CN116554922A - Process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbon - Google Patents
Process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbon Download PDFInfo
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- CN116554922A CN116554922A CN202310576056.0A CN202310576056A CN116554922A CN 116554922 A CN116554922 A CN 116554922A CN 202310576056 A CN202310576056 A CN 202310576056A CN 116554922 A CN116554922 A CN 116554922A
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- 239000002904 solvent Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000008569 process Effects 0.000 title claims abstract description 24
- 150000004945 aromatic hydrocarbons Chemical class 0.000 title claims abstract description 23
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000000926 separation method Methods 0.000 claims abstract description 34
- 238000001816 cooling Methods 0.000 claims abstract description 32
- 238000010992 reflux Methods 0.000 claims abstract description 25
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000012452 mother liquor Substances 0.000 claims abstract description 7
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000001624 naphthyl group Chemical group 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- 238000001640 fractional crystallisation Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 238000002425 crystallisation Methods 0.000 claims description 22
- 230000008025 crystallization Effects 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 10
- 238000005192 partition Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 230000000903 blocking effect Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 description 17
- 239000011229 interlayer Substances 0.000 description 11
- 239000000498 cooling water Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000007599 discharging Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- -1 naphthalene aromatic hydrocarbon Chemical class 0.000 description 5
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 239000000110 cooling liquid Substances 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002966 varnish Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1096—Aromatics or polyaromatics
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/30—Aromatics
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbon, which comprises the following steps of: s1, separating raw material carbon-decimal aromatic hydrocarbon by a multistage rectification system through a rectification method, fractionating Cheng Qiechu durene and S150 solvent, distilling components (S260 solvent oil) with the distillation range of 190-260 ℃, and simultaneously cutting products with the distillation range of 260-290 ℃; s2, sequentially carrying out multi-cavity fractional crystallization on the product obtained in the step S1 by a cooling crystallizer and solid-liquid separation by a filter type centrifuge, wherein mother liquor obtained after separation is high-boiling-point low-naphthalene aromatic hydrocarbon solvent oil, and solid phase is naphthalene and is used as a raw material of phthalic anhydride. The multistage rectification system comprises a first-stage rectification tower, a second-stage rectification tower, a third-stage rectification tower and a fourth-stage rectification tower which are sequentially connected in series, wherein the top of each stage of rectification tower is provided with a heat exchanger and a reflux tank, the bottom of each stage of rectification tower is provided with a reboiler, the side surface of each stage of rectification tower is provided with a feed inlet, and the side surface of the middle part of each fourth-stage rectification tower is connected with a discharge outlet.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbons.
Background
Since 2018, low naphthalene and ultra-low naphthalene high boiling aromatic hydrocarbon solvents are widely used in various industries such as paint with low naphthalene content, silver paste, medicine and the like, and also can be used in baking varnish solvents, insecticidal emulsions and rubber resin solvents. The low naphthalene and ultra-low naphthalene aromatic hydrocarbon solvents are the best solvents with strong dissolving power and environmental protection at present, and the paint prepared by the low naphthalene aromatic hydrocarbon solvents has bright, smooth, flat and firm paint film. In the production of ink, some formulas can be changed into water solubility, so that the toxicity of the ink is reduced, the operation environment can be improved, and the printing quality can be improved.
The low naphthalene and ultra-low naphthalene aromatic hydrocarbon solvent is prepared by taking reformed carbon deca-aromatic hydrocarbon as a raw material, efficiently rectifying, and then freezing and centrifuging to separate naphthalene components. In the prior art, the production process of the low-naphthalene high-boiling aromatic hydrocarbon solvent is too complex, the aromatic hydrocarbon solvent with low naphthalene content can be obtained after a series of complex processes, the production cost is high, and the low-naphthalene aromatic hydrocarbon solvent oil sources in the market are few.
The existing comprehensive processing production device for reforming carbon-ten-thousand-ton/year aromatic hydrocarbon in our company mainly comprises durene and byproduct aromatic hydrocarbon solvent oil S260 and S150, the produced solvent oil is naphthalene-containing, only low-end products can be used as common solvents, and the added value of the products is low. In view of the current device conditions and product quality of the company, it is necessary to perform naphthalene removal and separation on the existing S260 solvent by improving the device process, and the quality of the S260 solvent oil is improved to obtain the low-naphthalene high-boiling-point solvent oil S200 so as to adapt to the requirements of the market on high-end products, and the method has important significance for further improving the diversity of the products of the company and increasing the added value of the products.
Accordingly, the inventor has the problem of providing a process for extracting low naphthalene solvent oil by using hydrocarbon of ten carbon atoms, which is expected to achieve the purpose of having more practical value, by keeping the experience of the design development and actual production in the related industry for many years and researching and improving the existing structure and the defects.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a process for extracting low naphthalene solvent oil by using hydrocarbon with ten carbon atoms, which adopts a multistage rectification method to fractionate Cheng Qiechu durene and S150 solvent, the distilled range 190-260 ℃ forms a product (S260 solvent oil), meanwhile, the distilled range 260-290 ℃ forms a product, the distilled range product (the distilled range 190-260 ℃ forms a product) is subjected to freezing crystallization and then is subjected to solid-liquid separation by a centrifuge, the separated mother liquor is high-boiling point low naphthalene aromatic hydrocarbon solvent S200, and the solid phase is naphthalene and is used as a raw material of phthalic anhydride.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbon comprises the following steps:
s1, separating raw material carbon-decimal aromatic hydrocarbon by a multistage rectification system through a rectification method, fractionating Cheng Qiechu durene and an S150 solvent, forming a product (S260 solvent oil) with a distillation range of 190-260 ℃, and simultaneously cutting the product with the distillation range of 260-290 ℃;
s2, sequentially carrying out multi-cavity fractional crystallization and solid-liquid separation on the product (S260 solvent oil) obtained in the step S1 by a cooling crystallizer and a filtering type centrifugal machine, wherein mother liquor obtained after separation is high-boiling-point low-naphthalene aromatic hydrocarbon solvent oil, and solid phase is naphthalene and is used as raw material of phthalic anhydride.
Preferably, the multistage rectification system comprises a first-stage rectification tower, a second-stage rectification tower, a third-stage rectification tower and a fourth-stage rectification tower which are sequentially connected in series, wherein the top of each stage rectification tower is provided with a heat exchanger and a reflux tank, the bottom of each stage rectification tower is provided with a reboiler, the side surface of each stage rectification tower is provided with a feed inlet, the side surface of the middle part of each fourth-stage rectification tower is connected with a discharge outlet, the discharge outlet is communicated with a cooling crystallizer, and the discharge outlet of the cooling crystallizer is communicated with a filtering type centrifuge.
Preferably, the number of the tower plates in each stage of rectifying tower in the multistage rectifying system is 45-60, and the evaporation rate is controlled to be 6-8g/min;
the crystallization temperature of the materials in the cooling crystallizer is-5 to-26 ℃.
Preferably, the top temperature of the primary rectifying tower is 110-125 ℃, the top pressure of the primary rectifying tower is 28-38Kpa, the bottom temperature of the primary rectifying tower is 168-180 ℃, the bottom pressure of the primary rectifying tower is 32-48Kpa, and the reflux ratio is controlled to be 12:1-18:1;
the temperature of the top of the secondary rectifying tower is 115-135 ℃, the pressure of the top of the secondary rectifying tower is 22-28Kpa, the temperature of the bottom of the secondary rectifying tower is 185-195 ℃, the pressure of the bottom of the secondary rectifying tower is 28-38Kpa, and the reflux ratio is controlled to be 7:1-9:1;
the top temperature of the three-stage rectifying tower is 105-118 ℃, the top pressure of the three-stage rectifying tower is 10-18Kpa, the bottom temperature of the three-stage rectifying tower is 155-175 ℃, the bottom pressure of the three-stage rectifying tower is 15-28Kpa, and the reflux ratio is controlled to be 4:1-6:1;
the temperature of the top of the four-stage rectifying tower is 95-128 ℃, the pressure of the top of the tower is 5-12Kpa, the temperature of the bottom of the tower is 175-195 ℃, the pressure of the bottom of the tower is 8-18Kpa, and the reflux ratio is controlled to be 3:1-5:1.
Preferably, a plurality of component path separation plates are uniformly distributed in the cooling crystallizer from top to bottom in sequence, the component path separation plates uniformly divide the interior of the cooling crystallizer into a plurality of crystallization cavities, inclined plates are arranged in the crystallization cavities at the bottommost part, the inclined plates and the crystallization cavities form a discharging cavity, and the crystallization materials enter the discharging cavity through a discharging port and are finally discharged outwards through a discharging port.
Preferably, the side wall of the separation partition plate is communicated with a partition plate water inlet pipe, and the other side wall is communicated with a partition plate water outlet pipe.
Preferably, a plurality of groups of blocking baffles are distributed in the separation baffle in a staggered manner, and the blocking baffles form a serpentine water flow channel. The inner wall of the separation partition plate is penetrated with a feed opening.
Preferably, the outside of each crystallization cavity is sleeved with a jacket, the side wall of the lower end of the jacket is communicated with a jacket water inlet pipe, and the side wall of the upper end of the jacket is communicated with a jacket water outlet pipe.
The jacket water outlet pipe is connected with the partition plate water inlet pipe through a pipeline, and the partition plate water outlet pipe is connected with the jacket water inlet pipe through a pipeline.
The top of the cooling crystallizer is provided with a driving motor, the output end of the driving motor is vertically connected with a main shaft, and a main pipe channel is arranged in the main shaft; the outer wall of the main shaft and positioned in each crystallization cavity are respectively provided with a stirring wheel;
the inner bottom of the cooling crystallizer is provided with a supporting pipe, and a cooling water inlet is arranged in the supporting pipe; the top of the supporting tube is communicated with a connecting tube, and the cooling water inlet is respectively communicated with the bottom jacket and the connecting tube;
the main shaft is vertically inserted into the connecting pipe, and a bearing is sleeved at the joint of the main shaft and the connecting pipe.
An interlayer cavity is arranged between the main pipe channel and the main shaft, a shunt pipe is embedded in the inner wall of the stirring wheel, the upper port of the shunt pipe positioned on the inner wall of the uppermost stirring wheel is communicated with the top of the main pipe channel, the lower port of the shunt pipe is communicated with the interlayer cavity, cooling liquid is convenient to enter from the main pipe channel and flows back to the interlayer cavity along the shunt pipe, flows to the shunt pipe below through the interlayer cavity, and finally is discharged outwards through a cooling water outlet at the bottommost part.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts a multi-stage rectification and multi-cavity fractional crystallization method to fractionate Cheng Qiechu durene and S150 solvent, the distilled range is 190-260 ℃ to form a product (S260 solvent oil), meanwhile, the distilled range is cut into a product of 260-290 ℃, the product of the distilled range is subjected to freezing crystallization and then subjected to solid-liquid separation by a centrifuge, the separated mother liquor is the high boiling point low naphthalene aromatic hydrocarbon solvent S200, and the solid phase is naphthalene and is used as the raw material of phthalic anhydride.
2. The S200 low naphthalene solvent oil prepared by the method has the characteristics of strong dissolving power, low toxicity, small smell, high boiling point, slow volatilization, no water and olefin, no chlorine and heavy metal, stable chemical and physical properties, good leveling property and the like, and the solvent performance is excellent, particularly, the high dissolving power can be exerted in the later stage of evaporation, so that the smoothness of a coating film is good, no orange peel exists, the gloss is good, the use safety of the aromatic hydrocarbon solvent is improved, and the solvent oil can be used as a high-grade baking varnish solvent, a pesticide emulsifiable solvent, a polyurethane waterproof grouting material solvent, a plasticizer and the like.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a process system according to the present invention;
FIG. 2 is a schematic diagram of a cooling crystallizer according to the present invention;
FIG. 3 is a schematic cross-sectional view of a split spacer of the present invention;
in the figure: the primary rectifying tower 1, the reboiler 101, the heat exchanger 102, the reflux drum 103, the secondary rectifying tower 2, the tertiary rectifying tower 3, the quaternary rectifying tower 4, the cooling crystallizer 5, the main shaft 51, the stirring wheel 52, the main pipe channel 53, the shunt pipe 54, the separation baffle 55, the separation baffle 551, the feed opening 552, the jacket 56, the support pipe 57, the connecting pipe 58, the jacket water inlet pipe 59, the jacket water outlet pipe 510, the baffle water inlet pipe 511, the baffle water outlet pipe 512, the interlayer cavity 513, the cooling water outlet 514, the cooling water inlet 515, the sloping plate 516 and the filter centrifuge 6.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The raw material of the hydrocarbon is byproduct of a petroleum catalytic reforming aromatic hydrocarbon device (dimethylbenzene), and the main components of the hydrocarbon comprise durene, metatetratoluene, tetratoluene, naphthalene, methylnaphthalene and the like.
Based on weight: 3 to 15 percent of durene, 5 to 25 percent of metatetrene, 3 to 20 percent of tetratoluene, 1 to 5 percent of naphthalene, 2 to 10 percent of methylnaphthalene and the balance of impurities.
The definitions of the S260 solvent oil, the S150 solvent oil and the low naphthalene S200 solvent oil are respectively in the enterprise standards: the Jiangsu Hualun chemical industry Co., ltd. Standard, Q/321088GYF001-2016, is defined in detail.
Example 1
Referring to fig. 1-3, a process for extracting low naphthalene solvent oil using carbon-decimal aromatics includes the steps of:
s1, separating raw material carbon-decimal aromatic hydrocarbon by a multistage rectification system through a rectification method, fractionating Cheng Qiechu durene and an S150 solvent, forming a product (S260 solvent oil) with a distillation range of 190-260 ℃, and simultaneously cutting the product with the distillation range of 260-290 ℃;
s2, sequentially carrying out multi-cavity fractional crystallization on the product obtained in the step S1 by a cooling crystallizer and solid-liquid separation by a filter type centrifuge, wherein mother liquor obtained after separation is high-boiling-point low-naphthalene aromatic hydrocarbon solvent oil, and solid phase is naphthalene and is used as a raw material of phthalic anhydride.
The multistage rectification system comprises a first-stage rectification tower 1, a second-stage rectification tower 2, a third-stage rectification tower 3 and a fourth-stage rectification tower 4 which are sequentially connected in series, wherein the top of each stage rectification tower is provided with a heat exchanger 102 and a reflux tank 103, the bottom of each stage rectification tower is provided with a reboiler 101, the side surface of each stage rectification tower is provided with a feed inlet, the side surface of the middle part of the fourth-stage rectification tower 4 is connected with a discharge port and is communicated with a cooling crystallizer 5, the feed port of the cooling crystallizer 5 is communicated with a filtering centrifuge 6, and the crystallization temperature of materials in the cooling crystallizer 5 is-5 to-26 ℃.
The number of tower plates in each stage of rectifying tower in the multistage rectifying system is 45, and the evaporation rate is controlled to be 6g/min;
the top temperature of the first-stage rectifying tower is 110 ℃, the top pressure of the first-stage rectifying tower is 28Kpa, the bottom temperature of the first-stage rectifying tower is 168 ℃, the bottom pressure of the first-stage rectifying tower is 32Kpa, and the reflux ratio is controlled to be 12:1;
the temperature at the top of the secondary rectifying tower is 115 ℃, the pressure at the top of the secondary rectifying tower is 22Kpa, the temperature at the bottom of the secondary rectifying tower is 185 ℃, the pressure at the bottom of the secondary rectifying tower is 28Kpa, and the reflux ratio is controlled to be 7:1;
the top temperature of the three-stage rectifying tower is 105 ℃, the top pressure of the three-stage rectifying tower is 10Kpa, the bottom temperature of the three-stage rectifying tower is 155 ℃, the bottom pressure of the three-stage rectifying tower is 15Kpa, and the reflux ratio is controlled to be 4:1;
the temperature at the top of the four-stage rectifying tower is 95 ℃, the pressure at the top of the tower is 5Kpa, the temperature at the bottom of the tower is 175 ℃, the pressure at the bottom of the tower is 8Kpa, and the reflux ratio is controlled to be 3:1.
A plurality of component path separation plates 55 are uniformly distributed in the cooling crystallizer 5 from top to bottom in sequence, the component path separation plates 55 uniformly divide the interior of the cooling crystallizer 5 into a plurality of crystallization cavities, the side walls of the component path separation plates 55 are communicated with a separation plate water inlet pipe 511, and the other side walls are communicated with a separation plate water outlet pipe 512.
A plurality of baffle plates 551 are distributed in the separation baffle plate 55 in a staggered way, a snakelike water flow channel is formed by the baffle plates 551, a blanking port 552 penetrates through the inner wall of the separation baffle plate 55, an inclined plate 516 is arranged in a crystallization cavity at the bottommost part, the inclined plate 516 and the crystallization cavity form a discharging cavity, and crystallization materials enter the discharging cavity through the blanking port 552 and are finally discharged outwards through a discharge port, and the discharge port is formed in the side wall of the cooling crystallizer 5.
The outside of each crystallization cavity is sleeved with a jacket 56, the side wall of the lower end of the jacket 56 is communicated with a jacket water inlet pipe 59, and the side wall of the upper end of the jacket 56 is communicated with a jacket water outlet pipe 510.
The jacket water outlet pipe 510 is connected with the baffle water inlet pipe 511 through a pipeline, the baffle water outlet pipe 512 is connected with the jacket water inlet pipe 59 through a pipeline, cooling liquid enters through the jacket water inlet pipe 59 of the bottommost jacket 56, enters the baffle water inlet pipe 511 through a pipeline, cools and crystallizes materials in a serpentine water flow channel formed by the baffle plate 551, and finally is discharged outwards from the uppermost jacket water outlet pipe 510, which is a first cooling circulation channel;
the bottom of the stirring wheel 52 is connected with a scraping plate through a supporting rod, the scraping plate is attached to the upper end face of the separation partition plate 55, so that solid crystalline materials can be scraped off conveniently, and the crystalline mixed materials fall into a crystallization cavity of the next level through a blanking hole 552 to be crystallized continuously, so that a multi-cavity continuous crystallization effect is achieved.
The top of the cooling crystallizer 5 is provided with a driving motor, the output end of the driving motor is vertically connected with a main shaft 51, and a main pipe channel 53 is arranged in the main shaft 51; the outer wall of the main shaft 51 and positioned in each crystallization cavity are respectively provided with a stirring wheel 52;
a supporting pipe 57 is arranged at the inner bottom of the cooling crystallizer 5, and a cooling water inlet 515 is arranged in the supporting pipe 57; the top of stay tube 57 is linked together and is had connecting pipe 58, and cooling water import 515 is linked together with jacket 56 and connecting pipe 58 of bottommost respectively, and the setting of stay tube 57 does not influence the unloading of material.
The main shaft 51 is vertically inserted into the connecting pipe 58, and a bearing is sleeved at the joint of the main shaft 51 and the connecting pipe 58; an interlayer cavity 513 is arranged between the main pipe channel 53 and the main shaft 51, a shunt pipe 54 is embedded in the inner wall of the stirring wheel 52, the upper port of the shunt pipe 54 positioned on the inner wall of the stirring wheel 52 at the uppermost end is communicated with the top of the main pipe channel 53, the lower port of the shunt pipe 54 is communicated with the interlayer cavity 513, cooling liquid conveniently enters from the main pipe channel 53 and flows back to the interlayer cavity 513 along the shunt pipe 54, flows to the shunt pipe 54 below through the interlayer cavity 513, and finally is discharged outwards through a cooling water outlet 514 at the bottommost end, and the cooling liquid is a second cooling circulation channel.
Wherein the other parts of the interlayer cavity 513 except for the part communicated with the shunt tube 54 are all solid structures, and the formed second cooling channel is the part of the interlayer cavity 513 communicated with the shunt tube 54.
Under the double circulation cooling effect of the first cooling circulation channel and the second cooling circulation channel, the material can be subjected to multi-cavity continuous crystallization, and finally solid-liquid separation is carried out through the filter type centrifugal machine 6, and the separated mother liquor is the high-boiling-point low-naphthalene aromatic hydrocarbon solvent S200.
Example 2
Referring to fig. 1 to 3, this embodiment differs from embodiment 1 in that:
the number of tower plates in each stage of rectifying tower in the multistage rectifying system is 55, and the evaporation rate is controlled to be 7g/min;
the top temperature of the first-stage rectifying tower is 115 ℃, the top pressure of the first-stage rectifying tower is 32Kpa, the bottom temperature of the first-stage rectifying tower is 175 ℃, the bottom pressure of the first-stage rectifying tower is 40Kpa, and the reflux ratio is controlled to be 15:1;
the temperature at the top of the secondary rectifying tower is 120 ℃, the pressure at the top of the secondary rectifying tower is 25Kpa, the temperature at the bottom of the secondary rectifying tower is 188 ℃, the pressure at the bottom of the secondary rectifying tower is 32Kpa, and the reflux ratio is controlled to be 8:1;
the top temperature of the three-stage rectifying tower is 110 ℃, the top pressure of the three-stage rectifying tower is 12Kpa, the bottom temperature of the three-stage rectifying tower is 160 ℃, the bottom pressure of the three-stage rectifying tower is 20Kpa, and the reflux ratio is controlled to be 5:1;
the temperature at the top of the four-stage rectifying tower is 110 ℃, the pressure at the top of the four-stage rectifying tower is 8Kpa, the temperature at the bottom of the four-stage rectifying tower is 185 ℃, the pressure at the bottom of the four-stage rectifying tower is 12Kpa, and the reflux ratio is controlled to be 4:1.
Example 3
Referring to fig. 1 to 3, this embodiment differs from embodiment 1 in that:
the number of tower plates in each stage of rectifying tower in the multistage rectifying system is 60, and the evaporation rate is controlled to be 8g/min;
the top temperature of the first-stage rectifying tower is 125 ℃, the top pressure of the first-stage rectifying tower is 38Kpa, the bottom temperature of the first-stage rectifying tower is 180 ℃, the bottom pressure of the first-stage rectifying tower is 48Kpa, and the reflux ratio is controlled to be 18:1;
the temperature at the top of the secondary rectifying tower is 135 ℃, the pressure at the top of the secondary rectifying tower is 28Kpa, the temperature at the bottom of the secondary rectifying tower is 195 ℃, the pressure at the bottom of the secondary rectifying tower is 38Kpa, and the reflux ratio is controlled to be 9:1;
the top temperature of the three-stage rectifying tower is 118 ℃, the top pressure of the three-stage rectifying tower is 18Kpa, the bottom temperature of the three-stage rectifying tower is 175 ℃, the bottom pressure of the three-stage rectifying tower is 28Kpa, and the reflux ratio is controlled to be 6:1;
the temperature at the top of the four-stage rectifying tower is 128 ℃, the pressure at the top of the four-stage rectifying tower is 12Kpa, the temperature at the bottom of the four-stage rectifying tower is 195 ℃, the pressure at the bottom of the four-stage rectifying tower is 18Kpa, and the reflux ratio is controlled to be 5:1.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the connection may be mechanical connection, direct connection or indirect connection through an intermediate medium, and may be internal connection of two elements or interaction relationship of two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The control mode of the invention is automatically controlled by the controller, the control circuit of the controller can be realized by simple programming of a person skilled in the art, the supply of power also belongs to common knowledge in the art, and the invention is mainly used for protecting a mechanical device, so the invention does not explain the control mode and circuit connection in detail.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. A process for extracting low-naphthalene solvent oil by using carbon-decimal aromatic hydrocarbon is characterized by comprising the following steps of:
s1, separating raw material carbon-decimal aromatic hydrocarbon by a multi-stage rectification system through a rectification method, fractionating Cheng Qiechu durene and S150 solvent to form a product with a distillation range of 190-260 ℃, and simultaneously cutting the product with the distillation range of 260-290 ℃;
s2, sequentially carrying out multi-cavity fractional crystallization on the product obtained in the step S1 by a cooling crystallizer and solid-liquid separation by a filter type centrifuge, wherein mother liquor obtained after separation is high-boiling-point low-naphthalene aromatic hydrocarbon solvent oil, and solid phase is naphthalene and is used as a raw material of phthalic anhydride.
2. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon according to claim 1, wherein the process comprises the following steps: the multistage rectification system comprises a first-stage rectification tower, a second-stage rectification tower, a third-stage rectification tower and a fourth-stage rectification tower which are sequentially connected in series, wherein the top of each stage rectification tower is provided with a heat exchanger and a reflux tank, the bottom of each stage rectification tower is provided with a reboiler, the side surface of each stage rectification tower is provided with a feed inlet, the side surface of the middle part of each fourth-stage rectification tower is connected with a discharge port and is communicated with a cooling crystallizer, and the discharge port of the cooling crystallizer is communicated with a filtering centrifuge.
3. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon according to claim 1, wherein the process comprises the following steps: the number of tower plates in each stage of rectifying tower in the multistage rectifying system is 45-60, and the evaporation rate is controlled to be 6-8g/min;
the crystallization temperature of the materials in the cooling crystallizer is-5 to-26 ℃.
4. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon according to claim 1, wherein the process comprises the following steps: the top temperature of the primary rectifying tower is 110-125 ℃, the top pressure of the primary rectifying tower is 28-38Kpa, the bottom temperature of the primary rectifying tower is 168-180 ℃, the bottom pressure of the primary rectifying tower is 32-48Kpa, and the reflux ratio is controlled to be 12:1-18:1;
the temperature of the top of the secondary rectifying tower is 115-135 ℃, the pressure of the top of the secondary rectifying tower is 22-28Kpa, the temperature of the bottom of the secondary rectifying tower is 185-195 ℃, the pressure of the bottom of the secondary rectifying tower is 28-38Kpa, and the reflux ratio is controlled to be 7:1-9:1;
the top temperature of the three-stage rectifying tower is 105-118 ℃, the top pressure of the three-stage rectifying tower is 10-18Kpa, the bottom temperature of the three-stage rectifying tower is 155-175 ℃, the bottom pressure of the three-stage rectifying tower is 15-28Kpa, and the reflux ratio is controlled to be 4:1-6:1;
the temperature of the top of the four-stage rectifying tower is 95-128 ℃, the pressure of the top of the tower is 5-12Kpa, the temperature of the bottom of the tower is 175-195 ℃, the pressure of the bottom of the tower is 8-18Kpa, and the reflux ratio is controlled to be 3:1-5:1.
5. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon according to claim 1, wherein the process comprises the following steps: a plurality of component path separation plates are uniformly distributed in the cooling crystallizer from top to bottom in sequence, the inside of the cooling crystallizer is uniformly divided into a plurality of crystallization cavities by the component path separation plates, the side wall of each component path separation plate is communicated with a separation plate water inlet pipe, and the other side wall of each component path separation plate is communicated with a separation plate water outlet pipe.
6. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon of claim, wherein the process comprises the following steps of: a plurality of groups of blocking baffles are distributed in the separation baffle plate in a staggered manner, and a serpentine water flow channel is formed by the blocking baffles.
7. The process for extracting low naphthalene solvent oil from carbon-decimal aromatic hydrocarbon of claim, wherein the process comprises the following steps of: the outside of each crystallization cavity is sleeved with a jacket, the side wall of the lower end of the jacket is communicated with a jacket water inlet pipe, and the side wall of the upper end of the jacket is communicated with a jacket water outlet pipe;
the jacket water outlet pipe is connected with the partition plate water inlet pipe through a pipeline, and the partition plate water outlet pipe is connected with the jacket water inlet pipe through a pipeline.
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| CN218853506U (en) * | 2022-09-08 | 2023-04-14 | 山东多晶新材料科技有限公司 | Multi-cavity continuous crystallizer |
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| CN101318874A (en) * | 2008-06-18 | 2008-12-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
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