comparatively large (1 ~ 3 times for coal tar slag quality).If do not recycled, then the emission problem of extractant seems comparatively outstanding, limits promoting the use of of the method.
Summary of the invention
In order to solve the recovery problem of above-mentioned extractant, the efficient circulation realizing the composite extractant of furfural and esters solvent composition utilizes, and reduces energy consumption and the operating cost of coal tar waste residue extraction and separation technology process further.The invention provides the recovery method of composite extractant in a kind of coal tar waste residue extraction separation process.
In order to solve the recovery problem of above-mentioned extractant, the technical solution adopted in the present invention is as follows.
A recovery method for composite extractant in coal tar waste residue extraction separation process, the recovery method of extractant described in it follows these steps to carry out:
(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, mixing time 0.5 ~ 2.0h, rear standing 0.5 ~ 1.0h, then send into separation equipment and be separated, obtain mixed solution and solid slag;
(3) mixed solution is sent in alembic, and add the water of 6.7 ~ 23.4% of described composite extractant volume, be heated to boiling, the azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar;
(4) oil water mixture obtained in step (3) is sent into oil water separator, leave standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank;
(5) step (4) is obtained composite extractant and send into extraction tank in above-mentioned steps (1) to solid slag
Again embathe; Obtain water and send into reuse in above-mentioned steps (3);
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;
Additional technical feature is as follows further.
The temperature of described boiling is 60 ~ 100 DEG C.
The composite extractant of described recovery is directly used in embathing of coal tar waste residue, and the water of recovery is directly used in the water yield that step (3) is added.
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%.
In the tar of described acquisition, moisture content is lower than 3%.
The inventive method utilizes furfural or ester class and water can form the principle of azeotropic mixture, reduce the boiling point of solvent evaporation, whole composite extractant reclaimer operation carries out at ambient pressure, vapo(u)rizing temperature is no more than 100 DEG C, thus avoiding carrying secretly of the tar light component produced because of high temperature distillation, the purity of composite extractant and the quality of tar are reclaimed in impact.Secondly, due to the formation of this azeotropic mixture, the moisture that originally contains in coal tar waste residue is separated along with distillation procedure, and then the water content obtaining tar is lower than 3%, thus reduces follow-up dehydration of tar operation.Finally, because the composite extractant adopted at room temperature is slightly soluble in water or water insoluble, after condensation, stratification can directly be separated, and therefore water-oil separating is simple to operate, easy, is separated the water and composite extractant also reusable edible that obtain.Therefore, the inventive method have that composite extractant recovered temperature is low, handling safety is reliable, treating capacity is large, solvent loss is little and the tar water content that obtains lower than the advantage such as 3%.In addition, the waste hot steam of factory is adopted can also to reduce the cost of composite extractant recovery process of the present invention further as thermal source.
Accompanying drawing explanation
Fig. 1 is the flow chart of composite extractant recovery method of the present invention.
Detailed description of the invention
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.
Embodiment 1
At normal temperatures and pressures, furfural, methyl acetate are followed successively by 5% and 95% according to percent by volume 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and add the water of 6.7% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 4.6%, and the moisture content obtaining tar is about 0.8%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when methyl acetate and water form azeotropic mixture is 56.5 DEG C.During according to formation azeotropic mixture, volume fraction in two kinds of azeotropic mixtures shared by water, can calculate and form the moisture that altogether needs of azeotropic mixture, and then deduct that original water content in coal tar waste residue used can calculate that the volume adding water in alembic is described composite extractant volume 6.7%.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
Embodiment 2
At normal temperatures and pressures, furfural, ethyl acetate are followed successively by 12% and 88% according to percent by volume 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and add the water of 17.2% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 4.0%, and the moisture content obtaining tar is about 1.3%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when ethyl acetate and water form azeotropic mixture is 70.4 DEG C.During according to formation azeotropic mixture, the volume fraction in two kinds of azeotropic mixtures shared by water, can calculate, and the volume altogether needing to add water in alembic is 17.2% of described composite extractant volume.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
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 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and add the water of 11.4% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 3.7%, and the moisture content obtaining tar is about 1.2%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when ethyl acetate and water form azeotropic mixture is 70.4 DEG C, and methyl acetate and water form the azeotropic point 56.5 DEG C during azeotropic mixture.During according to formation azeotropic mixture, the volume fraction in three kinds of azeotropic mixtures shared by water, can calculate, and the volume altogether needing to add water in alembic is 11.4% of described composite extractant volume.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
Embodiment 4
At normal temperatures and pressures, furfural, isopropyl acetate are followed successively by 18% and 82% according to percent by volume 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and add the water of 23.4% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 2.2%, and the moisture content obtaining tar is about 2.3%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when isopropyl acetate and water form azeotropic mixture is 77.4 DEG C.During according to formation azeotropic mixture, the volume fraction in two kinds of azeotropic mixtures shared by water, can calculate, and the volume altogether needing to add water in alembic is 23.4% of described composite extractant volume.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
Embodiment 5
At normal temperatures and pressures, furfural, isopropyl acetate and ethyl acetate are followed successively by 18%, 50%, 32% according to percent by volume 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and add the water of 22.1% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 2.8%, and the moisture content obtaining tar is about 2.2%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when isopropyl acetate and water form azeotropic mixture is 77.4 DEG C, and azeotropic point when ethyl acetate and water form azeotropic mixture is 70.4 DEG C.During according to formation azeotropic mixture, the volume fraction in three kinds of azeotropic mixtures shared by water, can calculate, and the volume altogether needing to add water in alembic is 22.1% of described composite extractant volume.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
Embodiment 6
At normal temperatures and pressures, furfural, isopropyl acetate and methyl acetate are followed successively by 20%, 50%, 30% according to percent by volume 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 separation equipment and be separated, obtain mixed solution and solid slag; Carry out again embathing for twice by being separated the solid slag obtained, mixed solution is sent in alembic, and need to add the water of 22.2% of described composite extractant volume, be heated to boiling, azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar; The oil water mixture obtained is sent into oil water separator, leaves standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank; The extraction tank that acquisition composite extractant is sent in described step embathes again to solid slag; Acquisition water sends into reuse in the alembic in described step; Through the inventive method, the composite extractant loss late of recovery is about 2.7%, and the moisture content obtaining tar is about 2.5%.
In this embodiment, azeotropic point when furfural and water form azeotropic mixture is 98.0 DEG C, and azeotropic point when isopropyl acetate and water form azeotropic mixture is 77.4 DEG C, and methyl acetate and water form the azeotropic 56.5 DEG C during azeotropic mixture.During according to formation azeotropic mixture, the volume fraction in three kinds of azeotropic mixtures shared by water, can calculate, and the volume altogether needing to add water in alembic is 22.2% of described composite extractant volume.
As can be seen from the above-described embodiment, because the boiling point of the azeotropic mixture formed after add water in composite extractant is all no more than 100 DEG C, the waste hot steam of factory therefore can be adopted to the thermal source of alembic heating.
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 (7)
1. the recovery method of composite extractant in coal tar waste residue extraction separation process, the recovery method of extractant described in it follows these steps to carry out:
(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, mixing time 0.5 ~ 2.0h, rear standing 0.5 ~ 1.0h, then send into separation equipment and be separated, obtain mixed solution and solid slag;
(3) mixed solution is sent in alembic, and add the water of 6.7 ~ 23.4% of described composite extractant volume, be heated to boiling, the azeotropic mixture containing composite extractant and water evaporates from containing the mixed solution of tar, distillate is reclaimed in condensation, obtains oil water mixture and tar;
(4) oil water mixture obtained in step (3) is sent into oil water separator, leave standstill 0.5 ~ 1h, layering, obtain composite extractant and water; The tar obtained is transferred in tar tank;
(5) step (4) is obtained composite extractant and send into extraction tank in above-mentioned steps (1) to solid slag
Again embathe; Obtain water and send into reuse in above-mentioned steps (3);
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.
2., according to the recovery method of the composite extractant described in claim 1, the temperature of seething with excitement described in it is 60 ~ 100 DEG C.
3. according to the recovery method of the composite extractant described in claim 1, the composite extractant reclaimed described in it is directly used in embathing of coal tar waste residue, and the water of recovery is directly used in the water yield that step (3) is added.
4. the recovery method of composite extractant 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.
5. the recovery method of composite extractant 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.
6. method according to claim 1, obtains tar described in it and solid slag is respectively 20% ~ 50% and 30% ~ 65%.
7. method according to claim 1, in the tar obtained described in it, moisture content is lower than 3%.
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