CN108358742A - A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition - Google Patents
A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition Download PDFInfo
- Publication number
- CN108358742A CN108358742A CN201810341008.2A CN201810341008A CN108358742A CN 108358742 A CN108358742 A CN 108358742A CN 201810341008 A CN201810341008 A CN 201810341008A CN 108358742 A CN108358742 A CN 108358742A
- Authority
- CN
- China
- Prior art keywords
- methyl naphthalene
- pregnant solution
- naphthalene pregnant
- tower
- aromatic hydrocarbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/06—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by azeotropic 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provide it is a kind of from mixing C+10 heavy aromatic hydrocarbon composition in detach methyl naphthalene pregnant solution method, include the following steps：The methyl naphthalene pregnant solution that will be evaporated under reduced pressure in the heavy C10 aromartic for removing durol, ten aromatic solvent of naphthalene and low-carbon, is added the ethanol amine of graphene-containing, is uniformly mixed, and forms the methyl naphthalene pregnant solution that graphene is modified；The methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system, in the case where vacuum degree is 0.009MPa, then boils, is 80 85 DEG C by tower top temperature, column bottom temperature is 150 155 DEG C, and rectification under vacuum carries out primary purification；Then it in the case where vacuum degree is 0.009MPa, then boils, is 115 120 DEG C by tower top temperature, column bottom temperature is 140 145 DEG C, and rectification under vacuum carries out secondary purification；It is finally placed in the FLC liquid membrane crystal devices of the filler of composite material containing micro nanometer fiber, 2 4h of crystallisation by cooling at 15 ~ 25 DEG C, squeezes, sweating obtains methyl naphthalene finished product.
Description
Technical field
The invention belongs to C+10 heavy aromatic hydrocarbon separation technology fields, and in particular to one kind is from mixing C+10 heavy aromatic hydrocarbon composition
The method for detaching methyl naphthalene pregnant solution.
Background technology
For methyl naphthalene by 2 kinds of isomers, i.e. alpha-methyl-naphthalene and beta-methylnaphthalene, methyl naphthalene can be used as medicine and surface-active
Agent can also prepare mesophase pitch or carbon fiber, and wherein alpha-methyl-naphthalene can be used for preparing vinyl chloride fibers and terylene printing and dyeing
Vehicle surfactant, heat carrier, medicine intermediate, sulphur extractant, plasticizer and fiber dyeing auxiliaries, beta-methylnaphthalene can be used for
Prepare Vitamin K3, dyeing polyester fibers body carrier, fiber dyeing auxiliaries, organic pigment, concrete additive, detergent, emulsification
Agent, hemostat, wetting agent, plant growth regulator, beverage additive, feed addictive, oral contraceptive and coloured glue dye gigging
Material etc., currently, methyl naphthalene is mainly isolated from coking coal oil and PETROLEUM PROCESSING, especially petroleum catalytic cracking, catalytic reforming
All there are a certain number of methyl naphthalenes in the heavy aromatics prepared with techniques such as thermal crackings, is 230-245 DEG C by cutting boiling range
Contain alpha-methyl-naphthalene, beta-methylnaphthalene, naphthalene, quinoline alkali, indoles and biphenyl etc. in the naphthalene pregnant solution that fraction obtains, it is therefore necessary to
Processing is further purified to naphthalene pregnant solution.
Chinese patent CN 103288584B disclose the process that high-purity beta-methylnaphthalene is extracted in reformed arene C10, with
Catalytic reforming by-product aromatic hydrocarbons C10 is raw material, uses ripple silk net high efficiency packing rectifying column for rectifying device, and it is 235- to take boiling range
Then 254 DEG C of methylnaphthalene is crystallized in two steps using continuous multi-stage countercurrent fractional crystallisation method, beta-methylnaphthalene content is big
Methylnaphthalene in 80% is added in crystallizer, and 28 DEG C are first cooled to the rate of 2 DEG C/min, and non-crystallized stock is discharged,
Then 36 DEG C are warming up to the rate of 2 DEG C/min, the material of thawing are first cooled to 30.5 DEG C with the rate of 1 DEG C/min, discharge
Uncrystallized material, then 36 DEG C are warming up to, it is produced the material of fusing as qualified products.Beta-methylnaphthalene prepared by this method
Purity is up to 99%, and equipment investment is smaller, and production cost is relatively low, pollution-free byproduct.1074 59440A of Chinese patent CN are public
The process for purification for the beta-methylnaphthalene opened, the process for purification include molecule rectifying, fractional crystallisation and press filtration, and flash method is removed thick first
Moisture in base naphthalene fraction, then to being 6-10MPa and 24- in vacuum degree in molecular still of the inside containing condenser system
Molecule rectifying is carried out at 255 DEG C, then when temperature is down to -15 DEG C, naphthalene and quinoline are precipitated, when temperature is down to -22 DEG C or more,
Alpha-methyl-naphthalene is precipitated, and when temperature is down to -35 DEG C, is obtained beta-methylnaphthalene crude product, is then cooled to -35 to beta-methylnaphthalene crude product
DEG C when, beta-methylnaphthalene crude product is squeezed, beta-methylnaphthalene fine work is obtained.This method uses Liquid liquid Separation in molecule stage of rectification
Method, mean free path difference realizes the separation of different material after being escaped using variety classes molecule, and separation process temperature is low, will not
Lead to the cracking of raw material components, energy-saving and emission-reduction, resource utilization is high, and product purity is high.By the above-mentioned prior art it is found that by changing
The purity of beta-methylnaphthalene can be improved in the mode of the mode and crystallization that become rectifying, but yield is not high, can only achieve 40%.
Invention content
The technical problem to be solved in the present invention is to provide one kind detaching methyl naphthalene richness from mixing C+10 heavy aromatic hydrocarbon composition
The method of liquid collecting after methyl naphthalene pregnant solution to be added to the ethanol amine of graphene-containing, after the processing of secondary pressure distilation, is placed in
The processing of FLC liquid membrane crystal device crystallisation by cooling, obtains methyl naphthalene finished product.Alpha-methyl-naphthalene and β-in methyl naphthalene finished product prepared by this method
The purity of methyl naphthalene is high, the high income of methyl naphthalene.
In order to solve the above technical problems, the technical scheme is that：
A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition, it is characterised in that：
Include the following steps：
(1) methyl that will be evaporated under reduced pressure in the heavy C10 aromartic for removing durol, ten aromatic solvent of naphthalene and low-carbon
The ethanol amine of graphene-containing is added in naphthalene pregnant solution, is uniformly mixed, and forms the methyl naphthalene pregnant solution that graphene is modified；
(2) the methyl naphthalene pregnant solution that graphene prepared by step (1) is modified is transferred in reboiler, is subtracted using intermittent
It presses in distillation system, in the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, be 80-85 DEG C by tower top temperature,
Column bottom temperature is 150-155 DEG C, absolute pressure of top of the tower 20-50KPa, reflux ratio 1:5-8, rectification under vacuum 40-60min, not
The condensed trap condensing trapping reflux of gas phase is condensed, extraction obtains the methyl naphthalene pregnant solution of primary purification；
(3) the methyl naphthalene pregnant solution of primary purification prepared by step (2) is placed in vacuum distillation tower, be in vacuum degree-
Under 0.008MPa, the methyl naphthalene pregnant solution of primary purification is boiled again, the methyl naphthalene pregnant solution of primary purification is passed through into tower top temperature
It it is 115-120 DEG C, column bottom temperature is 140-145 DEG C, absolute pressure of top of the tower 20-30KPa, reflux ratio 1:8-10, decompression essence
20-30min, the uncooled condensed trap condensing trapping reflux of gas phase are evaporated, extraction obtains the methyl naphthalene enrichment of secondary purification
Liquid；
(4) the methyl naphthalene pregnant solution of secondary purification prepared by step (3) is placed in FLC liquid membrane crystal devices, -15~-
Crystallisation by cooling 2-4h at 25 DEG C, squeezing, sweating obtain methyl naphthalene finished product.
As a preferred embodiment of the above technical solution, in the step (1), the technique of methyl naphthalene pregnant solution vacuum distillation is：Tower
It is 132-133 DEG C to push up temperature, and column bottom temperature is 198-200 DEG C, and vacuum degree is -0.009Mpa, rectification under vacuum 60-80min.
As a preferred embodiment of the above technical solution, in the step (1), the matter of methyl naphthalene pregnant solution and graphene, ethanol amine
Amount is than being 1:0.001-0.003:0.05-0.1.
As a preferred embodiment of the above technical solution, in the step (2) or (3), condensing trapping device is metal condensation trapping
Device contains one layer of silver-colored catcher foil of plating in metal condensation trap.
As a preferred embodiment of the above technical solution, in the step (4), FLC liquid membrane crystal devices include tower crystallizer and crouch
Formula crystallizer, high efficiency packing is fibrous filler polymer composites in crystallizer.
As a preferred embodiment of the above technical solution, the fibrous filler polymer composites are polypropylene fibre and glass
The blended material of fiber.
As a preferred embodiment of the above technical solution, in the fibrous filler polymer composites fiber a diameter of micro-nano
Meter level.
As a preferred embodiment of the above technical solution, the air penetrability of the fibrous filler polymer composites is 75-85%.
As a preferred embodiment of the above technical solution, in the step (4), crystallisation by cooling is that a step crystallisation by cooling or two steps are cold
But it crystallizes.
As a preferred embodiment of the above technical solution, in the step (4), the technique of two step crystallisation by cooling is：First -15~-
At 20 DEG C after crystallisation by cooling 1-2h, squeezing crystallization after, after melting at -20~-25 DEG C crystallisation by cooling 1-2h.
Compared with prior art, the invention has the advantages that：
(1) contain quinoline, isoquinolin, naphthalene, Alpha-Methyl in the methyl naphthalene pregnant solution of mixing C+10 heavy aromatic hydrocarbon composition separation
The boiling point of naphthalene, beta-methylnaphthalene, indoles etc., these components is more close, therefore separating-purifying is difficult, and vacuum distillation is for not
The substance for just having been thermally decomposed, aoxidizing or having been polymerize up to boiling point, ambient pressure reduces boiling point and also reduces when vacuum distillation, therefore can
To be distilled at lower pressures, the boiling point containing naphthalene is 216.8 DEG C in methyl naphthalene pregnant solution, and the boiling point of quinoline is
235.4 DEG C, the boiling point of isoquinolin is 246.1 DEG C, and the boiling point of indoles is 254.1 DEG C, and the boiling point of alpha-methyl-naphthalene is 243.5 DEG C, β-
The boiling point of methyl naphthalene is 242.4 DEG C, and the boiling point of biphenyl is 244.8 DEG C, and the boiling point of dimethylnaphthalene is 267 DEG C, and the boiling point of model is
It 278.4 DEG C, according to the estimation formula lgP=A+B/T of the lower boiling point of decompression, estimates at -0.009MPa, alpha-methyl-naphthalene and β-first
The boiling point of base naphthalene is about 140-145 DEG C, therefore carries out second extraction separation to alpha-methyl-naphthalene and beta-methylnaphthalene, and methyl naphthalene can be improved
The purity of product, and further carried using the reflux of the condensing trapping device condensing trapping of Ag containing layer catcher foil in being evaporated under reduced pressure twice
The recovery rate of high methyl naphthalene ensures the yield of methyl naphthalene.In addition, the present invention is using filling micro nano-scale fiber shape filled polymer
The FLC liquid membrane crystals device of tower crystallizer and the Horizontal crystallizer composition of composite material to the methyl naphthalene pregnant solution of secondary purification into
One step of row or two step Freeze crystallizations, further increase the purity of methyl naphthalene.
(2) ethanol amine of graphene-containing is added in the methyl naphthalene pregnant solution of initial extraction by the present invention, ethanol amine conduct
Entrainer improves the separation degree of naphthalene, methyl naphthalene and dimethylnaphthalene and heterocyclic compound, and the minimal amount of graphene of addition can be shown
The inoxidizability and heat resistance for improving methyl naphthalene are write, the stability of the component in distillation process is improved, prevents the production of thermal cracking
It is raw, it ensure that the yield of methyl naphthalene.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 132 DEG C DEG C in tower top temperature,
Column bottom temperature is 198 DEG C, and vacuum degree is evaporated under reduced pressure 60min under conditions of being -0.009MPa, and obtained methyl naphthalene pregnant solution is pressed
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.001:0.05, the ethanol amine of graphene-containing is added, mixes
Uniformly, the methyl naphthalene pregnant solution that graphene is modified is formed.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 80 DEG C by tower top temperature, column bottom temperature is 150 DEG C,
Absolute pressure of top of the tower is 20KPa, reflux ratio 1:5, rectification under vacuum 40min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 115 DEG C, bottom of tower temperature
Degree is 140 DEG C, absolute pressure of top of the tower 20KPa, reflux ratio 1:8, rectification under vacuum 30min, uncooled gas phase is passed through catches containing silver-plated
Collect the condensing trapping device condensing trapping reflux of piece, extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 75%, the crystallisation by cooling 2h at -15 DEG C, is squeezed, hair
Sweat obtains methyl naphthalene finished product.
Embodiment 2：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 133 DEG C DEG C in tower top temperature,
Column bottom temperature is 200 DEG C, and vacuum degree is evaporated under reduced pressure 80min under conditions of being -0.009MPa, and obtained methyl naphthalene pregnant solution is pressed
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.003:0.1, the ethanol amine of graphene-containing is added, mixes
Uniformly, the methyl naphthalene pregnant solution that graphene is modified is formed.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 85 DEG C by tower top temperature, column bottom temperature is 155 DEG C,
Absolute pressure of top of the tower is 50KPa, reflux ratio 1:8, rectification under vacuum 60min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 120 DEG C, bottom of tower temperature
Degree is 145 DEG C, absolute pressure of top of the tower 30KPa, reflux ratio 1:10, rectification under vacuum 20min, uncooled gas phase is passed through catches containing silver-plated
Collect the condensing trapping device condensing trapping reflux of piece, extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 75-85%, the crystallisation by cooling 4h at -25 DEG C, pressure
It squeezes, sweating obtains methyl naphthalene finished product.
Embodiment 3：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 132.5 DEG C in tower top temperature
DEG C, column bottom temperature is 199 DEG C, and vacuum degree is evaporated under reduced pressure 70min under conditions of being -0.009MPa, obtained methyl naphthalene pregnant solution,
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.002:0.06, the ethanol amine of graphene-containing is added, mixes
Close the methyl naphthalene pregnant solution uniform, formation graphene is modified.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 82 DEG C by tower top temperature, column bottom temperature is 153 DEG C,
Absolute pressure of top of the tower is 40KPa, reflux ratio 1:6, rectification under vacuum 50min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 118 DEG C, bottom of tower temperature
Degree is 143 DEG C, absolute pressure of top of the tower 25KPa, reflux ratio 1:8.5, rectification under vacuum 25min, uncooled gas phase are passed through containing silver-plated
The condensing trapping device condensing trapping of catcher foil flows back, and extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 75-85%, first at -15 DEG C after crystallisation by cooling 1h,
After squeezing crystallization, crystallisation by cooling 1h, squeezing, sweating obtain methyl naphthalene finished product at -20 DEG C after melting.
Embodiment 4：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 132.5 DEG C in tower top temperature,
Column bottom temperature is 199.1 DEG C, and the methyl naphthalene pregnant solution that vacuum distillation 65min is obtained under conditions of vacuum degree is -0.009MPa is pressed
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.002:0.08, the ethanol amine of graphene-containing is added, mixes
Uniformly, the methyl naphthalene pregnant solution that graphene is modified is formed.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 84 DEG C by tower top temperature, column bottom temperature is 153 DEG C,
Absolute pressure of top of the tower is 35KPa, reflux ratio 1:7, rectification under vacuum 55min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 119 DEG C, bottom of tower temperature
Degree is 144 DEG C, absolute pressure of top of the tower 27KPa, reflux ratio 1:9, rectification under vacuum 30min, uncooled gas phase is passed through catches containing silver-plated
Collect the condensing trapping device condensing trapping reflux of piece, extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 75-85%, the crystallisation by cooling 3h at -20 DEG C, pressure
It squeezes, sweating obtains methyl naphthalene finished product.
Embodiment 5：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 132.5 DEG C in tower top temperature,
Column bottom temperature is 199.1 DEG C, and the methyl naphthalene pregnant solution that vacuum distillation 75min is obtained under conditions of vacuum degree is -0.009MPa is pressed
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.001:0.1, the ethanol amine of graphene-containing is added, mixes
Uniformly, the methyl naphthalene pregnant solution that graphene is modified is formed.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 80 DEG C by tower top temperature, column bottom temperature is 155 DEG C,
Absolute pressure of top of the tower is 20KPa, reflux ratio 1:8, rectification under vacuum 50min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 115 DEG C, bottom of tower temperature
Degree is 145 DEG C, absolute pressure of top of the tower 20KPa, reflux ratio 1:10, rectification under vacuum 20min, uncooled gas phase is passed through catches containing silver-plated
Collect the condensing trapping device condensing trapping reflux of piece, extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 75%, the crystallisation by cooling 2h at -25 DEG C, is squeezed, hair
Sweat obtains methyl naphthalene finished product.
Embodiment 6：
(1) the heavy C10 aromartic that will remove durol, ten aromatic solvent of naphthalene and low-carbon is 132.5 DEG C in tower top temperature,
Column bottom temperature is 199.1 DEG C, and vacuum degree is evaporated under reduced pressure 80min under conditions of being -0.009MPa, obtained methyl naphthalene pregnant solution,
Mass ratio according to methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.003:0.05, the ethanol amine of graphene-containing is added, mixes
Close the methyl naphthalene pregnant solution uniform, formation graphene is modified.
(2) the methyl naphthalene pregnant solution that graphene is modified is transferred in reboiler, using in intermittent reduced pressure distillation system,
In the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, is 85 DEG C by tower top temperature, column bottom temperature is 155 DEG C,
Absolute pressure of top of the tower is 20KPa, reflux ratio 1:8, rectification under vacuum 40min, uncooled gas phase pass through the condensation containing silver-plated catcher foil
Trap condensing trapping flows back, and extraction obtains the methyl naphthalene pregnant solution of primary purification.
(3) the methyl naphthalene pregnant solution of primary purification is placed in vacuum distillation tower, it, will in the case where vacuum degree is -0.009MPa
The methyl naphthalene pregnant solution of primary purification boils again, by the methyl naphthalene pregnant solution of primary purification by tower top temperature be 120 DEG C, bottom of tower temperature
Degree is 140 DEG C, absolute pressure of top of the tower 30KPa, reflux ratio 1:8, rectification under vacuum 25min, uncooled gas phase is passed through catches containing silver-plated
Collect the condensing trapping device condensing trapping reflux of piece, extraction obtains the methyl naphthalene pregnant solution of secondary purification.
(4) the methyl naphthalene pregnant solution of secondary purification is placed in the FLC liquid film knots of tower crystallizer and Horizontal crystallizer composition
In brilliant device, high efficiency packing is that micro/nano level polypropylene fibre polymerize with the filling of the blend fibre shape of glass fibre wherein in crystallizer
The air penetrability of object composite material, fibrous filler polymer composites is 85%, formerly at -15 DEG C after crystallisation by cooling 2h,
After squeezing crystallization, crystallisation by cooling 2h, squeezing, sweating obtain methyl naphthalene finished product at -25 DEG C after melting.
After testing, the yield for the methyl naphthalene finished product that prepared by embodiment 1-6 and the result of purity are as follows：
As seen from the above table, the purity for the methyl naphthalene that prepared by separation of the invention and method of purification is high, high income.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of method for detaching methyl naphthalene pregnant solution in C+10 heavy aromatic hydrocarbon composition from mixing, it is characterised in that：Including following
Step：
（1）The methyl naphthalene being evaporated under reduced pressure in the heavy C10 aromartic for removing durol, ten aromatic solvent of naphthalene and low-carbon is rich
The ethanol amine of graphene-containing is added in liquid collecting, is uniformly mixed, and forms the methyl naphthalene pregnant solution that graphene is modified；
（2）By step（1）The methyl naphthalene pregnant solution that the graphene of preparation is modified is transferred in reboiler, using intermittent reduced pressure essence
It evaporates in system, in the case where vacuum degree is -0.0085MPa, methyl naphthalene pregnant solution is boiled again, be 80-85 DEG C by tower top temperature, bottom of tower
Temperature is 150-155 DEG C, absolute pressure of top of the tower 20-50KPa, reflux ratio 1:5-8, rectification under vacuum 40-60min, it is uncooled
The condensed trap condensing trapping reflux of gas phase, extraction obtain the methyl naphthalene pregnant solution of primary purification；
（3）By step（2）The methyl naphthalene pregnant solution of the primary purification of preparation is placed in vacuum distillation tower, vacuum degree be-
Under 0.008MPa, the methyl naphthalene pregnant solution of primary purification is boiled again, the methyl naphthalene pregnant solution of primary purification is passed through into tower top temperature
It it is 115-120 DEG C, column bottom temperature is 140-145 DEG C, absolute pressure of top of the tower 20-30KPa, reflux ratio 1:8-10, decompression essence
20-30min, the uncooled condensed trap condensing trapping reflux of gas phase are evaporated, extraction obtains the methyl naphthalene enrichment of secondary purification
Liquid；
（4）By step（3）The methyl naphthalene pregnant solution of the secondary purification of preparation is placed in FLC liquid membrane crystal devices, at -15 ~ -25 DEG C
Crystallisation by cooling 2-4h, squeezing, sweating obtain methyl naphthalene finished product.
2. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 1,
It is characterized in that：The step（1）In, the technique of methyl naphthalene pregnant solution vacuum distillation is：Tower top temperature is 132-133 DEG C, tower
Bottom temperature is 198-200 DEG C, and vacuum degree is -0.009Mpa, rectification under vacuum 60-80min.
3. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 1,
It is characterized in that：The step（1）In, the mass ratio of methyl naphthalene pregnant solution and graphene, ethanol amine is 1:0.001-0.003:
0.05-0.1。
4. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 1,
It is characterized in that：The step（2）Or（3）In, condensing trapping device is metal condensation trap, is contained in metal condensation trap
There is one layer of silver-colored catcher foil of plating.
5. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 1,
It is characterized in that：The step（4）In, FLC liquid membrane crystal devices include tower crystallizer and Horizontal crystallizer, in crystallizer efficiently
Filler is fibrous filler polymer composites.
6. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 5,
It is characterized in that：The fibrous filler polymer composites are the blended material of polypropylene fibre and glass fibre.
7. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 5,
It is characterized in that：A diameter of micro/nano level of fiber in the fibrous filler polymer composites.
8. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 5,
It is characterized in that：The air penetrability of the fibrous filler polymer composites is 75-85%.
9. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 1,
It is characterized in that：The step（4）In, crystallisation by cooling is a step crystallisation by cooling or two step crystallisation by cooling.
10. the method that methyl naphthalene pregnant solution is detached in a kind of C+10 heavy aromatic hydrocarbon composition from mixing according to claim 9,
It is characterized in that：The step（4）In, the technique of two step crystallisation by cooling is：First at -15 ~ -20 DEG C after crystallisation by cooling 1-2h,
Squeezing crystallization after, after melting at -20 ~ -25 DEG C crystallisation by cooling 1-2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810341008.2A CN108358742A (en) | 2018-04-17 | 2018-04-17 | A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810341008.2A CN108358742A (en) | 2018-04-17 | 2018-04-17 | A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108358742A true CN108358742A (en) | 2018-08-03 |
Family
ID=63008398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810341008.2A Pending CN108358742A (en) | 2018-04-17 | 2018-04-17 | A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108358742A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115073257A (en) * | 2022-08-03 | 2022-09-20 | 连云港鹏辰特种新材料有限公司 | Method for separating and purifying 1-methylnaphthalene from methylnaphthalene enrichment mother liquor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202191722U (en) * | 2011-08-29 | 2012-04-18 | 中北大学 | Melting crystallizer |
| CN105272815A (en) * | 2014-06-10 | 2016-01-27 | 中国石化扬子石油化工有限公司 | Method for extracting methylnaphthalene in C10 aromatics |
-
2018
- 2018-04-17 CN CN201810341008.2A patent/CN108358742A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202191722U (en) * | 2011-08-29 | 2012-04-18 | 中北大学 | Melting crystallizer |
| CN105272815A (en) * | 2014-06-10 | 2016-01-27 | 中国石化扬子石油化工有限公司 | Method for extracting methylnaphthalene in C10 aromatics |
Non-Patent Citations (5)
| Title |
|---|
| 张振华: "洗油的分离与应用研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 徐克勋等: "《有机化工原料及中间体便览》", 31 December 1989, 辽宁省石油化工技术情报总站 * |
| 滕占才等: "高纯度β-甲基萘的制备工艺研究", 《黑龙江八一农垦大学学报》 * |
| 胡春等: "《有机化学实验》", 31 March 2007, 中国医药科技出版社 * |
| 陈英男等: "《常用化工单元设备的设计》", 30 June 2017, 华南理工大学出版社有限公司 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115073257A (en) * | 2022-08-03 | 2022-09-20 | 连云港鹏辰特种新材料有限公司 | Method for separating and purifying 1-methylnaphthalene from methylnaphthalene enrichment mother liquor |
| CN115073257B (en) * | 2022-08-03 | 2023-10-27 | 连云港鹏辰特种新材料有限公司 | Method for separating and purifying 1-methylnaphthalene from methylnaphthalene enrichment mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105418368B (en) | A kind of technique and device for producing high straight alcohol | |
| DE2552140C2 (en) | Process for the separation of C 2 + -hydrocarbons from gas mixtures containing hydrogen, methane, ethylene and ethane | |
| CN107253938B (en) | Cis-butenedioic anhydride direct hydrogenation prepares the production technology of high purity butylene dicarboxylic anhydride | |
| TWI314065B (en) | ||
| CN104557382B (en) | The method of separating-purifying firpene from turps | |
| CN107474866A (en) | A kind of preparation method of high-quality mesophase pitch | |
| CN108358742A (en) | A method of detaching methyl naphthalene pregnant solution from mixing C+10 heavy aromatic hydrocarbon composition | |
| CN102126958B (en) | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization | |
| CN101229988B (en) | Method for refining high-purity anthracene and carbazole from crude anthracene | |
| CN101412653A (en) | Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene | |
| CN113121346A (en) | Purification method of electronic grade dimethyl carbonate | |
| CN114031478B (en) | Method for extracting, rectifying and separating benzene and cyclohexene by adopting eutectic solvent | |
| CN106431836A (en) | Technology for separating ethyl alcohol-water system by means of extractive distillation and flash coupling | |
| CN108586184A (en) | A kind of separation and process for purification based on overcritical and ultrasonic wave beta-methylnaphthalene | |
| CN111606918B (en) | Method for preparing high-purity 1, 8-cineole from crude cinnamomum camphora oil | |
| CN104761566B (en) | A kind of method of low concentration eucalyptus oil crystallization and purification | |
| CN201292325Y (en) | Apparatus for producing durol by reforming C10 aromatic hydrocarbon production | |
| CN107266278A (en) | Highly dissoluble aromatic solvent GF S1800 high-purity production method | |
| CN107216903A (en) | A kind of method that cross-linking modified sedimentation separation of FCC clarified oils prepares mesophase pitch | |
| CN202337741U (en) | Device for producing durene with C10 heavy aromatic | |
| CN115872828B (en) | Method for separating and purifying mesitylene from reformed C9 aromatic hydrocarbon by using eutectic solvent | |
| CN114213208B (en) | Method for extracting, rectifying and purifying mesitylene by high-efficiency composite solvent | |
| CN109289930A (en) | A method of efficiently separating and purify 1- methyl naphthalene | |
| CN109970790A (en) | The extraction separating method and rectifier unit of dichloromethylphosphine | |
| CN110002945A (en) | The method for extraction and purification of indenes product and purifying plant system based on this method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180803 |
|
| WD01 | Invention patent application deemed withdrawn after publication |