CN109651092A - A kind of gas circulation coking crude phenol clean preparation method and its device - Google Patents
A kind of gas circulation coking crude phenol clean preparation method and its device Download PDFInfo
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- CN109651092A CN109651092A CN201910067528.3A CN201910067528A CN109651092A CN 109651092 A CN109651092 A CN 109651092A CN 201910067528 A CN201910067528 A CN 201910067528A CN 109651092 A CN109651092 A CN 109651092A
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000004939 coking Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 127
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 85
- 230000020477 pH reduction Effects 0.000 claims abstract description 80
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 70
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 68
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 66
- 150000002989 phenols Chemical class 0.000 claims abstract description 63
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000011280 coal tar Substances 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 11
- 230000003068 static effect Effects 0.000 claims abstract description 10
- 239000011734 sodium Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000005201 scrubbing Methods 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims description 15
- 239000011269 tar Substances 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000013589 supplement Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 230000029058 respiratory gaseous exchange Effects 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 3
- 239000011344 liquid material Substances 0.000 claims description 3
- 102000005393 Sodium-Potassium-Exchanging ATPase Human genes 0.000 claims description 2
- 108010006431 Sodium-Potassium-Exchanging ATPase Proteins 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims 2
- GWEIYKFDYAMAQP-UHFFFAOYSA-M sodium;phenol;phenoxide Chemical compound [Na+].OC1=CC=CC=C1.[O-]C1=CC=CC=C1 GWEIYKFDYAMAQP-UHFFFAOYSA-M 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 63
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 25
- 238000000034 method Methods 0.000 description 25
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 21
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 10
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000003546 flue gas Substances 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 239000007832 Na2SO4 Substances 0.000 description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 108010052164 Sodium Channels Proteins 0.000 description 2
- 102000018674 Sodium Channels Human genes 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- WJEIYVAPNMUNIU-UHFFFAOYSA-N [Na].OC(O)=O Chemical compound [Na].OC(O)=O WJEIYVAPNMUNIU-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000003434 inspiratory effect Effects 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/005—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from products, waste products or side-products of processes, not directed to the production of phenols, by conversion or working-up
- C07C37/007—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from products, waste products or side-products of processes, not directed to the production of phenols, by conversion or working-up from the tar industry
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/64—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring
- C07C37/66—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring by conversion of hydroxy groups to O-metal groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/86—Purification; separation; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/02—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring monocyclic with no unsaturation outside the aromatic ring
- C07C39/04—Phenol
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/235—Metal derivatives of a hydroxy group bound to a six-membered aromatic ring
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of gas circulation coking crude phenol clean preparation method and its device, it is therefore an objective to which energy conservation and environmental protection simultaneously reduces equipment corrosion；Coal tar is obtained carbolic oil fraction through distillation by the present invention, is carried out dephenolization by scrubbing with NaOH aqueous solution and is generated sodium phenolate solution；It is sent to decomposition tower top to flow from above to below, inversely be contacted with recyclegas, most of sodium phenolate is by CO2It decomposes to flow into after generating crude phenols and sodium carbonate and decomposes tower bottom；Crude phenols and Na are completed in static separation 6-8 hours2 CO3The separation of solution, the crude phenols after separation flow automatically to a crude phenols medial launder, are sent to acidification tower top and flow from above to below, inversely contact with recyclegas, sodium phenolate is by CO2Acidification tower bottom is flowed into after further decomposing；The CO of reaction is not participated in2Gas is by decomposition tower, acidification top of tower evolution, and into carbon dioxide balance tank, then the bottom cycle for being respectively delivered to decomposition tower by circulating fan and being acidified tower uses, it is established that the gas-circulating system of carbon dioxide decomposition.
Description
Technical field
The invention belongs to high temperature coal-tars, middle coalite tar deep process technology field, and in particular to a kind of gas circulation
Coking crude phenol clean preparation method and its device.
Background technique
Industrially from high temperature coal-tar, middle coalite tar extract phenolic substances method be, first to coal tar into
Row distillation, to obtain the relatively high carbolic oil fraction of phenol content.Its fraction is washed phenolic material with NaOH aqueous solution again
Matter is separated, and principle is that NaOH reacts generation sodium phenolate solution with phenolic substances (process is also washing process).Then lead to
It crosses and crude phenols is made with acidic materials decomposition sodium phenolate (process is also decomposable process).China's sodium phenolate decomposes production crude phenols at present
Mainly using flue gas, (active principle is CO2) decompose and two methods of sulfuric acid decomposition, the scientific and technological Limited Liability of Shandong Dezhou gold energy
House journal CN102206140A, which is announced, uses sulfur dioxide (SO2) gas decomposed, also there is document report using pure CO2Point
There are certain drawbacks in solution, the above several method.It is the CO utilized in flue gas that flue gas, which is decomposed,2Generation is reacted with sodium phenolate
Crude phenols and sodium carbonate (Na2CO3), due to containing a small amount of SO in flue gas2Gas (50mg/Nm3--200mg/Nm3) and a certain amount of
Water, have sulfurous acid generation in decomposable process, not only equipment caused to corrode, Na after disassembly2CO3In aqueous solution also
Na can be contained2SO3Equal impurity, are unfavorable for Na2CO3Recycling.In addition flue gas CO2Content it is very low, according to flue gas come
Its CO of source difference2Content generally 10%--20% and reaction efficiency it is very low, decompose gas there are about 80%--90% and be discharged by system
In the middle of atmosphere, environment is caused to seriously affect.With sulfur dioxide (SO2) gas decompose when, since the presence of water has Asia
Sulfuric acid generates, severe corrosion equipment, while unreacted sulfur dioxide (SO2) be discharged into atmosphere and have an impact to environment.Have a
Other enterprise uses pure CO2It decomposes, due to CO2Concentration height will cause Local C O2It is excessive to generate sodium bicarbonate (NaHCO3), bicarbonate
Sodium (NaHCO3) be easy Crystallization Plugging equipment the problem of.Sulfuric acid decomposition method has a large amount of sodium sulphate (Na2SO4) waste liquid generation, it is this
Sodium sulphate (Na2SO4) waste liquid contains many harmful substances, wastewater processing technology cannot be handled very well at present.
The above-mentioned main chemical equation of washing process and decomposable process is as follows:
C6H5OH + NaOH → C6H5ONa + H2O
SO2 + H2O→H2SO3
2C6H5ONa + CO2 + H2O → 2C6H5OH + Na2CO3
2C6H5ONa + SO2 + H2O → 2C6H5OH +Na2SO3
2C6H5ONa + H2SO4→ 2C6H5OH + Na2SO4
A small amount of sodium bicarbonate (NaHCO is also generated when carbon dioxide decomposition3), NaHCO3It is unstable be heated to 90 DEG C with
On, it is allowed to be completely converted into sodium carbonate.
Sulfuric acid process has continuous decomposition when decomposing sodium phenolate and interval decomposes two kinds of techniques, no matter is required using that technique
Sulfuric acid is mixed to sodium phenolate and is controlled 90 DEG C or so of decomposition temperature, between 20%--40%, sulfuric acid is added containing phenol in sodium phenolate
When decomposition, the sulfuric acid for not being in time for reaction can exist in the form of dilute sulfuric acid in equipment part, corrode under these conditions to equipment
It is very serious.The sewage disposal technology that sulfuric acid process decomposes current China of sodium sulfate waste liquid that sodium phenolate generates is difficult to handle, biology
When method handles sewage, if sodium sulphate content is exceeded to will cause activated sludge mortality, cause system normal when serious
Operation.When batch technology sulfuric acid decomposition sodium phenolate, since decomposable process is exothermic reaction, can also it be generated in sulfuric acid decomposition operation
Largely " acid mist ", seriously affects operating environment.The above problem is decomposed although disclosing with the presence of technical literature and recording persulfuric acid
Solution, " acid mist " generated when such as being washed and decomposed with sodium phenolate；To Na2SO4Waste liquid carries out crystallization treatment etc.；Fail to from
Fundamentally solve the problems, such as that environment is polluted in equipment corrosion and " three wastes ".Sulfur dioxide decomposes, and having data introduction and patent, (application is public
Cloth CN102206140A) disclose SO2The method for decomposing sodium phenolate co-production sodium sulfite.Although this method solves useless
The problem of liquid discharges still deposits equipment corrosion, unreacted SO2The problem of influencing operating environment, at present only few enterprise
Industry is using.Using pure CO2When decomposition, due to CO2Concentration is high, can make resolving device (decomposition tower and acidification tower) interior Local C O2It crosses
Amount, CO2Excessively have sodium bicarbonate (NaHCO3) generate, sodium bicarbonate (NaHCO3) solubility in water is low, there is crystallization to give birth to
At occluding device, the cycle of operation is influenced.It is the important link that phenol products are extracted in coal tar that sodium phenolate, which decomposes, from
The problem of currently used several method in China apparently corrodes in the prevalence of equipment, there is with short production cycle and exhaust gas to ring
The problem of border influences.Therefore, it is necessary to a kind of production technology of novel coal tar refining separation and Extraction crude phenols be developed, to solve
The equipment etching problem of sodium phenolate decomposable process and influence to environment.
Summary of the invention
Object of the present invention is to overcome the shortcomings of above-mentioned prior art, a kind of easy to operate, energy conservation and environmental protection is provided, can reduce and set
Standby burn into extends the gas circulation coking crude phenol during the high temperature coal-tar of the cycle of operation, middle coalite tar processing and refining
Clean preparation method and its device.
The method of the present invention establishes gas-circulating system, and 95% CO is greater than with concentration2Adjust recyclegas concentration, circulating air
Body is inversely contacted in decomposition tower with sodium phenolate and is once decomposed；Some undecomposed phenol in decomposition product
Sodium salt is sent to the interior further decomposition solution that inversely contacts with recyclegas of acidification tower and obtains crude phenols finished product and Na2CO3Solution, then
By Na2CO3Solution recycles.
Gas of the present invention circulation coking crude phenol clean preparation method the following steps are included:
(1) high temperature coal-tar or middle coalite tar are obtained into the carbolic oil fraction of phenol content 6%-20% through distillation, in vertical washing
Dephenolization by scrubbing is carried out to it with NaOH aqueous solution in tower, NaOH aqueous solution is contacted with carbolic oil fraction reverse flow, and two kinds of substances are mutual
It is immiscible, and have difference in specific gravity, phenolic substances is reacted with NaOH generates sodium phenolate solution；
C6H5OH + NaOH → C6H5ONa + H2O
(2) be 60 DEG C -80 DEG C by temperature, the sodium phenolate solution of concentration 20%-40% is transported to the decomposition tower top of two layers of filler,
It is flowed from above to below by packing layer, is CO with the effective component risen in tower2Recyclegas inversely contact, CO2Concentration control
In 15%-20%, most of sodium phenolate is by the CO in recyclegas2It decomposes and generates crude phenols and sodium carbonate (Na2CO3) flow into decompose afterwards
Tower bottom；
Sodium phenolate decomposition can be obtained into phenol products (crude phenols).Sodium phenolate is a kind of strong base-weak acid salt, any acidity ratio
The strong acid of phenol can decompose sodium phenolate, to obtain phenol products.
(3) under the conditions of 60 DEG C -80 DEG C, according to crude phenols and sodium carbonate (Na2CO3) solution the static separation 6-8 of difference in specific gravity it is small
When, complete crude phenols and Na2 CO3The separation of solution, the Na after separation2CO3Solution flows automatically to storage tank, and crude phenols flow automatically to a crude phenols
Medial launder；
The above reaction principle is:
2C6H5ONa + CO2 + H2O → 2C6H5OH + Na2CO3
Sodium phenolate is after once decomposing, most of sodium phenolate and CO2Reaction generates crude phenols and aqueous sodium carbonate.
(4) it is decomposed by primary, through also containing some unreacted sodium phenolate in static isolated crude phenols, with acid
Change tower raw material pump and be transported to the acidification tower top of two layers of filler under the conditions of pressure is not less than 0.4MPa, by packing layer from upper
And lower flowing, with recyclegas (the effective component CO from tower bottom2) inversely contact, sodium phenolate therein is by recyclegas
CO2Acidification tower bottom is flowed into after further decomposing；In order to keep acidification reaction more thorough, band spray-hole is equipped in acidification tower bottom
Acidification bubbler, with concentration be greater than 95% CO2Acidification bottom liquid material is further bubbled and is acidified and controls acidification tower bottom
CO in gas2Concentration 20%-25%.Material after sour bubblingization is under the conditions of 90 DEG C -95 DEG C, according to crude phenols and sodium carbonate
(Na2CO3) difference in specific gravity static separation 8--10 hours, complete crude phenols and Na2 CO3The separation of solution, the Na after separation2 CO3Solution
Storage tank is flowed automatically to, crude phenols reach quality requirement factory；
After second decomposes, 99% sodium phenolate is decomposed sodium phenolate, undecomposed sodium phenolate stay in sodium carbonate liquor into
One step recycles or processing, and crude phenols reach quality requirement factory sale.
(5) CO of reaction is not participated in2Gas is by decomposition tower, acidification top of tower evolution, into carbon dioxide balance tank, then by
Circulating fan is respectively delivered to decomposition tower and is acidified the bottom cycle use of tower, so that the gas for setting up carbon dioxide decomposition follows
Loop system.
Carbon dioxide decomposition system realizes gas closed-circulation, and sodium phenolate decomposable process is in decomposition tower and acidification tower
It carries out, sodium phenolate solution enters in tower from tower top, and (gas is air and CO to the gas risen with tower lower part2Mixture, CO2It is dense
Degree is about 15%-25%) inversely contact, sodium phenolate and part CO2Decomposable process is completed in reaction.
To keep system CO2Balance, can circulating fan export and be acidified tower bottom acidification bubbler supplement concentration
CO greater than 95%2Gas.
Gas of the present invention recycles coking crude phenol cleaning production apparatus, including decomposition tower, acidification tower, a crude phenols medial launder,
It is acidified tower raw material pump, sodium carbonate liquor medial launder, sodium carbonate liquor pump, carbon dioxide balance tank, acidification bubbler and circulated air
Machine；Decomposition tower, acidification tower are all made of filler for flower ring tower；Decomposition tower is mounted on ground, top gas pipeline and acidification top of tower
Gas pipeline connection, bottom gas pipeline are connect with acidification tower bottom gas pipeline, the crude phenols pipeline of bottom one time and a crude phenols
The connection of medial launder top feed pipe, the sodium carbonate liquor pipeline and sodium carbonate liquor medial launder top feed pipe of bottom connect
It connects；Acidification tower is mounted on ground, and bottom crude phenols pipeline is connect with finished product crude phenols pipeline, and bottom carbonic acid sodium channel and sodium carbonate are molten
The connection of liquid medial launder top feed pipe；Crude phenols medial launder is mounted on ground, upper part feed pipe and decomposition tower lower part
Crude phenols pipeline connection, lower part outlet pipeline are connect with acidification tower raw material pump intake pipeline；Acidification tower raw material pump is mounted on ground
Face, inlet duct are connect with a crude phenols medial launder lower part outlet pipeline, and outlet conduit and acidification tower top feed pipe connect
It connects；Sodium carbonate liquor medial launder is mounted on ground, the distribution of upper part feed pipe and decomposition tower, acidification tower lower part sodium carbonate liquor
Pipeline connection, lower part outlet pipeline are connect with sodium carbonate liquor pump intake pipeline；Sodium carbonate liquor pump is mounted on ground, entrance
Pipeline is connect with sodium carbonate liquor medial launder lower part outlet pipeline, and outlet conduit is sent pipeline outside with sodium carbonate liquor and connect；Dioxy
Change Carbon balance tank to be mounted in a high platform, gas feed converges pipeline and connect with decomposition tower and acidification overhead gas, gas
Body outlet is connect with circulating fan gas access；Acidification bubbler is mounted on acidification tower bottom and supplies with 95% fresh carbon dioxide
It is connected to pipeline；Circulating fan is mounted on ground, and gas access is connect with carbon dioxide balance tank, gas vent and decomposition tower and
Converge pipeline connection in acidification tower bottom gas access.
Individual calling is provided on carbon dioxide balance tank top to cut down and single-suction valve；The diameter and inspiratory capacity of single inlet valve are according to phenol
The fresh carbon dioxide concentration of sodium salt treating capacity and supplement determines that design suction pressure power is -500Pa, when system pressure is low
It waits sucking air and -500Pa is not less than with balance system pressure.The diameter and expiration amount that individual calling is cut down are also according to sodium phenolate treating capacity
And the fresh carbon dioxide concentration of supplement determines, single breathing valve design exhalation pressure is+500Pa.The decomposition tower, acidification tower are
One section of tower of two layers of stainless steel Pall ring filler.
For the pressure of the balanced gas circulatory system, individual calling is provided on carbon dioxide balance tank top and is cut down and single-suction valve,
When system bears positive pressure, single breathing valve opens exhaled gas and releases positive pressure；When system bears negative pressure, it is empty that single-suction valve opens sucking
Gas is released negative pressure.It thereby guarantees that system pressure in a certain range, guarantee to be safely operated and reduces gas emissions.Single-suction valve
Diameter and inspiratory capacity determine according to the fresh carbon dioxide concentration of sodium phenolate treating capacity and supplement, design suction pressure is-
500Pa sucks air when system pressure is low and is not less than -500Pa with balance system pressure；The diameter and expiration that individual calling is cut down
Amount be also according to the fresh carbon dioxide concentration of sodium phenolate treating capacity and supplement determine, single breathing valve design exhalation pressure be+
500Pa, when system pressure is high be discharged gas to tar distillation system heating furnace burn (coking crude phenol production process be from
Phenolic substances is extracted in coal tar, extraction process needs a tar distillation heating furnace), and balance system pressure is not higher than
500Pa。
The decomposition tower, acidification tower are one section of tower of two layers of filler.The decomposition tower, acidification tower tower body material are 304,
Filler is stainless steel (304) Pall ring filler.Gas is established by decomposition tower, acidification tower, carbon dioxide balance tank and circulating fan
Systemic circulatory system, the unreacting gas that decomposition tower, acidification tower top escape enters carbon dioxide balance tank, then is conveyed by circulating fan
It is recycled to decomposition tower and acidification tower bottom.It is big in the acidification bubbler supplement concentration that circulating fan exported and be acidified tower bottom
In 95% CO2Gas keeps system CO2Balance.
It is greater than 95% CO using concentration2Gas is as supplement CO2Gas source, and control into decomposition tower and acidification tower circulating air
Body CO2Concentration is 15%--20%, is acidified tower bottom CO2Concentration is 20%--25%.It is arranged on carbon dioxide gas compensator top single
Suction is cut down, and is sucked air when system pressure is low with balance system pressure and is not less than -500Pa.It is balanced in carbon dioxide gas
Tank top setting individual calling is cut down, and gas to tar distillation system heating furnace is discharged when system pressure is high and burns, is to balance
Pressure of uniting is not higher than+500Pa.
The present invention suitable for high temperature coal-tar, gas circulation coking crude phenol during coalite tar processing and refining it is clear
Clean production establishes the decomposition gas circulatory system compared with prior art, and 95% CO is greater than with concentration2As gas-circulating system
Supplement CO2Extra a small amount of gas is discharged into tar distillation system heating furnace and burned, solves existing sodium phenolate operation splitting by gas source
Existing equipment corrodes (sulfuric acid decomposition and SO2Decompose), the cycle of operation short (pure CO2Decompose), tail gas pollution environment (flue gas point
Solution) the problems such as, extra a small amount of gas is discharged into tar distillation system heating furnace and is burned, discharges, realizes without exhaust gas
Long-term operation and clean manufacturing.With automatization level, high, easy to operate, energy conservation and environmental protection, with low investment, good in economic efficiency etc. are excellent
Point.
Detailed description of the invention
Fig. 1 is flow sheet of the present invention；
In figure: K01 is decomposition tower, and K02 is acidification tower, and P01 is acidification tower raw material pump, and P02 is sodium carbonate liquor pump, and B01 is to follow
Ring blower, T01 are a crude phenols medial launder, and T02 is sodium carbonate liquor medial launder, and T03 is carbon dioxide balance tank, and M01 is acid
Change bubbler.
1 is sodium phenolate entrance, and 2 be to be acidified the fresh carbon dioxide of bubbler to fill into mouth, 3 exported for circulating fan it is fresh
Carbon dioxide fills into mouth, and 4 send mouth outside for sodium carbonate liquor, and 5 export for product crude phenols.
Specific embodiment
The method specifically includes following steps:
(1) high temperature coal-tar obtains the carbolic oil fraction of phenol content about 6%-8% by distillation, is washed with NaOH aqueous solution to it
It washs, NaOH is reacted with phenolic substances generates sodium phenolate solution.Be 60 DEG C -80 DEG C by temperature, the sodium phenolate solution of concentration 25% with
1000--1500 kilograms/when flow be transported to top decomposition tower (K01) of two layers of stainless steel Pall ring filler, by filler
Layer flows from above to below, recyclegas (the effective component CO with rising2) inversely contact, into the CO of acidification tower (K02)2Concentration
Control 18% or so；Most sodium phenolates are by the CO in recyclegas2It decomposes and generates crude phenols and sodium carbonate (Na2CO3) flow into afterwards
The bottom decomposition tower (K01).
(2) pass through the material once decomposed under the conditions of 60 DEG C -80 DEG C, according to crude phenols and sodium carbonate (Na2CO3) difference in specific gravity
In the bottom decomposition tower (K01), static separation about 6 hours, completes crude phenols and Na2 CO3The separation of solution, the Na after separation2 CO3It is molten
Liquid flows automatically to storage tank, and crude phenols flow automatically to a crude phenols medial launder (T01)；
(3) it decomposes by primary through also containing some unreacted sodium phenolate in static isolated crude phenols, with acidification tower
(K02) raw material pump is transported to top acidification tower (K02) of two layers of stainless steel Pall ring filler, warp under the conditions of pressure 0.4MPa
It crosses packing layer to flow from above to below, with recyclegas (the effective component CO from tower bottom2) inversely contact, sodium phenolate quilt therein
CO in recyclegas2Acidification bottom tower (K02) is flowed into after further decomposing；
(4) in order to keep acidification reaction more thorough, it is equipped with the acidification bubbler (M01) with spray-hole in the acidification tower bottom (K02),
It is greater than 95% CO with concentration2Bubbling acidification is carried out to the acidification bottom tower (K02) liquid material
(5) material after acidified bubblingization is under the conditions of 90-95 DEG C, according to crude phenols and sodium carbonate (Na2CO3) difference in specific gravity is static
Crude phenols and Na are completed in separation about 10 hours2 CO3The separation of solution, the Na after separation2 CO3Solution flows automatically to storage tank, and crude phenols reach
It dispatches from the factory to quality requirement.Decomposition tower (K01), the acidification tower bottom (K02) are provided with indirect heater, and control column bottom temperature is requiring model
In enclosing.
Decomposition tower (K01), acidification tower (K02) are all made of filler for flower ring tower；Decomposition tower (K01) is mounted on ground, top
Gas pipeline is connect with acidification top of tower gas pipeline, and bottom gas pipeline is connect with acidification tower bottom gas pipeline, bottom one
Secondary crude phenols pipeline is connect with crude phenols medial launder (T01) top feed pipe, the sodium carbonate liquor pipeline and sodium carbonate of bottom
The connection of solution medial launder (T02) top feed pipe；Acidification tower (K02) is mounted on ground, and bottom crude phenols pipeline and finished product are thick
The connection of phenol pipeline, bottom carbonic acid sodium channel are connect with the top sodium carbonate liquor medial launder (T02) feed pipe；Among crude phenols
Slot (T01) is mounted on ground, and upper part feed pipe is connect with the crude phenols pipeline of decomposition tower lower part one time, lower part outlet pipeline and acid
Change the connection of tower (K02) raw material pump intake pipeline；Acidification tower (K02) raw material pump is mounted on ground, inlet duct and a crude phenols
The connection of medial launder (T01) lower part outlet pipeline, outlet conduit are connect with the acidification top tower (K02) feed pipe；Sodium carbonate liquor
Medial launder (T02) is mounted on ground, and the distribution of upper part feed pipe and decomposition tower (K01), the acidification lower part tower (K02) sodium carbonate are molten
The connection of liquid pipe road, lower part outlet pipeline are connect with sodium carbonate liquor pump (P02) inlet duct；Sodium carbonate liquor pumps (P02) installation
On ground, inlet duct is connect with sodium carbonate liquor medial launder (T02) lower part outlet pipeline, outlet conduit and sodium carbonate liquor
Send pipeline connection outside；Carbon dioxide balance tank (T03) is mounted in a high platform, gas feed and decomposition tower (K01) and
Acidification tower (K02) top gas body converges pipeline connection, and gas vent is connect with the gas access circulating fan (B01)；It is acidified bubbler
(M01) it is mounted on the acidification tower bottom (K02) and is connect with 95% fresh carbon dioxide service；Circulating fan (B01) is mounted on
Ground, gas access are connect with carbon dioxide balance tank (T03), gas vent and decomposition tower (K01) and acidification bottom tower (K02)
Converge pipeline connection in gas access.
Unreacted gas escapes into carbon dioxide balance tank (T03) by decomposition tower (K01), acidification tower (KO2) top,
It is used again by the bottom cycle that circulating fan (B01) is respectively delivered to decomposition tower (K01) and is acidified tower (K02).In circulating fan
(B01) acidification bubbler (M01) the supplement concentration for exporting and being acidified the bottom tower (KO2) is greater than 95% carbon dioxide (CO2) gas
Body keeps system carbon dioxide (CO2) balance.
On the carbon dioxide balance tank top (T03), setting single suction is cut down, and single-suction valve specification is: DN80, HXF-DX type work as system
Air is sucked when pressure is low, and -500Pa is not less than with balance system pressure；It is arranged on the carbon dioxide balance tank top (T03)
Individual calling is cut down, and single-suction valve specification is: gas is discharged to tar in DN80, HXF7 band adapter tube (back-fire relief) type when system pressure is high
Distallation systm heating furnace is burned, and is not higher than+500Pa with balance system pressure；Between being equipped in carbon dioxide balance tank (T03)
Heater is connect, control loop gas temperature is at 60 DEG C -- between 80 DEG C.
Claims (10)
1. a kind of gas recycles coking crude phenol clean preparation method, it is characterized in that:
High temperature coal-tar or middle coalite tar are obtained into the carbolic oil fraction of phenol content 6%-20% through distillation, in vertical scrubbing tower
Dephenolization by scrubbing is carried out to it with NaOH aqueous solution, NaOH aqueous solution reacts generation with NaOH with carbolic oil fraction reverse flow contact phenol
Sodium phenolate solution；
By temperature be 60 DEG C -80 DEG C, the sodium phenolate solution of concentration 20%-40% is transported to the decomposition tower top of two layers of filler, is passed through
It crosses packing layer to flow from above to below, is CO with the effective component risen in tower2Recyclegas inversely contact, CO2Concentration control exists
15%-20%, most of sodium phenolate is by the CO in recyclegas2It decomposes and generates crude phenols and sodium carbonate (Na2CO3) decomposition tower is flowed into afterwards
Bottom；
Under the conditions of 60 DEG C -80 DEG C, according to crude phenols and sodium carbonate (Na2CO3) difference in specific gravity static separation 6-8 hours of solution, it completes
Crude phenols and Na2 CO3The separation of solution, the Na after separation2CO3Solution flows automatically to storage tank, and crude phenols flow automatically to a crude phenols medial launder；
(4) a static isolated crude phenols are transported under the conditions of pressure is not less than 0.4MPa by acidification tower raw material pump
There is the acidification tower top of two layers of filler, flowed from above to below by packing layer, is CO with the effective component from tower bottom2Circulation
Gas inversely contacts, and sodium phenolate therein is by the CO in recyclegas2Acidification tower bottom is flowed into after further decomposing；
(5) CO of reaction is not participated in2Gas is by decomposition tower, acidification top of tower evolution, into carbon dioxide balance tank, then by recycling
Blower is respectively delivered to decomposition tower and is acidified the bottom cycle use of tower, to set up the gas cyclic system of carbon dioxide decomposition
System.
2. gas as described in claim 1 recycles coking crude phenol clean preparation method, it is characterized in that being equipped with band in acidification tower bottom
The acidification bubbler of spray-hole is greater than 95% CO with concentration2Gas is further bubbled acidification bottom liquid material and is acidified and controls
CO in relieving haperacidity Tower bottom gas2Concentration is in 20%-25%；Material after sour bubblingizations under the conditions of temperature is 90 DEG C -95 DEG C, according to
According to crude phenols and sodium carbonate (Na2CO3) difference in specific gravity static separation 8-10 hours, complete crude phenols and Na2CO3The separation of solution, after separation
Na2CO3Solution flows automatically to storage tank, and crude phenols reach quality requirement factory.
3. gas as claimed in claim 1 or 2 recycles coking crude phenol clean preparation method, it is characterized in that being holding system CO2It is flat
Weighing apparatus is greater than 95% CO in the acidification bubbler supplement concentration that circulating fan exported and be acidified tower bottom2Gas.
4. gas as claimed in claim 1 or 2 recycles coking crude phenol clean preparation method, it is characterized in that being balanced gas cyclic system
The pressure of system, on carbon dioxide balance canister body top, setting individual calling is cut down and single-suction valve, and when system bears positive pressure, single breathing valve is beaten
Exhaled gas is opened to release positive pressure；When system bears negative pressure, single-suction valve opens sucking AB Air Bleed negative pressure；Thereby guarantee that system pressure
Power is safely operated in a certain range and reduces gas emissions.
5. gas as claimed in claim 4 recycles coking crude phenol clean preparation method, it is characterized in that the diameter and air-breathing of single-suction valve
Amount determines that design suction pressure is -500Pa according to the fresh carbon dioxide concentration of sodium phenolate treating capacity and supplement, works as system
Air is sucked when pressure is low, and -500Pa is not less than with balance system pressure.
6. gas as claimed in claim 4 recycles coking crude phenol clean preparation method, it is characterized in that diameter that individual calling is cut down and expiration
Amount determines that single breathing valve design exhalation pressure is+500Pa according to the fresh carbon dioxide concentration of sodium phenolate treating capacity and supplement, when
Gas to tar distillation system heating furnace is discharged when system pressure is high to burn, and balance system pressure is not higher than+500Pa.
7. gas as described in claim 1 recycles coking crude phenol cleaning production apparatus, it is characterized in that include decomposition tower, acidification tower,
Crude phenols medial launder, acidification tower raw material pump, sodium carbonate liquor medial launder, sodium carbonate liquor pump, carbon dioxide balance tank, acidification
Bubbler and circulating fan；Decomposition tower, acidification tower are all made of filler for flower ring tower；Decomposition tower is mounted on ground, top gas pipe
Road is connect with acidification top of tower gas pipeline, and bottom gas pipeline is connect with acidification tower bottom gas pipeline, the crude phenols of bottom one time
Pipeline is connect with a crude phenols medial launder top feed pipe, on the sodium carbonate liquor pipeline and sodium carbonate liquor medial launder of bottom
The connection of portion's feed pipe；Acidification tower is mounted on ground, and bottom crude phenols pipeline is connect with finished product crude phenols pipeline, bottom sodium carbonate pipe
Road is connect with sodium carbonate liquor medial launder top feed pipe；Crude phenols medial launder is mounted on ground, upper part feed pipe
It is connect with the crude phenols pipeline of decomposition tower lower part one time, lower part outlet pipeline is connect with acidification tower raw material pump intake pipeline；It is former to be acidified tower
Material pump is mounted on ground, and inlet duct is connect with a crude phenols medial launder lower part outlet pipeline, on outlet conduit and acidification tower
The connection of portion's feed pipe；Sodium carbonate liquor medial launder is mounted on ground, under the distribution of upper part feed pipe and decomposition tower, acidification tower
The connection of portion's sodium carbonate liquor pipeline, lower part outlet pipeline are connect with sodium carbonate liquor pump intake pipeline；Sodium carbonate liquor pump installation
On ground, inlet duct is connect with sodium carbonate liquor medial launder lower part outlet pipeline, and outlet conduit is sent outside with sodium carbonate liquor
Pipeline connection；Carbon dioxide balance tank is mounted in a high platform, and gas feed and decomposition tower and acidification overhead gas converge
Pipeline connection is closed, gas vent is connect with circulating fan gas access；Acidification bubbler be mounted on acidification tower bottom and with it is 95% new
Fresh carbon dioxide service connection；Circulating fan is mounted on ground, and gas access is connect with carbon dioxide balance tank, and gas goes out
Mouth converges pipeline and connect with decomposition tower and acidification tower bottom gas access.
8. gas as claimed in claim 7 recycles coking crude phenol cleaning production apparatus, it is characterized in that decomposition tower, acidification tower bottom setting
Indirect heater, to control column bottom temperature in claimed range.
9. gas recycles coking crude phenol cleaning production apparatus as described in claim 7 or 8, it is characterized in that single-suction valve specification is
DN80, HXF-DX type, single-suction valve specification are DN80, HXF7 band adapter tube (back-fire relief) type.
10. gas recycles coking crude phenol cleaning production apparatus as described in claim 7 or 8, it is characterized in that the decomposition tower, acidification
Tower is one section of tower of two layers of filler.
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| CN201910067528.3A CN109651092B (en) | 2019-01-24 | 2019-01-24 | Clean production method and device for gas circulation coking crude phenol |
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| CN110330408A (en) * | 2019-07-23 | 2019-10-15 | 山西永东化工股份有限公司 | A kind of gas Cycle-decomposition coking crude phenol coproduction light calcium production method |
| CN110590509A (en) * | 2019-09-25 | 2019-12-20 | 山西永东化工股份有限公司 | Production method for carbon dioxide cyclic decomposition coking crude phenol coproduction desulfurizer |
| CN112521253A (en) * | 2020-12-18 | 2021-03-19 | 中冶焦耐(大连)工程技术有限公司 | Carbon dioxide decomposition system and process for sodium phenolate |
| CN112850978A (en) * | 2021-01-19 | 2021-05-28 | 青岛科技大学 | Extraction and electrolysis integration-based treatment method for wastewater in coal tar production |
| CN112939746A (en) * | 2021-02-04 | 2021-06-11 | 中冶焦耐(大连)工程技术有限公司 | Pre-pump mixing tower type continuous washing dephenolizing process |
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| CN209508091U (en) * | 2019-01-24 | 2019-10-18 | 山西永东化工股份有限公司 | A kind of gas circulation coking crude phenol cleaning production apparatus |
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| CN102381943A (en) * | 2011-08-30 | 2012-03-21 | 河南宝舜化工科技有限公司 | System and technology for producing coked crude phenol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330408A (en) * | 2019-07-23 | 2019-10-15 | 山西永东化工股份有限公司 | A kind of gas Cycle-decomposition coking crude phenol coproduction light calcium production method |
| CN110590509A (en) * | 2019-09-25 | 2019-12-20 | 山西永东化工股份有限公司 | Production method for carbon dioxide cyclic decomposition coking crude phenol coproduction desulfurizer |
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| CN112521253B (en) * | 2020-12-18 | 2023-11-28 | 中冶焦耐(大连)工程技术有限公司 | Carbon dioxide decomposition system and process of sodium phenolate |
| CN112850978A (en) * | 2021-01-19 | 2021-05-28 | 青岛科技大学 | Extraction and electrolysis integration-based treatment method for wastewater in coal tar production |
| CN112939746A (en) * | 2021-02-04 | 2021-06-11 | 中冶焦耐(大连)工程技术有限公司 | Pre-pump mixing tower type continuous washing dephenolizing process |
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| CN109651092B (en) | 2024-01-05 |
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