CN203139681U - Complete equipment for separating and extracting phenols in middle-temperature and low-temperature coal tar by extraction method - Google Patents

Complete equipment for separating and extracting phenols in middle-temperature and low-temperature coal tar by extraction method Download PDF

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Publication number
CN203139681U
CN203139681U CN 201320070977 CN201320070977U CN203139681U CN 203139681 U CN203139681 U CN 203139681U CN 201320070977 CN201320070977 CN 201320070977 CN 201320070977 U CN201320070977 U CN 201320070977U CN 203139681 U CN203139681 U CN 203139681U
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China
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kettle
solvent
discharging opening
extraction
phenols
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宗志敏
闵小建
朱影
刘双泰
严立
赵鹤翔
孙秀花
李瑶
李占库
赵云鹏
樊星
魏贤勇
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China University of Mining and Technology CUMT
Shaanxi Coal and Chemical Technology Institute Co Ltd
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China University of Mining and Technology CUMT
Shaanxi Coal and Chemical Technology Institute Co Ltd
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Abstract

The utility model provides complete equipment for separating and extracting phenols in middle-temperature and low-temperature coal tar by an extraction method and belongs to complete equipment for extracting low-temperature coal tar. The complete equipment for extracting the phenols in the middle-temperature and low-temperature coal tar is formed by five kettles, four pots and three condensers: a middle-temperature and low-temperature coal tar extraction and separation kettle, an extracted light oil extracting agent concentration kettle I, a solvent pot I, an extracted rough phenol extracting agent concentration kettle II, a solvent pot II, a solvent extracting and refining rough phenol kettle III, an extracted and refined rough phenol filtering pot, an extracted and refined rough phenol extracting agent concentration kettle, a solvent pot III, a condenser I, a condenser II and a condenser III. According to the complete equipment disclosed by the utility model, the fine separation of low-carbon hydrocarbons and mixed phenols in the middle-temperature and low-temperature coal tar can be rapidly, conveniently selectively and highly-purely realized under a very moderate condition; the condensation effect of a plurality of grades of the condensers is obvious, the environmental pollution is small and the condensers are easy to recycle and circularly use; and the large-scale production and utilization of good-quality high additional values including separation, transferring and the like of the low-temperature coal tar are easy to realize.

Description

The complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction
Technical field
The utility model relates to a kind of complete set of equipments that extracts coalite tar, particularly the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction.
Background technology
Middle coalite tar is the byproduct of producing blue charcoal, coal gas.The organic compound content of non-hydrocarbons is very high in the middle coalite tar, the phenolic compound in the acidic components particularly, its content can be up to 10% one 30% of total amount of liquid, in lower boiling phenolic compound mainly comprise C3-C4 alkylphenol, naphthols and alkyl naphthol etc.
In coalite tar be a kind of industrial chemicals that high added value is arranged, can be for the production of organic chemicals such as liquid fuel, phenols, alkane and aromatic hydrocarbons, also can be from wherein isolating a lot of important chemical intermediates.Be that basic material can be produced many kinds of products with the phenols: as plastics, binding agent, pesticide, disinfectant, surfactant, tanning agent etc.
The processing method of afterwards carrying phenol is distilled by domestic elder generation commonly used: in these class methods mainly with alkali cleaning dephenolize method separation and Extraction phenolic compound.This method mainly exists the dephenolize rate lower, and alkali acid consumption is big, wash-out often, the time is long, the energy consumption height, the difficult recovery of polyhydric phenols and higher phenols particularly is easy to cause disadvantages such as the easy oxidational losses of phenols.Next be utilize selective solvent extraction process processing separate in coalite tar: these class methods comprise superheated water extraction process and selective solvent extraction process and first salts solution extraction process and alcohol solution extraction process, also have the method that adopts the ion exchange resin adsorbing separation to extract phenolic compound in the coal tar.Coalite tar separation processing method is mainly used in research process in such at present, corresponding processing method, process conditions and corollary equipment prematurity still, and corresponding engineering reliability, economic and practical and scale feasibility be less report all.
Because there are very big difference in composition and the high temperature coal-tar of middle coalite tar, so can not be with existing high temperature coal-tar method for processing, technology and device processes coalite tar.
Summary of the invention
Technical problem: the purpose of this utility model provides a kind of compact conformation, and energy consumption is low, the complete set of equipments of phenols in the coalite tar in the high extraction separation and Extraction of extract and separate efficient.
Technical scheme: carry the complete set of equipments of phenol during the purpose of this utility model is achieved in that in the coalite tar, it is made up of five stills, four jars and three groups of condensers; It is respectively middle coalite tar extract and separate still; No. 1 extractant concentration kettle of extraction light oil; No. 1 solvent tank; No. 2 extractant concentration kettle of extraction crude phenols; No. 2 solvent tanks; The crude phenols still is made with extra care in No. 3 solvent extractions; Extracting and refining crude phenols filtering tank; Extracting and refining crude phenols extractant concentration kettle; No. 3 solvent tanks and No. 1 condenser, No. 2 condensers and No. 3 condensers.
Upper right sidepiece discharging opening links to each other with the upper left side feeding mouth pipeline of extraction light oil extractant concentration kettle in the middle coalite tar extract and separate still, and the middle part discharging opening links to each other with the feeding mouth pipeline of the refining crude phenols still upper left side of No. 3 solvent extractions under the middle coalite tar extract and separate still; The discharging opening of No. 1 extractant concentration kettle of extraction light oil upper right side is connected with the feeding mouth pipeline of No. 1 condenser, and No. 2 extractant concentration kettle of the discharging opening at middle part and extraction crude phenols upper left side feeding mouth pipeline is connected under No. 1 extractant concentration kettle of extraction light oil; No. 1 condenser discharging opening is connected with middle part feeding mouth pipeline on No. 1 solvent tank, and the middle part discharging opening is connected with the discharging opening pipeline of middle coalite tar extract and separate still upper right side under No. 1 solvent tank; The feeding mouth of extraction crude phenols extractant concentration kettle upper left side respectively with No. 1 extractant concentration kettle of extraction light oil under the discharging opening at middle part and No. 2 solvent tanks discharging opening pipeline at middle part be connected, the discharging opening of No. 2 extractant concentration kettle of extraction crude phenols upper right side is connected with No. 2 condenser feeding mouth pipelines, and the material outlet of No. 2 extractant concentration kettle of extraction crude phenols middle and lower part directly is connected with the refining crude phenols still feeding mouth of No. 3 solvent extractions; The feeding mouth road at middle part is connected on No. 2 condenser discharging opening pipes and No. 2 solvent tanks, the discharging opening at middle part is connected with the feeding mouth pipeline that crude phenols still upper left side is made with extra care in No. 3 solvent extractions under No. 2 solvent tanks, the refining crude phenols still upper right quarter discharging opening of No. 3 solvent extractions is connected with the middle part feeding mouth pipeline of going up of extracting and refining crude phenols filtering tank, and the discharging opening by middle part under the refining crude phenols still of No. 3 solvent extractions of triple valve is connected with the middle part feeding mouth pipeline of going up of extracting and refining crude phenols filtering tank simultaneously; The following middle part discharging opening of extracting and refining crude phenols filtering tank is connected with the feeding mouth pipeline of extracting and refining crude phenols extractant concentration kettle upper left side; The discharging opening of No. 3 extractant concentration kettle of extracting and refining crude phenols upper right side is connected with No. 3 condenser feeding mouth pipelines; No. 3 the condenser discharging opening is connected with the feeding mouth pipeline on No. 3 solvent tank tops; The discharging opening of No. 3 solvent tank bottoms is connected with the feeding mouth pipeline of the refining crude phenols still upper right side of No. 3 solvent extractions.
Coalite tar extract and separate still comprises a withstand voltage kettle in described, be covered with the magnetic stirring apparatus, the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, inlay the liftable filter of filter membrane mesh, the autoclave body top cover is provided with No. 1 extractant and No. 2 extractant material inlets at upper left sidepiece, also be provided with Pressure gauge, upper right sidepiece is provided with discharging opening, is provided with visual windows in the pressure kettle, and the middle part is provided with material outlet under the still.
No. 1 extractant concentration kettle of described extraction light oil comprises a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the upper left side is provided with light oil and No. 1 solvent material entrance that obtains with coalite tar in the extraction on the top cover of pressure kettle, upper right sidepiece is provided with discharging opening, Pressure gauge is provided with visual windows in the kettle, the lower middle portion of kettle is not provided with the discharging opening that concentrates light oil.
Described No. 1 solvent tank comprises a normal pressure jar, and normal pressure jar middle and upper part is provided with No. 1 solvent feeding mouth of condensation, and following middle part is provided with the solvent discharging opening No. 1; Described No. 2 solvent tanks comprise a normal pressure jar, and the normal pressure jar is provided with the feeding mouth of No. 2 solvents that condenser condenses gets off, and the bottom is provided with the solvent discharging opening No. 2.
No. 2 extractant concentration kettle of described extraction crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the top cover left upper portion of pressure kettle is provided with crude phenols and No. 2 solvent material entrances that obtain for the extraction coalite tar, right upper portion is provided with material outlet, Pressure gauge is provided with visual windows in the kettle, the lower middle bottom of kettle is provided with the discharging opening that concentrates crude phenols.
Described No. 2 solvent tanks comprise a normal pressure jar, and the normal pressure jar is provided with the feeding mouth valve of No. 2 solvents that condenser condenses gets off, and the bottom is provided with the solvent discharging opening No. 2.
The refining crude phenols still of described No. 3 solvent extractions comprises a withstand voltage kettle, is covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, is provided with the liftable filter of inlaying the filter membrane mesh in the autoclave body, heat(ing) coil; The feeding mouth of coalite tar and No. 2 extractants during the upper left side is provided with on the top cover of pressure kettle, upper right side are provided with extraction mixed material discharging opening, Pressure gauge, are provided with visual windows in the kettle, and the kettle middle and lower part is provided with extraction refining of crude phenol mixed material discharging opening.
Described extracting and refining crude phenols filtering tank comprises a withstand voltage kettle, is covered with extraction refining of crude phenol mixed material feeding mouth on the withstand voltage kettle, and withstand voltage kettle bottom is provided with extraction refining of crude phenol mixed material discharging opening.
No. 3 extractant concentration kettle of described extracting and refining crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the top cover upper left side of pressure kettle is provided with extraction refining of crude phenol mixed material feeding mouth and No. 3 solvent material entrances, upper right sides and is provided with material outlet, Pressure gauge, be provided with visual windows in the kettle, the middle and lower part of kettle is provided with the discharging opening that concentrates crude phenols respectively.
Described No. 3 solvent tanks comprise a normal pressure jar, and normal pressure jar middle and upper part is provided with the feeding mouth of number solvent that the device condensation that is condensed gets off, and the middle and lower part is provided with the solvent discharging opening No. 3.
Described No. 1 condenser, No. 2 condensers and No. 3 condensers are three shell and tube condensers that size does not wait, and condenser comprises the discharging opening of material after the material charging aperture that is condensed and the condensation; No. 1 condenser has charging aperture and discharging opening; No. 2 condenser has charging aperture and discharging opening; No. 3 condenser has charging aperture and discharging opening.
Beneficial effect, owing to adopted such scheme, in complete set of equipments, utilize selected suitable extractant, can be quick, easy under condition as mild as a dove, optionally, high-purity realizes therefrom in the coalite tar low charcoal hydro carbons and mixes the meticulous of phenols and separate; Utilize the complete set of equipments in the utility model, be easy to realize hanging down in the coalite tar enrichment and the recovery of charcoal hydrocarbon and aldehydes matter; The recovery repeatedly that utilizes this complete set of equipments can finish multiple extraction agent is with high yield used; Solvent for use is the lower solvent of boiling point or mixed solvent, saves operation energy and cost in operating; Because unit operations all is to carry out in the equipment of sealing, the multi-stage condensing device condensation effect that complete set of equipments of the present utility model adopts is remarkable, and environmental pollution is little and be easy to reclaim and recycle; Complete set of equipments of the present utility model is expected to large-scale production and utilization, is easy to realize high-quality high value added utilizations such as coalite tar separation and conversion.
Advantage: with separate, extract in the coalite tar phenols legacy equipment relatively, utilizing this complete set of equipments biggest advantage to be can be optionally, high-purity ground realize in the coalite tar low charcoal hydro carbons with mix the meticulous of phenols and separate; Operate quick, easy, be easy to large-scale production; Operating cost is low, effects of energy saving and emission reduction is remarkable.
Description of drawings
Fig. 1 is the structure chart of coalite tar extract and separate still equipment in the utility model.
Fig. 2 is the structure chart of No. 1 extractant concentration kettle of the utility model extraction light oil equipment.
Fig. 3 is the structure chart of No. 1 solvent tank equipment of the utility model.
Fig. 4 is the structure chart of No. 2 extractant concentration kettle of the utility model extraction crude phenols equipment.
Fig. 5 is the structure chart of No. 2 solvent tank equipment of the utility model.
Fig. 6 is the structure chart of the refining crude phenols still equipment of No. 3 solvent extractions of the utility model.
Fig. 7 is the structure chart of the utility model extracting and refining crude phenols filtering tank equipment.
Fig. 8 is the structure chart of No. 3 extractant concentration kettle of the utility model extracting and refining crude phenols equipment.
Fig. 9 is the structure chart of No. 3 solvent tank equipment of the utility model.
Figure 10-the 1st, the structure chart of first group of condenser apparatus of the utility model.
Figure 10-the 2nd, the structure chart of second group of condenser apparatus of the utility model.
Figure 10-the 3rd, the structure chart of the 3rd group of condenser apparatus of the utility model.
Figure 11 is the process chart of carrying the phenol complete set of equipments in the utility model in the coalite tar.
Among the figure, 1, magnetic agitation slurry; 2, heat(ing) coil; 3, inlay the liftable filter of filter membrane mesh; 4, upper left sidepiece material inlet; 5, temperature thermocouple; 6, Pressure gauge; 7, upper right sidepiece discharging opening; 8, middle coalite tar extract and separate still; 9, visual windows in the still; 10, descend the middle part material outlet; 11, upper left side material inlet; 12, upper right side material outlet; 13, No. 1 extractant concentration kettle of extraction light oil; 14, descend the middle part material outlet; 15, No. 1 condenser charging aperture; 16, No. 1 condenser discharging opening; 17, No. 1 solvent tank; 18, go up the middle part material inlet; 19, descend the middle part material outlet; 20, No. 2 extractant concentration kettle of extraction crude phenols; 21, upper left side material inlet; 22, upper right side material outlet; 23, descend the middle part material outlet; 24, No. 2 condenser charging apertures; 25, No. 2 condenser discharging openings; 26, No. 2 solvent tanks; 27, go up the middle part material inlet; 28, descend the middle part material outlet; 29, the refining crude phenols still of No. 3 solvent extractions; 30, upper left side material inlet; 31, upper right side material outlet; 32, descend the middle part material outlet; 33, go up the middle part material inlet; 34, extracting and refining crude phenols filtering tank; 35, descend the middle part material outlet; 36, No. 3 extractant concentration kettle of extracting and refining crude phenols; 37, upper left side material inlet; 38, upper right side material outlet; 39, descend the middle part material outlet; 40, No. 3 condenser charging apertures; 41, No. 3 condenser discharging openings; 42, go up the middle part material inlet; 43, No. 3 solvent tanks; 44, descend the middle part material outlet; 45-1, No. 1 condenser; 45-2, No. 2 condensers; , 45-3, No. 3 condensers.
The specific embodiment
Below in conjunction with accompanying drawing an embodiment in the utility model is further described:
Embodiment 1: carry the complete set of equipments of phenol in the middle coalite tar, it is made up of five stills, four jars and three groups of condensers; It is respectively middle coalite tar extract and separate still 8; No. 1 extractant concentration kettle 13 of extraction light oil; No. 1 solvent tank 17; No. 2 extractant concentration kettle 20 of extraction crude phenols; No. 2 solvent tanks 26; Crude phenols still 29 is made with extra care in No. 3 solvent extractions; Extracting and refining crude phenols filtering tank 34; No. 3 extractant concentration kettle 36 of extracting and refining crude phenols; No. 3 solvent tanks 43 and No. 1 condenser 45-1, No. 2 condenser 45-2 and No. 3 condenser 45-3.
In Figure 11, upper left side feeding mouth 11 pipelines of upper right sidepiece discharging opening 7 and No. 1 extractant concentration kettle 13 of extraction light oil link to each other in the middle coalite tar extract and separate still 8, and middle part discharging openings 10 link to each other with feeding mouth 30 pipelines of refining crude phenols still 29 upper left sides of No. 3 solvent extractions under the middle coalite tar extract and separate still 8; The discharging opening 12 of No. 1 extractant concentration kettle 13 upper right sides of extraction light oil is connected with feeding mouth 15 pipelines of No. 1 condenser 45-1, and No. 2 extractant concentration kettle of the discharging opening 14 at 13 times middle parts of extraction No. 1 extractant concentration kettle of light oil and extraction crude phenols 20 upper left side feeding mouths 21 pipelines are connected; No. 1 condenser 45-1 discharging opening 16 is connected with middle part feeding mouth 18 pipelines on No. 1 solvent tank 17, and middle part discharging opening 19 is connected with discharging opening 7 pipelines of middle coalite tar extract and separate still 8 upper right sides under No. 1 solvent tank; The feeding mouth 21 of extraction crude phenols No. 2 extractant concentration kettle 20 upper left sides respectively with No. 1 extractant concentration kettle 13 of extraction light oil under the discharging opening 7 at middle part and No. 2 solvent tanks discharging opening 28 pipelines at middle part be connected, the discharging opening 22 of No. 2 extractant concentration kettle 20 upper right sides of extraction crude phenols is connected with No. 2 condenser 45-2 feeding mouth 24 pipelines, and the material outlet 23 of No. 2 extractant concentration kettle 20 middle and lower parts of extraction crude phenols directly is connected with the refining crude phenols still feeding mouth 30 of No. 3 solvent extractions; The feeding mouth 27 tunnel at middle part is connected on No. 2 condenser 45-2 discharging opening pipes 25 and No. 2 solvent tanks 26, the discharging opening 28 at middle part is connected with feeding mouth 30 pipelines that crude phenols still 29 upper left sides are made with extra care in No. 3 solvent extractions under No. 2 solvent tanks, the refining crude phenols still 29 upper right quarter discharging openings 31 of No. 3 solvent extractions are connected with middle part feeding mouth 33 pipelines of going up of extracting and refining crude phenols filtering tank 34, and the discharging opening 32 by the refining 29 times middle parts of crude phenols still of No. 3 solvent extractions of triple valve is connected with middle part feeding mouth 33 pipelines of going up of extracting and refining crude phenols filtering tank 34 simultaneously; Feeding mouth 37 pipelines of No. 3 extractant concentration kettle 36 upper left sides of following middle part discharging opening 35 and extracting and refining crude phenols of extracting and refining crude phenols filtering tank 34 are connected; The discharging opening 38 of No. 3 extractant concentration kettle 36 upper right sides of extracting and refining crude phenols is connected with No. 3 condenser 45-3 feeding mouth 40 pipelines; No. 3 condenser 45-3 discharging opening 41 is connected with feeding mouth 42 pipelines on No. 3 solvent tank 43 tops; The discharging opening 44 of No. 3 solvent tank 43 bottoms is connected with feeding mouth 30 pipelines of refining crude phenols still 24 upper right sides of No. 3 solvent extractions.
Realize that utility model content used three kinds or three class extraction agent are as follows respectively:
The 1# solvent comprises: the mixed liquor of one or more solvents in kerosene, solvent naphtha, low carbon chain hydrocarbon solvent, benzinum, the coal tar washing lotion;
The 2# solvent comprises: the mixed liquor of one or more solvents in acetone, butanone, methyl alcohol, ethanol, cyclohexanol, glacial acetic acid, the distilled water;
The 3# solvent comprises: the mixed liquor of one or more solvents in chloroform, methyl-sulfoxide, carbon disulfide, oxolane, toluene, the ethyl acetate.
In Fig. 1, middle coalite tar extract and separate still 8 comprises a withstand voltage kettle, be covered with the magnetic stirring apparatus 1, the thermocouple 5 that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil 2 in the autoclave body, inlay the liftable filter 3 of filter membrane mesh, the autoclave body top cover is provided with No. 1 extractant and No. 2 extractant material inlets 4 at upper left sidepiece, also is provided with Pressure gauge 6, and upper right sidepiece is provided with discharging opening 7, be provided with visual windows 9 in the pressure kettle, the middle part is provided with material outlet 10 formations under the still.
The coalite tar therefrom material inlet 4 of coalite tar extract and separate still 8 upper left quarters enters, under magnetic stirring apparatus 1 slowly stirred, therefrom the material inlet 4 of coalite tar extract and separate still 8 upper left quarters added 1# solvent and the 2# solvent solvent of the 1:1 volume ratio that coalite tar volume 2-4 doubly measures in the kettle.Utilize heat(ing) coil 2 and thermocouple 5, temperature maintenance is 30 in the control kettle 0C-50 0About C, through static after 10 minutes to 10 hours the stirring, utilize to be provided with visual windows 9 in the kettle and can clearly to observe the kettle mixed solution and obviously be divided into two-layer up and down.Utilize the external force effect, the inflow suitable for reading that impels the whole clumps of last phase mixed solution to inlay the liftable filter 3 of filter membrane mesh extracts in No. 1 extractant concentration kettle 13 of light oil, utilize the gravity effect, following phase mixed solution middle part under still is provided with material outlet 10 and flows into the refining crude phenols still of No. 3 solvent extractions.Same extracting operation repeatedly, continuous several times finds by overtesting: the last phase constituent that flows in No. 1 extractant concentration kettle 13 of extraction light oil mainly is made up of the low charcoal chain hydrocarbon in 1# solvent and the middle coalite tar, flows in the refining crude phenols still of No. 3 solvent extractions down in the phase constituent mainly by containing 2# solvent-thick mixed phenol-newborn solution composition of lighting up of the mixing of pitch on a small quantity.
In Fig. 2, No. 1 extractant concentration kettle 13 of extraction light oil comprises a withstand voltage kettle, be covered with the magnetic stirring apparatus 1 and the thermocouple 5 that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil 2 in the autoclave body, the upper left side is provided with light oil and No. 1 solvent material entrance 11 that obtains with coalite tar in the extraction on the top cover of pressure kettle, and upper right sidepiece is provided with discharging opening 12, Pressure gauge 6, be provided with visual windows 9 in the kettle, the lower middle portion of kettle is not provided with the discharging opening 14 that concentrates light oil and constitutes.
The mixed solution of the low charcoal chain hydrocarbon in 1# solvent and the middle coalite tar is after therefrom the material outlet 10 of coalite tar extract and separate still 8 left middle and lower parts flows into kettlies through the material inlet 11 of No. 1 extractant concentration kettle 13 upper left sides of extraction light oil, under magnetic stirring apparatus 1 slowly stirs, utilize heat(ing) coil 2 and thermocouple 5, temperature maintenance is 60 in the control kettle 0C-90 0About C, 1# solvent constantly gasification is to enter condenser from No. 1 condenser 45-1 charging aperture 15 behind the steam,, from directly entering No. 1 solvent tank 17, No. 1 condenser 45-1 discharging opening 16 concentrates, the material outlet 14 of No. 1 extractant concentration kettle 13 middle and lower parts of low charcoal chain hydrocarbon extraction light oil in the middle coalite tar after the enrichment emits through condensed 1# solvent.Test is found: utilize this equipment distillation 1# solvent to have the very high rate of recovery and can use repeatedly, concentration effect is obviously and have a very high yield at the bottom of still for the low charcoal chain hydrocarbon in the middle coalite tar.
In Fig. 3, No. 1 solvent tank 17 comprises a normal pressure jar, and normal pressure jar middle and upper part is provided with No. 1 solvent feeding mouth 18 of condensation, and following middle part is provided with solvent discharging opening 19 No. 1; Described No. 2 solvent tanks 26 comprise a normal pressure jar, and the normal pressure jar is provided with the feeding mouth 27 of No. 2 solvents that condenser condenses gets off, and the bottom is provided with No. 2 solvent discharging openings 28 and constitutes.
Through condensed 1# solvent solution from No. 1 condenser 45-1 discharging opening 16 directly enters No. 1 solvent tank 17, as required after 1# solvent and the 2# solvent through external influence power therefrom the feeding mouth 4 of coalite tar extract and separate still 8 upper left quarters flows into from No. 1 solvent tank 17 middle and lower part discharging opening 19 coalite tar extract and separate still 8 extract use repeatedly as new extractant again, the 1# solvent that flows out of No. 2 condenser 45-2 discharging openings 25 also flows back to solvent tank No. 1 from No. 1 solvent tank 17 feeding mouths 18 through pipeline simultaneously.Test is found: utilize this equipment distillation 1# solvent to have very high cooling, recovering effect and can use repeatedly.
In Fig. 4, No. 2 extractant concentration kettle 20 of extraction crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus 1 and the thermocouple 5 that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil 2 in the autoclave body, the top cover left upper portion of pressure kettle is provided with crude phenols and No. 2 solvent material entrances 21 that obtain for the extraction coalite tar, and right upper portion is provided with material outlet 22, Pressure gauge 6, be provided with visual windows 9 in the kettle, the lower middle bottom of kettle is provided with the discharging opening 23 that concentrates crude phenols and constitutes.
No. 2 extractant concentration kettle 20 of extraction crude phenols are as the standby still of a cover of system.Wherein also mix some mixed phenols if the mixed solution in therefrom separating on the back mutually in the coalite tar extract and separate still 8 flows into to be detected before No. 1 extractant concentration kettle of extraction light oil 13, this moment therefrom the material outlet 7 at coalite tar extract and separate still 8 upper right middle parts flow out mainly by entering kettle behind the material inlet 21 of low charcoal chain hydrocarbon through No. 2 extractant concentration kettle 20 loam cake upper left sides of extraction crude phenols in 1# solvent and the middle coalite tar.Add the 2# solvent of 2 times of amounts of mixed liquor volume in the kettle again from the material inlet 21 of extraction crude phenols No. 2 extractant concentration kettle 20 upper left quarters, utilizing heat(ing) coil 2 and thermocouple 5, temperature maintenance is 30 in the control kettle 0C-50 0The C left and right sides static 10 minutes-10 hours utilizes to be provided with visual windows 9 in the kettle and can clearly to observe the kettle mixed solution and obviously be divided into two-layer up and down.Last phase constituent in the still utilizes heat(ing) coil 2 and thermocouple 5 under magnetic stirring apparatus 1 slowly stirs, temperature maintenance is 60 in the control kettle 0C-90 0About C, 1# solvent constantly gasification is to enter condenser from No. 2 condenser 45-1 charging apertures 24 behind the steam,, from directly entering No. 1 solvent tank 17, No. 2 condenser 45-1 discharging openings 25 concentrate, the low charcoal chain hydrocarbon in the middle coalite tar after the enrichment directly enters the refining crude phenols still feeding mouth 30 of No. 3 solvent extractions from the material outlet 23 of No. 2 extractant concentration kettle 20 middle and lower parts of extraction crude phenols through condensed 1# solvent.Following phase constituent in the still utilizes heat(ing) coil 2 and thermocouple 5 under magnetic stirring apparatus 1 slowly stirs, temperature maintenance is 80 in the control kettle 0C-120 0About C, 2# solvent constantly gasification is to enter condenser from No. 2 condenser 45-1 charging apertures 24 behind the steam,, from directly entering No. 2 solvent tanks 26, No. 2 condenser 45-1 discharging openings 25 concentrate, the thick mixing phenols in the middle coalite tar after the enrichment directly enters the refining crude phenols still 29 of No. 3 solvent extractions from the material outlet 23 of No. 2 extractant concentration kettle 20 middle and lower parts of extraction crude phenols through condensed 2# solvent.Test is found: utilize the low charcoal hydrocarbons in the further high-purity meticulous separation in ground of this equipment, the enrichment coalite tar, simultaneously for the loss that reduces aldehydes matter provides possibility, the concentration effect at the bottom of still of the low charcoal chain hydrocarbon in the middle coalite tar is obvious and have a very high yield.
In Fig. 5, No. 2 solvent tank 26 comprises a normal pressure jar, and the normal pressure jar is provided with the feeding mouth valve 27 of No. 2 solvents that condenser condenses gets off, and the bottom is provided with No. 2 solvent discharging openings 28 and constitutes.
Through condensed 2# solvent from No. 2 condenser 45-2 discharging openings 25 directly enter No. 2 solvent tanks 26, as required after 2# solvent and the 1# solvent through the external influence masterpiece be new extractant respectively from No. 1 day solvent tank 17 and No. 2 solvent tank 26 middle and lower part discharging openings 28 mixes in proportion afterwards by the feeding mouth 4 of coalite tar extract and separate still 8 upper left quarters enter use repeatedly again.Test is found: utilize this equipment distillation 2# solvent to have very high cooling, recovering effect and can use repeatedly.
In Fig. 6, the refining crude phenols still 29 of No. 3 solvent extractions comprises a withstand voltage kettle, is covered with the magnetic stirring apparatus 1 and the thermocouple 5 that lead in the kettle on the withstand voltage kettle, is provided with the liftable filter 3 of inlaying the filter membrane mesh in the autoclave body, heat(ing) coil 2; The feeding mouth 30 of coalite tar and No. 2 extractants during the upper left side is provided with on the top cover of pressure kettle, the upper right side is provided with extraction mixed material discharging opening 31, Pressure gauge 6, be provided with visual windows 9 in the kettle, the kettle middle and lower part is provided with extraction refining of crude phenol mixed material discharging opening 32 and constitutes.
The mixing breast candle solution (following phase constituent) that the contains 2# solvent-thick mixed phenol-a small amount of pitch therefrom material outlet at 8 times middle parts of coalite tar extract and separate still enters kettle after flowing out material inlet 30 through the refining crude phenols still 29 loam cake upper left sides of No. 3 solvent extractions.The 3# solvent and the 2# solvent solvent that add the 1:10 volume ratio of 2 times of amounts of mixed liquor volume in the kettle from the material inlet 31 of refining crude phenols still 29 upper left quarters of No. 3 solvent extractions.Utilizing heat(ing) coil 2 and thermocouple 5, temperature maintenance is 30 in the control kettle 0C-50 0The C left and right sides static 10 minutes-10 hours utilizes to be provided with visual windows 9 in the kettle and can clearly to observe the kettle mixed solution and obviously be divided into two-layer up and down.Utilize the external force effect, impel and go up the phase mixed solution and all be provided with extraction mixed material discharging opening 31 and flow directly in the extracting and refining crude phenols filtering tank 34 and filter in the clump upper right side of inlaying the liftable filter 3 of filter membrane mesh, utilize the gravity effect, a spot of phase mixed solution down middle part under still is provided with material outlet 32 and flows directly into filtration the extracting and refining crude phenols filtering tank 34.Same extracting operation repeatedly, continuous several times finds by overtesting: mainly forms by containing 2# solvent-mixed phenol in the phase constituent on the refining crude phenols still 29 of No. 3 solvent extractions, descend phase constituent mainly by the newborn solution of lighting up of the mixing that contains 3# solvent-pitch-heavy hydrocarbon on a small quantity.
In Fig. 7, extracting and refining crude phenols filtering tank 34 comprises a withstand voltage kettle, is covered with extraction refining of crude phenol mixed material feeding mouth 33 on the withstand voltage kettle, and withstand voltage kettle bottom is provided with extraction refining of crude phenol mixed material discharging opening 34 and constitutes.
The material inlet 33 that last phase constituent (2# solvent-mixed phenol) in the refining crude phenols still 29 of No. 3 solvent extractions is provided with through extracting and refining crude phenols filtering tank 34 loam cakes middle part behind the discharging opening 31 of the refining crude phenols still 29 kettle upper right quarters of No. 3 solvent extractions again enters filtering tank 34, utilizes external force to filter the granule foreign of removing minute quantity in filtering tank.2# solvent behind the removal impurity-refining phenols that mixes directly enters No. 3 extractant concentration kettle 36 of extracting and refining crude phenols through filtering tank 34 middle and lower part material outlets 35.Gap in test, phase constituent (3# solvent-pitch-heavy hydrocarbon) enters filtering tank 34 at the material inlet 33 that extracting and refining crude phenols filtering tank 34 is provided with through extracting and refining crude phenols filtering tank 34 loam cakes middle part again under in the refining crude phenols still 29 of a small amount of No. 3 solvent extractions behind the discharging opening 32 of kettle middle and lower part, utilizes external force to filter the pitch impurity of removing minute quantity in filtering tank.3# solvent-heavy hydrocarbon behind the removal pitch directly enters No. 3 extractant concentration kettle 36 of extracting and refining crude phenols through filtering tank 34 middle and lower part material outlets 35.Test shows: extracting and refining crude phenols filtering tank 34 can be removed ultra-fine powder well, helps the purity that improves crude phenols.
In Fig. 8, No. 3 extractant concentration kettle 36 of extracting and refining crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus 1 and the thermocouple 5 that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil 2 in the autoclave body, the top cover upper left side of pressure kettle is provided with extraction refining of crude phenol mixed material feeding mouth and No. 3 solvent material entrances 37, upper right sides and is provided with material outlet 38, Pressure gauge 6 is provided with visual windows 9 in the kettle, the middle and lower part of kettle is provided with the discharging opening 39 that concentrates crude phenols respectively and constitutes.
Refining mixing phenols after being rich in the 2# solvent and removing pitch is through filtering tank 34 middle and lower part material outlets 35, and the material feeding mouth 37 that is provided with through No. 3 extractant concentration kettle of extracting and refining crude phenols 36 upper left sidepieces directly enters in the still again.Under magnetic stirring apparatus 1 slowly stirs, utilize heat(ing) coil 2 and thermocouple 5, control No. 3 interior temperature maintenance of extractant concentration kettle 36 kettlies about 800C-1200C, 2# solvent constantly gasification enters condenser for behind the steam from No. 3 condenser 45-3 charging apertures 40, directly enters the jar from No. 2 solvent tank 26 middle and upper part material inlets 27 from No. 3 condenser 45-3 discharging openings 41 process pipelines through condensed 2# solvent.Emit refining mixed phenol product from the discharging opening of the middle and lower part of No. 3 extractant concentration kettle 36 of extracting and refining crude phenols.In the gap of test, on a small quantity from the refining crude phenols still 29 of No. 3 solvent extractions down the material inlet 33 that is provided with through extracting and refining crude phenols filtering tank 34 loam cakes middle part of phase constituent (3# solvent-pitch-heavy hydrocarbon) enter filtering tank 34 again and remove the material inlet valve 37 that is provided with through No. 3 extractant concentration kettle of extracting and refining crude phenols 36 upper left sidepieces again behind the pitch impurity of minute quantities and directly enter in the still.Under magnetic stirring apparatus 1 slowly stirs, utilize heat(ing) coil 2 and thermocouple 5, temperature maintenance is about 400C-800C in the control kettle, two flowers of sulfur carbon constantly gasification enter condenser for behind the steam from No. 3 condenser 45-3 charging apertures 40, directly enter the jar from No. 2 solvent tank 26 middle and upper part material inlets 27 through pipeline from No. 3 condenser 45-3 discharging openings process triple valves through condensed 2# solvent.Directly enter the jar from No. 3 solvent tank 43 middle and upper part material inlets 42 through pipeline from No. 3 condenser 45-3 discharging openings 41 through condensed 3# solvent.Emit the heavy hydrocarbon product from the discharging opening of the middle and lower part of No. 3 extractant concentration kettle 36 of extracting and refining crude phenols.Test is found: utilize the mixing aldehydes matter in the further high-purity meticulous separation in ground of this equipment, the enrichment coalite tar, the concentration effect at the bottom of still of the phenols hydrocarbon in the middle coalite tar is obvious and have a very high yield.Utilize this equipment solvent distillation to have the very high rate of recovery and can use repeatedly, the mixing phenols in the middle coalite tar and heavy hydrocarbon concentration effect are obviously and have a very high yield.
In Fig. 9, No. 3 solvent tank 43 comprises a normal pressure jar, and normal pressure jar middle and upper part is provided with the feeding mouth 42 of No. 3 solvents that the device condensation that is condensed gets off, and the middle and lower part is provided with No. 3 solvent discharging openings 44 and constitutes.
From the feeding mouth 42 of No. 3 condenser 45-3 discharging openings 41 through No. 3 solvent tanks 43, directly enter through condensed 3# solvent, use repeatedly through the feeding mouth 37 that No. 3 solvent tank 43 middle and lower part discharging openings 44 flow into No. 3 extractant concentration kettle 36 upper left quarters of extracting and refining crude phenols again as new extractant through external influence power 3# solvent as required.Test is found: utilize this equipment distillation 3# solvent to have very high cooling, recovering effect and can use repeatedly.
In Figure 10-1, Figure 10-2, Figure 10-3,1-No. 3 groups comprise that the shell and tube condenser that four sizes do not wait, condenser comprise the discharging opening of material after the material charging aperture that is condensed and the condensation; No. 1 condenser 45-1 has charging aperture 15 and discharging opening 16; No. 2 condenser 45-2 has charging aperture 24 and discharging opening 25; No. 3 condenser 45-3 has charging aperture 40 and discharging opening 41 to constitute.

Claims (10)

1. the complete set of equipments of phenols in the coalite tar in the extraction separation and Extraction, it is characterized in that: carry the complete set of equipments of phenol in the middle coalite tar, it is made up of five stills, four jars and three groups of condensers; It is respectively middle coalite tar extract and separate still; No. 1 extractant concentration kettle of extraction light oil; No. 1 solvent tank; No. 2 extractant concentration kettle of extraction crude phenols; No. 2 solvent tanks; The crude phenols still is made with extra care in No. 3 solvent extractions; Extracting and refining crude phenols filtering tank; Extracting and refining crude phenols extractant concentration kettle; No. 3 solvent tanks and No. 1 condenser, No. 2 condensers and No. 3 condensers;
Upper right sidepiece discharging opening links to each other with the upper left side feeding mouth pipeline of extraction light oil extractant concentration kettle in the middle coalite tar extract and separate still, and the middle part discharging opening links to each other with the feeding mouth pipeline of the refining crude phenols still upper left side of No. 3 solvent extractions under the middle coalite tar extract and separate still; The discharging opening of No. 1 extractant concentration kettle of extraction light oil upper right side is connected with the feeding mouth pipeline of No. 1 condenser, and No. 2 extractant concentration kettle of the discharging opening at middle part and extraction crude phenols upper left side feeding mouth pipeline is connected under No. 1 extractant concentration kettle of extraction light oil; No. 1 condenser discharging opening is connected with middle part feeding mouth pipeline on No. 1 solvent tank, and the middle part discharging opening is connected with the discharging opening pipeline of middle coalite tar extract and separate still upper right side under No. 1 solvent tank; The feeding mouth of extraction crude phenols extractant concentration kettle upper left side respectively with No. 1 extractant concentration kettle of extraction light oil under the discharging opening at middle part and No. 2 solvent tanks discharging opening pipeline at middle part be connected, the discharging opening of No. 2 extractant concentration kettle of extraction crude phenols upper right side is connected with No. 2 condenser feeding mouth pipelines, and the material outlet of No. 2 extractant concentration kettle of extraction crude phenols middle and lower part directly is connected with the refining crude phenols still feeding mouth of No. 3 solvent extractions; The feeding mouth road at middle part is connected on No. 2 condenser discharging opening pipes and No. 2 solvent tanks, the discharging opening at middle part is connected with the feeding mouth pipeline that crude phenols still upper left side is made with extra care in No. 3 solvent extractions under No. 2 solvent tanks, the refining crude phenols still upper right quarter discharging opening of No. 3 solvent extractions is connected with the middle part feeding mouth pipeline of going up of extracting and refining crude phenols filtering tank, and the discharging opening by middle part under the refining crude phenols still of No. 3 solvent extractions of triple valve is connected with the middle part feeding mouth pipeline of going up of extracting and refining crude phenols filtering tank simultaneously; The following middle part discharging opening of extracting and refining crude phenols filtering tank is connected with the feeding mouth pipeline of extracting and refining crude phenols extractant concentration kettle upper left side; The discharging opening of No. 3 extractant concentration kettle of extracting and refining crude phenols upper right side is connected with No. 3 condenser feeding mouth pipelines; No. 3 the condenser discharging opening is connected with the feeding mouth pipeline on No. 3 solvent tank tops; The discharging opening of No. 3 solvent tank bottoms is connected with the feeding mouth pipeline of the refining crude phenols still upper right side of No. 3 solvent extractions.
2. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: coalite tar extract and separate still comprises a withstand voltage kettle in described, be covered with the magnetic stirring apparatus that leads in the kettle on the withstand voltage kettle, thermocouple, be provided with heat(ing) coil in the autoclave body, inlay the liftable filter of filter membrane mesh, the autoclave body top cover is provided with No. 1 extractant and No. 2 extractant material inlets at upper left sidepiece, also be provided with Pressure gauge, upper right sidepiece is provided with discharging opening, be provided with visual windows in the pressure kettle, the middle part is provided with material outlet under the still.
3. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: No. 1 extractant concentration kettle of described extraction light oil comprises a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the upper left side is provided with light oil and No. 1 solvent material entrance that obtains with coalite tar in the extraction on the top cover of pressure kettle, upper right sidepiece is provided with discharging opening, Pressure gauge, be provided with visual windows in the kettle, the lower middle portion of kettle is not provided with the discharging opening that concentrates light oil.
4. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: described No. 1 solvent tank comprises a normal pressure jar, normal pressure jar middle and upper part is provided with No. 1 solvent feeding mouth of condensation, and following middle part is provided with the solvent discharging opening No. 1; Described No. 2 solvent tanks comprise a normal pressure jar, and the normal pressure jar is provided with the feeding mouth of No. 2 solvents that condenser condenses gets off, and the bottom is provided with the solvent discharging opening No. 2.
5. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: No. 2 extractant concentration kettle of described extraction crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the top cover left upper portion of pressure kettle is provided with crude phenols and No. 2 solvent material entrances that obtain for the extraction coalite tar, right upper portion is provided with material outlet, Pressure gauge, be provided with visual windows in the kettle, the lower middle bottom of kettle is provided with the discharging opening that concentrates crude phenols.
6. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: described No. 2 solvent tanks comprise a normal pressure jar, the normal pressure jar is provided with the feeding mouth valve of No. 2 solvents that condenser condenses gets off, and the bottom is provided with the solvent discharging opening No. 2; The refining crude phenols still of described No. 3 solvent extractions comprises a withstand voltage kettle, is covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, is provided with the liftable filter of inlaying the filter membrane mesh in the autoclave body, heat(ing) coil; The feeding mouth of coalite tar and No. 2 extractants during the upper left side is provided with on the top cover of pressure kettle, upper right side are provided with extraction mixed material discharging opening, Pressure gauge, are provided with visual windows in the kettle, and the kettle middle and lower part is provided with extraction refining of crude phenol mixed material discharging opening.
7. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: described extracting and refining crude phenols filtering tank comprises a withstand voltage kettle, be covered with extraction refining of crude phenol mixed material feeding mouth on the withstand voltage kettle, withstand voltage kettle bottom is provided with extraction refining of crude phenol mixed material discharging opening.
8. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: No. 3 extractant concentration kettle of described extracting and refining crude phenols comprise a withstand voltage kettle, be covered with the magnetic stirring apparatus and the thermocouple that lead in the kettle on the withstand voltage kettle, be provided with heat(ing) coil in the autoclave body, the top cover upper left side of pressure kettle is provided with extraction refining of crude phenol mixed material feeding mouth and No. 3 solvent material entrances, the upper right side is provided with material outlet, Pressure gauge, be provided with visual windows in the kettle, the middle and lower part of kettle is provided with the discharging opening that concentrates crude phenols respectively.
9. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: described No. 3 solvent tanks comprise a normal pressure jar, normal pressure jar middle and upper part is provided with the feeding mouth of number solvent that the device condensation that is condensed gets off, and the middle and lower part is provided with the solvent discharging opening No. 3.
10. the complete set of equipments of phenols in the coalite tar in a kind of extraction separation and Extraction according to claim 1, it is characterized in that: described No. 1 condenser, No. 2 condensers and No. 3 condensers are three shell and tube condensers that size does not wait, and condenser comprises the discharging opening of material after the material charging aperture that is condensed and the condensation; No. 1 condenser has charging aperture and discharging opening; No. 2 condenser has charging aperture and discharging opening; No. 3 condenser has charging aperture and discharging opening.
CN 201320070977 2013-02-07 2013-02-07 Complete equipment for separating and extracting phenols in middle-temperature and low-temperature coal tar by extraction method Expired - Lifetime CN203139681U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103111088A (en) * 2013-02-07 2013-05-22 陕西煤业化工技术研究院有限责任公司 Complete equipment for extracting phenols in medium and low temperature coal tar
CN104324519A (en) * 2014-11-04 2015-02-04 中国科学院过程工程研究所 Method for directly separating phenols from coal pyrolytic oil
WO2015076974A1 (en) * 2013-11-19 2015-05-28 Uop Llc Process for removing ash and heavy hydrocarbons from coal tar
CN105112084A (en) * 2015-09-16 2015-12-02 陕西煤业化工技术研究院有限责任公司 Device and method for extracting phenol products from medium-low temperature coal tar

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103111088A (en) * 2013-02-07 2013-05-22 陕西煤业化工技术研究院有限责任公司 Complete equipment for extracting phenols in medium and low temperature coal tar
WO2015076974A1 (en) * 2013-11-19 2015-05-28 Uop Llc Process for removing ash and heavy hydrocarbons from coal tar
CN104324519A (en) * 2014-11-04 2015-02-04 中国科学院过程工程研究所 Method for directly separating phenols from coal pyrolytic oil
CN105112084A (en) * 2015-09-16 2015-12-02 陕西煤业化工技术研究院有限责任公司 Device and method for extracting phenol products from medium-low temperature coal tar

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