CN110003939A - A kind of efficient carbolic oil dephenolization method - Google Patents
A kind of efficient carbolic oil dephenolization method Download PDFInfo
- Publication number
- CN110003939A CN110003939A CN201910361755.7A CN201910361755A CN110003939A CN 110003939 A CN110003939 A CN 110003939A CN 201910361755 A CN201910361755 A CN 201910361755A CN 110003939 A CN110003939 A CN 110003939A
- Authority
- CN
- China
- Prior art keywords
- extractant
- tower
- water
- phenol
- carbolic oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 36
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 150000002989 phenols Chemical class 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000605 extraction Methods 0.000 claims abstract description 30
- -1 phenols compounds Chemical class 0.000 claims abstract description 5
- 238000004064 recycling Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000002904 solvent Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 6
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 6
- 229940043265 methyl isobutyl ketone Drugs 0.000 claims description 6
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical group CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 14
- 239000011280 coal tar Substances 0.000 abstract description 13
- 150000001896 cresols Chemical class 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000011269 tar Substances 0.000 abstract description 5
- 238000000638 solvent extraction Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 19
- 238000012360 testing method Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 6
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 229930003836 cresol Natural products 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to coal tar processing technology fields, disclose a kind of efficient carbolic oil dephenolization method, this method uses double solvent extraction technology, the small molecular alcohol of selection is to the selective dissolution of rudimentary phenol, the small molecular alcohol dissolved in the thick dephenolize oil of raffinate phase circulating repetition can use after distillation is directly separated recycling, extractant loses very little, and the rate of recovery is high, reduces operating cost；This method suitable for high temperature coal-tar carbolic oil fraction and in coalite tar carbolic oil fraction phenolic compound separation, particularly with the extraction of the rudimentary phenol such as phenol, cresols, the rate of recovery of phenolic compound is up to 89% or more, achieved the purpose that efficiently, separating phenols compounds with high selectivity, and there is no pollutant emission.
Description
Technical field
The invention belongs to coal tar processing technology fields, and in particular to a kind of efficient carbolic oil dephenolization method.
Background technique
Contain multi-chemical in coal tar, for a long time, the resource always as a kind of speciality chemical is domestic and international
Enterprise development and utilization.Rudimentary phenol is one of the staple product separated from coal tar, since the molecule of phenol is weakly acidic,
So with acid-base method (react with phenol generation sodium phenolate with sodium hydroxide solution, sodium phenolate is reduced into phenol by stronger acids again, finally from
Coal tar isolates phenolic compound in fraction containing phenol) it is easy to isolate rudimentary phenolic product from coal tar, this method tool
There are the advantages such as phenol high income, process are simple, operating cost is low, is applied in industrial production always, but the disadvantage is that produce in the process
Raw reluctant acid sludge, alkaline residue.Increasingly stringent with environmental requirement, the shortcomings that acid-base method, shows more prominent, in order to
Meet current environmental requirement, people start to develop new separation phenol technology over the past decade, and new technology is broadly divided into two sides
To --- acid-base method technological improvement and non-acid-base method separate phenol technology, wherein improved acid-base method is only the reduction of pollutant
Discharge amount, be not fully solved the emission problem of alkaline residue and acid sludge, and most of non-acid-base method separation phenol technologies are without dirt
Object discharge is contaminated, the technology of environment-friendly type is belonged to.
Non- acid-base method phenol technology be can be separated according to the information having disclosed and solvent extraction, ion liquid abstraction are divided into
Method, superheated vapour abstraction technique etc..Although non-soda acid separation phenol technology solves the emission problem of pollutant, different skills
Art still has certain.Wherein solvent used in solvent extraction has glycerine, diethanol amine, small molecule organic amine
Aqueous solution and ammonium hydroxide, the aqueous solution of some inorganic salts etc., due to the limitation of selected solvent and process flow, this kind of skill
The shortcomings such as that all there is phenolic compound yields is low for art, extraction efficiency is low, and that there are also solvent losses is big, raw for some technologies
Produce the problems such as costly；Ion liquid abstraction technology can obtain relatively high phenolic compound selectivity, but due to ionic liquid
Higher cost, regeneration expense and consumption are likely to result in this kind of technology producing cost height, to influence its economy；Overheat
Water vapour abstraction technique needs to operate at a higher temperature, and one side energy consumption is higher, on the other hand since used water steams
Oil gas is mixed in vapour, water supply steam circulation use brings difficulty.
Summary of the invention
The purpose of the present invention is to provide a kind of efficient carbolic oil dephenolization method, reaches and divided efficiently, with high selectivity
Purpose from phenolic compound, and there is no pollutant emission.
To achieve the above object, the invention adopts the following technical scheme:
The present invention provides a kind of efficient carbolic oil dephenolization method, comprising the following steps:
Carbolic oil and extractant A are sent into extraction tower and carry out counter-current extraction, extraction phase solvent A containing phenol is obtained and raffinate phase slightly takes off
The volume ratio of carbolic oil, the extractant A and carbolic oil is 0.1~10:1, and extraction temperature is 20~80 DEG C, extracting pressure is normal
Pressure, extractant A are the aqueous solution of small molecular alcohol, and the concentration containing small molecular alcohol is 10~90wt% in extractant；
The thick dephenolize oil of raffinate phase is sent into stripping tower I after flowing out from the top of extraction tower, removes in stripping tower I by air lift
The small molecular alcohol dissolved in the thick dephenolize oil of raffinate phase obtains dephenolize oil, and the dephenolize oil flowed out from stripping tower I tower bottom is sent as product
Outside out-of-bounds, the small molecular alcohol come out from stripping tower I tower top is recycled after being condensed for configuring extractant A；
The extraction phase solvent A containing phenol is sent into dealcoholysis tower after exchanging heat, and is distilled in dealcoholysis tower by small molecular alcohol and water and phenol
Class compound separates, and the small molecular alcohol flowed out from dealcoholysis column overhead is used to configure extractant A after being condensed, from dealcoholysis tower tower
The water of bottom outflow and the mixed liquor of phenolic compound enter separator after heat exchange is cooled to 35~40 DEG C and are divided into water containing phenol and phenol
Class compound, phenolic compound are sent out out-of-bounds as crude phenols product, and water containing phenol is admitted to stripping column；
Water containing phenol from separator and extractant B are sent into stripping column and carry out counter-current extraction, the extractant B with contain phenol
The volume ratio of water is 5~50:100, and the dephenolize water flowed out from stripping column bottom enters stripping tower II extractant B after air lift
It is separated with water, wherein extractant B is recycled, and water is for preparing extractant A recycling；At the top of from stripping column
The B of solvent containing phenol of outflow is sent into destilling tower, and phenolic compound and extractant B after distilling in the B of solvent containing phenol are separated,
Wherein phenolic compound is sent out out-of-bounds as crude phenols product, and extractant B is recycled；The extraction temperature of stripping column is 50
DEG C, extracting pressure be normal pressure.
Preferably, the volume ratio of the extractant A and carbolic oil is 0.8~5:1.
Preferably, the concentration of the extractant A is 20~80wt%.
Preferably, the extractant A is methanol aqueous solution or ethanol water or methanol aqueous solution and ethanol water
Mixture.
Preferably, the extractant B is Di Iso Propyl Ether or methyl iso-butyl ketone (MIBK).
Preferably, the volume ratio of the extractant B and the water containing phenol is 5~20:100.
Compared with prior art, the beneficial effects of the present invention are:
The present invention uses double solvent extraction technology, develops suitable process flow, has reached efficient, has separated phenol with high selectivity
The purpose of class compound, and there is no pollutant emission；The small molecular alcohol of selection extracts molten the selective dissolution of rudimentary phenol
Circulating repetition uses after agent A and extractant B can be recycled, and extractant loses very little, reduces operating cost；This method is suitable
For the separation of phenolic compound in high temperature coal-tar carbolic oil distillate and middle coalite tar carbolic oil fraction, particularly with benzene
The extraction of the rudimentary phenol such as phenol, cresols, the rate of recovery of phenolic compound is up to 89% or more.
Detailed description of the invention
Fig. 1 is a kind of efficient carbolic oil dephenolization method flow diagram of the present invention.
It is attached marked in the figure: 1 be extraction tower, 2 be stripping tower I, 3 be dealcoholysis tower, 4 be separator, and 5 be stripping column, and 6 be gas
Stripper II, 7 be destilling tower.
Specific embodiment
The following examples are intended to illustrate the invention, but is not used to limit the scope of protection of the present invention.Unless otherwise specified, real
Apply the conventional means that technological means used in example is well known to those skilled in the art.Test method in following embodiments, such as
It is conventional method without special instruction.
The test process and test method of embodiment are as follows:
The present embodiment is respectively with low temperature in table mountain high temperature coal-tar carbolic oil distillate (170~210 DEG C of fractions) and Yulin
Coal tar carbolic oil fraction (170~210 DEG C of fractions) is feedstock oil, and composition and property are listed in Tables 1 and 2 respectively, are testing
It is tested on device, the process flow of experimental provision is as shown in Figure 1, i.e. respectively with methanol aqueous solution, ethanol water or first
The mixture of alcohol solution and ethanol water exists as extractant A, the concentration control of extractant small molecular alcohol
Two levels of 50wt% and 75wt%, extractant A and carbolic oil carry out counter-current extraction, the diameter of extraction tower 1 in extraction tower 1
For 100mm, height 3000mm, theoretical cam curve 15, at 50 DEG C, 1 pressure of extraction tower is normal pressure for extraction temperature control.
The thick dephenolize oil of raffinate phase is sent into stripping tower I2 after flowing out from the top of extraction tower 1 (stripping tower I2 is packed tower, internal diameter
150mm, height 1500mm), it is obtained in stripping tower I2 by the small molecular alcohol dissolved in the thick dephenolize oil of air lift removing raffinate phase
Dephenolize oil, when methanol aqueous solution is as extractant A, stripping tower I2 pushes up temperature and controls at 60~70 DEG C, stripping tower I2 tower top
Methanol send to solvent circulating tank through condensation and is recycled for preparing extractant A, and stripping tower I2 tower bottom dephenolize oil is as product
Device out；When ethanol water is as extractant A, the control of stripping tower I2 tower top temperature is at 75~85 DEG C, stripping tower I2 tower
Ethyl alcohol is obtained after the condensation of top gas body to send to solvent circulating tank for preparing extractant A recycling, stripping tower I2 tower bottom dephenolize
Oil goes out device as product；When the mixture of methanol aqueous solution and ethanol water is as extractant A, stripping tower I2 tower top
Temperature control obtains methanol after 75~85 DEG C, the condensation of stripping tower I2 overhead gas and the mixture of ethyl alcohol is sent to solvent circulating tank
Extractant A is prepared, stripping tower I2 tower bottom dephenolize oil goes out device as product.
Extraction phase solvent A containing phenol is sent into dealcoholysis tower 3 after exchanging heat, and in dealcoholysis tower 3, (desolventizing tower 3 is packed tower, internal diameter
150mm, packed height 1600mm) in small molecular alcohol and water and phenolic compound are separated through distilling, from 3 tower top stream of dealcoholysis tower
Small molecular alcohol out is recycled after being condensed for preparing extractant A.When methanol aqueous solution is as extractant A, take off
At 65~75 DEG C, the methanol of removing flows out the control of 3 tower top temperature of alcohol tower from tower top, is sent after condensing to solvent circulating tank for matching
Extractant A processed is recycled, and the mixed liquor of tower bottom water and phenolic compound is sent after heat exchange is cooled to 35~40 DEG C to separation
Device 4 is divided into water containing phenol (water phase) and phenolic compound (phenol phase) in separator 4, and wherein phenol is mutually used as product carrying device, water
Mutually send to stripping column 5 (stripping column 5 internal diameter 100mm, height 3000mm, theoretical cam curve 15, extraction temperature are 50 DEG C,
Extracting pressure is normal pressure)；When ethanol water is as extractant A, the control of 3 tower top temperature of dealcoholysis tower is at 80~90 DEG C, tower
It obtains hydrous ethanol (concentration of alcohol about 95w%) after the condensation of top gas body and send to solvent circulating tank to follow for preparing extractant A
Ring uses, and the mixed liquor of tower bottom water and phenolic compound is sent after heat exchange is cooled to 35~40 DEG C to separator 4, in separator 4
In be divided into water containing phenol (water phase) and phenolic compound (phenol phase), wherein phenol is mutually used as product carrying device, and water phase is sent to back extraction
Tower 5；When the mixture of methanol aqueous solution and ethanol water is as extractant A, the control of 3 tower top temperature of dealcoholysis tower 80~
90 DEG C, methanol, ethyl alcohol and a small amount of water (methanol and concentration of alcohol are greater than 95w%) are obtained after overhead gas condensation and send to solvent and recycles
Tank is recycled for preparing extractant A, and the mixed liquor of tower bottom water and phenolic compound is after heat exchange is cooled to 35~40 DEG C
It send to separator 4, water containing phenol (water phase) and phenolic compound (phenol phase) is divided into separator 4, wherein phenol is mutually sent as product
Device out, water phase are sent to stripping column 5.
Entering the top of stripping column 5 from the water containing phenol of separator 4, extractant B enters the lower part of stripping column 5,
The volume flow of water containing phenol and extractant B are controlled in two levels of 100:5 and 100:20, the B of solvent containing phenol after counter-current extraction
It flows out, is sent to destilling tower 7 (destilling tower 7 is packed tower, internal diameter 150mm, packed height 1600mm) through steaming at the top of stripping column 5
Phenolic compound and extractant B are obtained after evaporating, wherein molten extractant B is recycled, phenolic compound goes out as crude phenols product
Device；The dephenolize water flowed out from 5 bottom of stripping column, into stripping tower II6, (stripping tower II6 is packed tower, and internal diameter 150mm is filled out
Expect height 1500mm), through extractant B a small amount of in air lift removing water, wherein extractant B is recycled, and water is for preparing
Extractant A is recycled.When diisopropyl ether is as extractant B, stripping tower II6 head temperature and distillation tower top temperature control
System is within the scope of 55~65 DEG C；When methyl iso-butyl ketone (MIBK) is as extractant B, stripping tower II6 head temperature and distillation tower top
Temperature controls within the scope of 80~90 DEG C.
The composition and property of 1 table mountain high temperature coal-tar carbolic oil distillate of table
| Project | Index | Elemental analysis, wt% | Index |
| Density (20 DEG C), kg/m3 | 982.0 | C | 88.99 |
| Rudimentary phenol content, wt% | 11.31 | H | 6.90 |
| Wherein: phenol content, wt% | 3.13 | S | 0.53 |
| Cresol content, wt% | 5.95 | N | 0.73 |
| Diformazan phenol content, wt% | 2.22 | O | 2.85 |
The composition and property of coalite tar carbolic oil fraction in 2 Yulin of table
| Project | Index | Elemental analysis, wt% | Index |
| Density (20 DEG C), kg/m3 | 937.6 | C | 85.03 |
| Rudimentary phenol content, wt% | 35.10 | H | 6.98 |
| Wherein: phenol content, wt% | 6.40 | S | 0.41 |
| Cresol content, wt% | 19.34 | N | 0.76 |
| Diformazan phenol content, wt% | 9.36 | O | 6.82 |
Embodiment 1-5
According to above-mentioned test process and test method, arranged by the test result of raw material of table mountain high temperature coal-tar carbolic oil distillate
In table 3.
Test result of the table 3 using table mountain high temperature coal-tar carbolic oil distillate as raw material at different conditions
Note: phenol in the sum of phenol, cresols, xylenol amount/raw material carbolic oil in the rudimentary phenol rate of recovery=crude phenols product, cresols,
The sum of xylenol amount * 100；The sum of phenol, cresols, concentration of xylenol in rudimentary phenol selectivity=crude phenols product.
Embodiment 6-10
According to above-mentioned test process and test method, using coalite tar carbolic oil fraction in Yulin as the test knot of raw material
Fruit is listed in table 4.
Table 4 is using test result of the coalite tar carbolic oil fraction as raw material at different conditions in Yulin
Note: phenol, cresols in the sum of phenol, cresols and xylenol amount/raw material carbolic oil in the rudimentary phenol rate of recovery=crude phenols product
With the sum of xylenol amount * 100；The sum of phenol, cresols and concentration of xylenol in rudimentary phenol selectivity=crude phenols product.
The embodiment of the above, only presently preferred embodiments of the present invention, is only used to explain the present invention, not limit
The scope of the present invention processed to those of ordinary skill in the art certainly can be according to skill disclosed in this specification
Art content makes other embodiments easily by way of replacing or changing, therefore all made in the principle of the present invention
Changes and improvements etc., should be included in scope of the present invention patent.
Claims (6)
1. a kind of efficient carbolic oil dephenolization method, which comprises the following steps:
Carbolic oil and extractant A are sent into extraction tower and carry out counter-current extraction, extraction phase solvent A containing phenol is obtained and raffinate phase slightly takes off
The volume ratio of carbolic oil, the extractant A and carbolic oil is 0.1 ~ 10:1, and extraction temperature is 20 ~ 80 DEG C, extracting pressure is normal
Pressure, extractant A are the aqueous solution of small molecular alcohol, and the concentration containing small molecular alcohol is 10 ~ 90wt% in extractant；
The thick dephenolize oil of raffinate phase is sent into stripping tower I after flowing out from the top of extraction tower, removes in stripping tower I by air lift
The small molecular alcohol dissolved in the thick dephenolize oil of raffinate phase obtains dephenolize oil, and the dephenolize oil flowed out from stripping tower I tower bottom is sent as product
Outside out-of-bounds, the small molecular alcohol come out from stripping tower I tower top is recycled after being condensed for configuring extractant A；
The extraction phase solvent A containing phenol is sent into dealcoholysis tower after exchanging heat, and is distilled in dealcoholysis tower by small molecular alcohol and water and phenol
Class compound separates, and the small molecular alcohol flowed out from dealcoholysis column overhead is used to configure extractant A after being condensed, from dealcoholysis tower tower
The water of bottom outflow and the mixed liquor of phenolic compound enter separator after heat exchange is cooled to 35 ~ 40 DEG C and are divided into water containing phenol and phenols
Compound, wherein phenolic compound is sent out out-of-bounds as crude phenols product, and water containing phenol is admitted to stripping column；
Water containing phenol from separator and extractant B are sent into stripping column and carry out counter-current extraction, the extractant B with contain phenol
The volume ratio of water is 5 ~ 50:100, and the dephenolize water flowed out from stripping column bottom enters stripping tower II extractant B after air lift
It is separated with water, wherein extractant B is recycled, water is for preparing extractant A recycling；At the top of from stripping column
The B of solvent containing phenol of outflow is sent into destilling tower, and phenolic compound and extractant B after distilling in the B of solvent containing phenol are separated,
Wherein phenolic compound is sent out out-of-bounds as crude phenols product, and extractant B is recycled；The extraction temperature of stripping column is 50
DEG C, extracting pressure be normal pressure.
2. a kind of efficient carbolic oil dephenolization method according to claim 1, which is characterized in that the extractant A and
The volume ratio of carbolic oil is 0.8 ~ 5:1.
3. a kind of efficient carbolic oil dephenolization method according to claim 1, which is characterized in that the extractant A's
Concentration is 20 ~ 80wt%.
4. a kind of efficient carbolic oil dephenolization method according to claim 1, which is characterized in that the extractant A is
The mixture of methanol aqueous solution or ethanol water or methanol aqueous solution and ethanol water.
5. a kind of efficient carbolic oil dephenolization method according to claim 1, which is characterized in that the extractant B is
Di Iso Propyl Ether or methyl iso-butyl ketone (MIBK).
6. a kind of efficient carbolic oil dephenolization method according to claim 1, which is characterized in that the extractant B with
The volume ratio of the water containing phenol is 5 ~ 20:100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910361755.7A CN110003939A (en) | 2019-04-30 | 2019-04-30 | A kind of efficient carbolic oil dephenolization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910361755.7A CN110003939A (en) | 2019-04-30 | 2019-04-30 | A kind of efficient carbolic oil dephenolization method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110003939A true CN110003939A (en) | 2019-07-12 |
Family
ID=67175299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910361755.7A Pending CN110003939A (en) | 2019-04-30 | 2019-04-30 | A kind of efficient carbolic oil dephenolization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110003939A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627623A (en) * | 2019-09-06 | 2019-12-31 | 陕西煤业化工集团神木天元化工有限公司 | Separation system and method for alkaline nitride in phenol product |
| CN113817490A (en) * | 2021-10-18 | 2021-12-21 | 胜帮科技股份有限公司 | Coupling device and coupling process for coal tar phenol extraction and phenol-containing water treatment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000044699A1 (en) * | 1999-01-29 | 2000-08-03 | Ecovac Pyrocycling Technologies Inc. | Process for the production of phenolic-rich pyrolysis oils for use in making phenol-formaldehyde resol resins |
| JP2002047226A (en) * | 2000-07-26 | 2002-02-12 | National Institute Of Advanced Industrial & Technology | Method for separating and recovering phenol compound and hydrocarbon oil from mixture containing the components |
| CN102219649A (en) * | 2011-04-22 | 2011-10-19 | 煤炭科学研究总院 | Method of extracting phenolic compound from coal liquefied oil or coal tar |
| CN106278827A (en) * | 2016-07-22 | 2017-01-04 | 煤炭科学技术研究院有限公司 | A kind of method and device of extract and separate phenolic compound from coal derived oils |
-
2019
- 2019-04-30 CN CN201910361755.7A patent/CN110003939A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000044699A1 (en) * | 1999-01-29 | 2000-08-03 | Ecovac Pyrocycling Technologies Inc. | Process for the production of phenolic-rich pyrolysis oils for use in making phenol-formaldehyde resol resins |
| JP2002047226A (en) * | 2000-07-26 | 2002-02-12 | National Institute Of Advanced Industrial & Technology | Method for separating and recovering phenol compound and hydrocarbon oil from mixture containing the components |
| CN102219649A (en) * | 2011-04-22 | 2011-10-19 | 煤炭科学研究总院 | Method of extracting phenolic compound from coal liquefied oil or coal tar |
| CN106278827A (en) * | 2016-07-22 | 2017-01-04 | 煤炭科学技术研究院有限公司 | A kind of method and device of extract and separate phenolic compound from coal derived oils |
Non-Patent Citations (3)
| Title |
|---|
| 中国化工防治污染技术协会: "《化工废水处理技术》", 28 April 2000, 化学工业出版社 * |
| 尚建选等: "《低阶煤分质转化多联产技术》", 31 May 2013, 煤炭工业出版社 * |
| 张明等: "《煤制合成天然气技术与应用》", 31 October 2017, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627623A (en) * | 2019-09-06 | 2019-12-31 | 陕西煤业化工集团神木天元化工有限公司 | Separation system and method for alkaline nitride in phenol product |
| CN113817490A (en) * | 2021-10-18 | 2021-12-21 | 胜帮科技股份有限公司 | Coupling device and coupling process for coal tar phenol extraction and phenol-containing water treatment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106588579B (en) | A method of extracting phenolic compound from carbolic oil | |
| CN101143805B (en) | Method for separating phenols compounds from phenol-containing raw material oil | |
| CN105016554A (en) | Semi-coke wastewater treatment process | |
| CN102633597B (en) | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture | |
| CN103896739B (en) | Method for extracting phenol compounds from direct coal liquefied oil through extractive distillation | |
| CN110003939A (en) | A kind of efficient carbolic oil dephenolization method | |
| CN103435482A (en) | Separation method and separation device of synthesis gas ethylene glycol product | |
| CN103752158A (en) | Method for treating glyphosate hydrolyzing tail gas | |
| CN103788026A (en) | Method of purifying propylene epoxide | |
| CN105198711A (en) | Coked crude phenol refining device and method | |
| CN109942492A (en) | A kind of caprolactam refining technique | |
| CN110015949B (en) | Method for extracting phenolic substances from raw oil containing phenol | |
| CN104946303A (en) | Method for selectively separating phenol mixture from oil | |
| CN103145286A (en) | Pre-treatment method of high-concentration wastewater | |
| CN105602613B (en) | The method of phenol, aromatic hydrocarbons and alkane in one-step method separation coal direct liquefaction oil | |
| CN106044918A (en) | Coal gasification wastewater treatment system and process with thermally coupled auxiliary reboiling and rectifying columns | |
| CN100447120C (en) | Technological process for refining trimethylolpropane | |
| CN102634381B (en) | System and method for treating benzene-contained separating water of coking benzol | |
| CN102351358B (en) | Method and system for treating phenol-containing acidic water by direct liquefaction with coal | |
| CN109825322A (en) | A method of extracting phenolic substances from coal tar or coal direct liquefaction oil | |
| CN110003941A (en) | A kind of solvent dephenolization method of mixed triolein or long distillate carbolic oil | |
| CN110668910B (en) | Benzene distillation residue recovery device, recovery method and application | |
| CN101870529A (en) | Method for treating phenolic wastewater in smashed coal pressure gasification | |
| CN110003942A (en) | A kind of solvent extraction method of carbolic oil dephenolize | |
| CN103319300A (en) | Process method for preparing industrial naphthalene through continuous distillation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: No. 21 Miner Road, Pingdingshan City, Henan Province, 467001 Applicant after: China Pingmei Shenma Holding Group Co.,Ltd. Applicant after: Shengde Guang Technology Development (Beijing) Co.,Ltd. Applicant after: CHINA University OF MINING AND TECHNOLOGY BEIJING Address before: 467001 No.21 middle miner Road, Pingdingshan City, Henan Province Applicant before: CHINA PINGMEI SHENMA ENERGY CHEMICAL GROUP Co.,Ltd. Applicant before: Shengde Guang Technology Development (Beijing) Co.,Ltd. Applicant before: CHINA University OF MINING AND TECHNOLOGY BEIJING |
|
| CB02 | Change of applicant information |