CN110449031A - A kind of device and method separating organic liquid impurities - Google Patents
A kind of device and method separating organic liquid impurities Download PDFInfo
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- CN110449031A CN110449031A CN201910633801.4A CN201910633801A CN110449031A CN 110449031 A CN110449031 A CN 110449031A CN 201910633801 A CN201910633801 A CN 201910633801A CN 110449031 A CN110449031 A CN 110449031A
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Abstract
The application belongs to separating-purifying class chemical technology field, more particularly to a kind of device and method for separating organic liquid impurities, it is sieved by molecule and dissolves particle class impurity, colored impurity, the impurity of macromolecule, gel-like impurity, inorganic salts etc. in diffusion removal dicyandiamide solution, and select the substance etc. of screening or enrichment suitable molecular weight by molecular weight；The core component of device includes surge tank, feed pump, membrane separation plant etc.；Feed pump is for feeding and providing proper temperature and pressure；Organic nanofiltration membrane is set in membrane separation plant, carries out separation by the difference of molecular size range based on the seperation film with different size aperture or dissolve in film based on different material to separate with the realization of the difference of diffusion rate；Described device takes up little area, energy conservation, purification efficiency is high, applicability is wide, can be independently operated, or be embedded in existing equipment, all have broad application prospects in general chemical and electron level chemical raw material field.
Description
Technical field
The application belongs to separating-purifying class chemical technology field, and in particular to it is a kind of separate organic liquid impurities device and
Method.
Background technique
Organic compound in the narrow sense is mainly made of carbon, protium, is certain containing carbon compound, but not
Oxide, sulfide, carbonic acid, carbonate, cyanide, rhodanide, cyanate, carbide, carborane, alkyl gold including carbon
Category, metal carbonyl, metal the substances such as organoligand complexes.Organic matter is biogenous material base, all life
Body all contains organic compound.Fat, amino acid, protein, sugar, ferroheme, chlorophyll, enzyme, hormone etc..Biology is intracorporal new old
The genetic phenomenon of metabolism and biology, is directed to the transformation of organic compound.In addition, it is many have with human lives it is closely related
Substance, such as petroleum, natural gas, cotton, dyestuff, chemical fibre, plastics, organic glass, natural and synthetic drug, and organic compound
Object has close ties.
The purity of organic compound and the content of impurity have very big influence for its performance and application, even determine
It qualitatively influences, such as the purity of drug, the purity of monomer etc. used in polymer preparation has high purity to want
It asks.As increasingly strict and China's economic society of environmental requirement is constantly progressive, the high-end chemistry of high-purity, low impurity content
The requirement of product also increasingly increases.In general, the removal of impurity mainly has following a few class methods: 1) biggish particle in organic matter
Shape substance can be removed by filtration；If 2) organic matter is liquid, distillation, rectifying, fractionation, molecular distillation etc. can be passed through
Method separating-purifying；3) product is that solid can be purified by recrystallization method；4) product has color, can be inhaled by active carbon
The modes such as attached purify；5) if it is macromolecular and monomer, perhaps oligomer can be purified by the precipitation method or dialysis；6) water
Dividing can be removed by the methods of azeotropic or desiccant；7) other methods.These method integrated uses can be several with preliminary purification
Most of organic matter to certain purity, such as analyze it is pure, it is chemical pure etc..But when impurity require content it is lower, or
When conventional method can not achieve, such as microgel and trace oligomer in polymer monomer, pigment in natural products,
The extremely low and superfine solid particle of content or plurality of impurities are coexisted in system and are disposably removed in HPLC mobile phase, are passed
When system method can not achieve or cost of implementation is very high, the method for purification and device of new green energy conservation are very important.
Summary of the invention
Aiming at the shortcomings in the prior art, this application provides it is a kind of separate organic liquid impurities device and method, with
Realize some particular/special requirement high-purities, environment sensitive and conventional method cannot achieve or the very high impurity of energy consumption is gone
It removes, while device simple structure, cost are controllable, space occupied is few, have very big industrialization potential.
In order to achieve the above objectives, the solution of the application is:
A kind of device separating organic liquid impurities, head tank, surge tank, charging including passing sequentially through piping connection
Pump, membrane separation plant；
Wherein, head tank is to store organic liquid to be separated；Surge tank is to direct by organic liquid to be separated
It forms feeding liquid or organic solvent is added and organic liquid to be separated is diluted to feeding liquid；Feed pump according to UF membrane for setting
The size of standby middle organic nanofiltration membrane, the temperature and pressure of flow adjustment feeding liquid are formed into film liquid；It is provided in membrane separation plant
Organic nanofiltration membrane, will carry out separating-purifying into film liquid and form trapped fluid and penetrating fluid.
The liquid that shuts off can according to need injection surge tank mixed with organic liquid to be separated after, carry out separating again
Filter, or liquid discharging recovery pipe of being shut off directly recycle.Trapped fluid can be divided into retention circulation fluid and retention out-feed liquid as a result,.
Wherein, retention circulation fluid is recycled into surge tank and continues through in membrane separation plant after mixing with organic liquid to be separated
Organic nanofiltration membrane carries out multi-cycle separation, and retaining out-feed liquid can directly discharge.
Penetrating fluid also can according to need directly be collected or further progress purifying；To the further of penetrating fluid
Purifying can use common separation mode, such as distillation, rectifying, fractionation, molecular distillation, recrystallization, can also use this Shen
The device and method for the separation organic liquid impurities that please be provided carry out.
Further, the infiltration end of membrane separation plant and/or retention end can be connect by pipeline with surge tank, make UF membrane
Equipment, surge tank further constitute multi-cycle separation system between feed pump, make from membrane separation plant penetrating fluid and/or
Trapped fluid returns to mix in surge tank with organic liquid to be separated forms feeding liquid again, and feeding liquid is adjusted using feed pump
Formed after temperature and pressure into film liquid, enter back into membrane separation plant into film liquid, organic nanofiltration membrane effect under formed trapped fluid and
Penetrating fluid.
Further, multi-stage separation can also be arranged in the device of separation organic liquid impurities provided by the present application, it can will
The devices of multiple separation organic liquid impurities are together in series, and make the penetrating fluid of upper level as the to be separated organic molten of next stage
Liquid enters the further separating-purifying of next stage arrangement.The series of specific multi-stage separation film device designs according to actual needs.
Further, conventional separation devices also be can connect after membrane separation plant, separation further is carried out to penetrating fluid and is mentioned
It is pure.
In this application, organic nanofiltration membrane can be using organic nanofiltration of the various materials and model of tolerance organic solvent
Film；By way of example and not limitation, the PuraMem film of Ying Chuan Specialty Chemical (Shanghai) Co., Ltd. can be used, not according to purposes
Together, the film of polyimide substrate either polyacrylonitrile, the size of various films and the molecular weight of screening etc. be can choose
It is determined according to isolated component to be purified.
In this application, each section of pipeline and valve are the special steel material preparation of special steel material or inner liner polytetrafluoroethylene
It forms.
The application device can be independently operated, also be desirably integrated into the existing all kinds of Chemical Manufactures containing organic solvent and
In the equipment of purification, enrichment, separation, purification of production process chinese raw materials etc. operation are realized.
The application also provides a kind of method for separating organic liquid impurities, comprising:
S1. material liquid is removed into big particulate matter by common filter device and obtains organic solvent to be separated, with
Organic nanofiltration membrane is avoided to be destroyed；
S2. organic solution to be separated described in step S1 is directly formed into feeding liquid, or under organic solvent effect according to
It is required that being diluted to form feeding liquid；
S3. the feeding liquid that step S2 is obtained is adjusted to be formed into film liquid by feed pump progress temperature and pressure；
S4. separating-purifying is carried out by organic nanofiltration membrane into film liquid by what step S3 was obtained, obtains trapped fluid and penetrating fluid.
Further, after step S4 further include:
S5. the obtained trapped fluid of step S4 is back in step S2, further with it is to be separated organic described in step S2
Solution carries out being mixed to form feeding liquid.
As long as what step S4 was obtained shut off, liquid is still kept homogeneously, which can be according to the specific of practical rejection
It is required that determine proper ratio or all to return to step S2, and separated again.
Further, after step S4 further include:
S6. the obtained penetrating fluid of step S4 is again passed by into organic nanofiltration membrane and carries out separating-purifying.
It, can be according to requiring to change corresponding temperature and pressure parameter when separating-purifying reduces impurity content again.
Further, after step S4 further include:
S7. the obtained penetrating fluid of step S4 is again passed by into distillation or rectifying or fractionation or molecular distillation or recrystallization
Carry out separating-purifying.
In this application, organic solution to be separated can be the solid particle polluter containing superfine, super low loading
In the organic solution of the formation such as pure solvent or mixed solvent；It is also possible to containing the high molecular weight impurity such as oligomer, microgel
Polymerizable type monomer solution；It is also possible to the extractive with organic solvent solution containing natural products；It is also possible to containing useless profit
The organic solution with a large amount of impurity such as lubricating oil and other organic solutions that will not destroy film.
Further, the weight percent of organic compound is at least 80% in organic solution to be separated；Further preferably
It is 90%；It is still more preferably 95%.
Further, the temperature of step S3 into film liquid is -30 DEG C to 100 DEG C, further preferably -10 DEG C to 70 DEG C；More into
One step is preferably 10 DEG C to 50 DEG C.
Further, the pressure of step S3 into film liquid is 5bar to 70bar；Further preferably 20bar to 60bar；More into
One step is preferably 30bar to 50bar.Due to the not no pressure of being followed by of feed liquor film, so transmembrane pressure is exactly into before film liquid
The pressure in face.
Further, the size of temperature and pressure organic nanofiltration membrane according to step S4, flow described in step S3 are adjusted
It is whole.The foundation of adjustment is adjusted by the working curve of detection different solutions at various pressures.
Further, the area of organic nanofiltration membrane described in step S4 is the requirement for being able to satisfy the amount of separation, is not also wasted, specifically
It is determined according to the amount and retention/transmitance ratio of separation organic solution, and specific operating condition.
In this application, according to the property of isolated principle and target product, organic nanofiltration membrane used can be identical
, it is also possible to different.
By adopting the above scheme, the beneficial effect of the application is:
Device provided by the present application realizes the separating-purifying of organic compound using organic nanofiltration membrane, the energy master needed
If changing the electric energy of feeding liquid temperature and pressure, power consumption has great saving compared with traditional distillation etc.；And the device
Compact, occupied area is small, can be embedded into the production line of existing all kinds of Chemical Manufactures and purification, the structure new as one
Unit targetedly purifies certain special impurity.
Method provided by the present application for some temperature sensitive compounds, such as Chinese medical extract purifying, containing can
Purification of compound of polymerisable double bond etc. all shows great advantage, the indeterminable crucial skill of even traditional technique
Art problem can also be solved by this method, for example, in organic solvent superfine, super low loading the removal of solid particle etc..
In short, the application can simplify the method for many traditional separating-purifyings, separation costs can be effectively reduced, and
It is easy to use, high degree of automation, and occupy little space.Point being not easily accomplished in many traditional separate modes
From, for example, after natural product extraction except color, high molecular weight impurity and the removal of microgel etc. in polymerisable monomer, using this Shen
Very high practicability is please all embodied.The application is in the separation of general chemical product and the purification of electron level chemical products simultaneously
Etc. all show huge market potential, there is great market application prospect, for many tradition industrial products liters
Grade, which is regenerated, wide applicability.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the device of separation organic liquid impurities provided by the embodiments of the present application；
Fig. 2 is the sample before and after being separated using the method for separation organic liquid impurities provided by the present application to waste lubricating oil
The pattern of product；It is left: before UF membrane；It is right: after UF membrane.
Description of symbols:
1 head tank, 11 organic solutions to be separated, 2 surge tanks, 21 feeding liquids, 3 feed pumps, 31 are into film liquid, 4 UF membranes
Equipment, 41 trapped fluids, 411 retention circulation fluids, 412 retention out-feed liquids, 42 penetrating fluids.
Specific embodiment
Below with reference to specific embodiment, the application is further described.It is noted that following embodiment is only used for
Illustrate the application not for the use scope for limiting the application.Without departing from the concept of this application, it can also make
The application of several deformation and other aspects.This belongs to the protection scope of the application.
Such as Fig. 1, a kind of device separating organic liquid impurities, head tank 1, surge tank including passing sequentially through piping connection
2, feed pump 3, membrane separation plant 4.
Wherein, head tank 1 is to store organic liquid 11 to be separated；Surge tank 2 is to by organic liquid to be separated
11, which directly form feeding liquid 21 or addition organic solvent, is diluted to feeding liquid 21 for organic liquid 11 to be separated；Feed pump 3 is used
It is formed according to the temperature and pressure that the size of organic nanofiltration membrane, flow adjust feeding liquid 21 in membrane separation plant 4 into film liquid 31；
Organic nanofiltration membrane is provided in membrane separation plant, to separate from into film liquid 31 according to molecule infiltration and molecular weight screening principle
Impurity.
In this application, organic liquid 11 to be separated directly forms feeding liquid 21 after entering surge tank 2 in head tank 1, or
Organic solvent effect under be diluted to form feeding liquid 21, feeding liquid 21 by feed pump 3 adjust temperature and pressure after formed into
Film liquid 31 after entering membrane separation plant 4 into film liquid 31, forms trapped fluid 41 and penetrating fluid 42 under organic nanofiltration membrane effect.
In this application, it when the viscosity of organic liquid 11 to be separated is greater than 500cp, can be carried out using organic solvent dilute
It releases；Organic solvent can be using alcohols or esters or ethers or arene or alkanes etc..
The action principle of organic nanofiltration membrane is: organic liquid to be separated is received under certain temperature and pressure with organic
Filter membrane contact, organic nanofiltration membrane have different permeabilities for component present in organic liquid, can be separated to have
Each component in machine liquid passes through organic nanofiltration membrane with different rates, that is, penetrates organic nanofiltration membrane, and the driving of permeable membrane
If advocating transmembrane pressure, i.e. the pressure difference of film two sides；Under transmembrane pressure effect, the faster component of infiltration rate is received by organic
Filter membrane, becomes penetrating fluid, and the slower component of infiltration rate becomes the liquid that shuts off in retention lateral enrichment.
The liquid 41 that shuts off can according to need injection surge tank 2 mixed with organic liquid 11 to be separated after, divided again
From filtering, or liquid discharging recovery pipe of being shut off directly recycles.Trapped fluid 41 can be divided into retention circulation fluid 411 and cut as a result,
Reserve feed liquid 412.Wherein, retention circulation fluid 411 is recycled into surge tank 2 and continues after mixing with organic liquid 11 to be separated
Multi-cycle separation is carried out by the organic nanofiltration membrane in membrane separation plant 4, and retaining out-feed liquid 412 can directly discharge.
In this application, the retention end of membrane separation plant 4 can also be connect by pipeline with surge tank 2, set UF membrane
Standby 4, multi-cycle separation system is further constituted between surge tank 2, feed pump 3, makes the circulation fluid that shuts off from membrane separation plant 4
411 return to and are mixed to form feeding liquid 21 in surge tank 2 with organic liquid 11 to be separated, and feeding liquid 21 is adjusted using feed pump 3
It is formed after whole temperature and pressure into film liquid 31, enters back into membrane separation plant 4 into film liquid 31, formed and cut under organic nanofiltration membrane effect
Stay liquid 41 and penetrating fluid 42.
Further, it is possible to which membrane separation plant 4 is gone out with surge tank 2, the liquid that shuts off respectively using three-way valve and branch line
Expect recovery pipe connection, the whereabouts of trapped fluid 41 is controlled by three-way valve.
Penetrating fluid 42 also can according to need directly be collected or further progress purifying；To penetrating fluid 42 into
The purifying of one step can use common separation mode, such as distillation, rectifying, fractionation, molecular distillation, recrystallization, can also use
The device and method of separation organic liquid impurities provided by the present application carry out.
In this application, the infiltration end of membrane separation plant 4 can be connect by pipeline with surge tank 2, make membrane separation plant
4, multi-cycle separation system is further constituted between surge tank 2, feed pump 3, returns to the penetrating fluid 42 from membrane separation plant 4
Be mixed to form feeding liquid 21 in surge tank 2 with organic liquid 11 to be separated, feeding liquid 21 using feed pump 3 adjust temperature and
It is formed after pressure into film liquid 31, enters back into membrane separation plant 4 into film liquid 31, form 41 He of trapped fluid under organic nanofiltration membrane effect
Penetrating fluid 42.
Further, it is possible to which membrane separation plant 4 is gone out with surge tank 2, penetrating fluid respectively using three-way valve and branch line
Expect recovery pipe connection, the whereabouts of penetrating fluid 42 is controlled by three-way valve.
Further, multi-stage separation can also be arranged in the device of separation organic liquid impurities provided by the present application, it can will
The devices of multiple separation organic liquid impurities are together in series, and make the penetrating fluid of upper level as the to be separated organic molten of next stage
Liquid enters the further separating-purifying of next stage arrangement.The series of specific multi-stage separation film device designs according to actual needs.
Further, conventional separation devices also be can connect after membrane separation plant 4, further penetrating fluid 42 is separated
Purification.
In this application, organic nanofiltration membrane can be using organic nanofiltration of the various materials and model of tolerance organic solvent
Film；By way of example and not limitation, the PuraMem film of Ying Chuan Specialty Chemical (Shanghai) Co., Ltd. can be used, not according to purposes
Together, the film of polyimide substrate either polyacrylonitrile, the size of various films and the molecular weight of screening etc. be can choose
It is determined according to isolated component to be purified.
In this application, each section of pipeline and valve are the special steel material preparation of special steel material or inner liner polytetrafluoroethylene
It forms.
The application device can be independently operated, also be desirably integrated into the existing all kinds of Chemical Manufactures containing organic solvent and
In the equipment of purification, enrichment, separation, purification of production process chinese raw materials etc. operation are realized.
A kind of method separating organic liquid impurities provided by the present application, comprising:
S1. material liquid is removed into big particulate matter by common filter device and obtains organic solvent to be separated, with
Organic nanofiltration membrane is avoided to be destroyed；
S2. organic solution to be separated described in step S1 is directly formed into feeding liquid, or under organic solvent effect according to
It is required that being diluted to form feeding liquid；
S3. the feeding liquid that step S2 is obtained is adjusted to be formed into film liquid by feed pump progress temperature and pressure；
S4. separating-purifying is carried out by organic nanofiltration membrane into film liquid by what step S3 was obtained, obtains trapped fluid and penetrating fluid.
Further, can also include: after step S4
S5. the obtained trapped fluid of step S4 is back in step S2, further with it is to be separated organic described in step S2
Solution carries out being mixed to form feeding liquid.
Preferably, as long as the liquid that shuts off that step S4 is obtained still is kept homogeneously, which can be according to practical retention
The specific requirement of rate determines proper ratio or all to return to step S2, and separated again.
Further, can also include: after step S4
S6. the obtained penetrating fluid of step S4 is again passed by into organic nanofiltration membrane and carries out separating-purifying.
It, can be according to requiring to change corresponding temperature and pressure parameter when separating-purifying reduces impurity content again.
Further, can also include: after step S4
S7. the obtained penetrating fluid of step S4 is again passed by into distillation or rectifying or fractionation or molecular distillation or recrystallization
Carry out separating-purifying.
Further, organic solution to be separated can be containing superfine, super low loading solid particle polluter it is pure molten
In the organic solution of the formation such as agent or mixed solvent；Be also possible to containing the high molecular weight impurity such as oligomer, microgel can
Polymerization type monomer solution；It is also possible to the extractive with organic solvent solution containing natural products；It is also possible to containing waste lubricating oil
Deng the organic solution with a large amount of impurity and other organic solutions that will not destroy film.
Further, the weight percent of organic compound is at least 80% in organic solution to be separated；Further preferably
It is 90%；It is still more preferably 95%.
Further, the temperature of step S3 into film liquid is -30 DEG C to 100 DEG C, further preferably -10 DEG C to 70 DEG C；More into
One step is preferably 10 DEG C to 50 DEG C.
Further, the pressure of step S3 into film liquid is 5bar to 70bar；Further preferably 20bar to 60bar；More into
One step is preferably 30bar to 50bar.Due to the not no pressure of being followed by of feed liquor film, so transmembrane pressure is exactly into before film liquid
The pressure in face.
Further, the size of temperature and pressure organic nanofiltration membrane according to step S4, flow described in step S3 are adjusted
It is whole.The foundation of adjustment is adjusted by the working curve of detection different solutions at various pressures.
Further, the area of organic nanofiltration membrane described in step S4 is the requirement for being able to satisfy the amount of separation, is not also wasted, specifically
It is determined according to the amount and retention/transmitance ratio of separation organic solution, and specific operating condition.
In this application, according to the property of isolated principle and target product, organic nanofiltration membrane used can be identical
, it is also possible to different.Solid particle polluter or mixing if it is superfine, super low loading in purification organic solution
The organic solution of the formation such as solvent can be selected according to the molecular weight of organic solvent molecule in its organic solution, guarantee to cut
The film for selecting transmitance high in the case where staying rate；It include containing the high molecular weight impurity such as oligomer, microgel if it is purification
Polymerizable type monomer solution, or include the extractive with organic solvent solution containing natural products, it according to molecule and can cut
The difference of impurity is stayed to select；When purifying the organic solution with a large amount of impurity such as waste lubricating oil, selection can be through the overwhelming majority
The film of recyclable lubricating oil.In addition, in second level or multilevel device, the first order can choose the film for filtering out impurity, second
Grade can choose the film of recycling design.
Application Example 1: superfine in pure solvent or various organic solutions, super low loading solid particle polluter point
From
Organic solution to be separated after conventional separation method preliminary purification is introduced into surge tank and forms feeding liquid,
Then according to shapes such as pressure, temperature, the sample introduction speed of various specific performance parameter setting feed pumps of subsequent organic nanofiltration membrane
At into film liquid, separating-purifying is carried out by organic nanofiltration membrane again into film liquid, solid particle is because organic nanofiltration cannot be diffused into
In film, solvent or solution after purification form penetrating fluid and obtain product, and trapped fluid is the concentration containing solid particle isolated
Liquid further increases yield if necessary and can use after the liquid circulation fluid that shuts off is returned to surge tank by circulator and further divides
From until suitable yield.
In this application embodiment, solid particle polluter in separating isopropanol solution, per kilogram solution contains nanometer extremely
The solid particle polluter that 1-10 milligrams of micron order can not achieve these remaining solid particles through operations such as conventional filterings and centrifugation
The separation of impurity carries out UF membrane purification using technical solution provided by the present application, and organic nanofiltration membrane is using win wound PuraMem
Flux membrane module is room temperature into film liquid temperature, and pressure 20bar, filtration flux is 40LMH (rising every square meter hour), and particle is gone
Except rate is more than 99%.
Application Example 2: the separation of foreign pigment and/or the concentration of extracting solution in natural product extraction liquid
By taking honeysuckle-leaf antimicrobial component extracting solution as an example, solvent is dehydrated alcohol, after traditional extraction, is evaporated ethanol sample face
Color is in brown, and target separation product is light-colored powder.UF membrane purification, You Jina are carried out using technical solution provided by the present application
Filter membrane is directly entered membrane separation plant using wound 500 membrane module of DuraMem, ethanol extract is won, and is room temperature into film liquid temperature,
Pressure is 30bar, and filtration flux 10LMH, routinely product crystallization can be obtained in heating concentration to penetrating fluid further progress.It is this kind of
The extraction of natural products can remove ethyl alcohol using heating.
Another kind of is temperature sensitivity natural product extraction, such as obtains the extraction of the qinghaosu of the Nobel Prize, cannot use liter
The mode production concentration that the mode of temperature distillation is concentrated the extract liquors such as ethyl alcohol, ether or is distilled with heating is too low, when vacuum distillation
Between it is too long, this kind of temperature sensitivity natural products further can pass through big point of retention biology using isolation technics provided by the present application
Son extracts, to realize the concentration of natural products, purification.For extracting Astragaloside IV in Radix Astragali, through first order film point
From obtained penetrating fluid (concentration 1-2%) as new feeding liquid, natural products Astragaloside IV organic macromolecule, second level separation
Selection can penetrate the seperation film of small-molecular-weight, PuraMem Flux membrane module be created using winning, into -10 DEG C of film liquid temperature, pressure
30bar, filtration flux 8LMH.The liquid that shuts off circulation is again introduced into surge tank, until the close saturation of the liquid that shuts off, from the liquid outlet guide that shuts off
Out, product is obtained after low temperature recrystallization or vacuum distillation ethyl alcohol.
Application Example 3: macromolecule impurity, such as microgel in the polymerized monomers such as pentaerythritol tetraacrylate, point
From
The polymerized monomers such as pentaerythritol tetraacrylate are because of its high functionality, in necks such as functional coating such as UV solidifications
There is very extensive purposes in domain, adds the curing system of such monomer because high functionality causes polymerization speed fast, and the degree of cross linking is high,
Therefore prepares coating is high-efficient, hardness is big, has very more advantages.But the synthesis of this kind of monomer is usually to be urged using acid
Prepared by the dehydration of change, the generation of inevitably crosslinking and oligomer and microgel is simultaneously mixed into monomer.Its result
Be the ester system that original viscosity should be very low viscosity increase, be restricted in many application aspects, for example, UV solidify in leaching
The application such as painting or spraying.But this kind of impurity is good with monomer intermiscibility, monomer boiling point height, the easy hot polymerization of these high functionalities
It closes, a possible selection cannot be provided with the Methods For Purification of conventional vacuum distillation, membrane separating method.Specifically implemented
Journey is as follows:
It is separated using two-stage membrane separation device.The pentaerythrite tetrapropylene acid rouge of domestic certain company production is made into
The tetrahydrofuran solution of 50wt% selects the seperation film of suitable molecular weight as initial feeding liquid first, is created using winning
PuraMem Flux membrane module is room temperature, pressure 30bar, filter efficiency 20LMH into film liquid temperature.Penetrating fluid enters second
Grade separator, this time uses the seperation film of small-molecular-weight, creates PuraMemSelective membrane module using winning, which can
Pentaerythritol tetraacrylate is retained to allow tetrahydrofuran to penetrate, to realize the removal of solvent, is this time into film liquid temperature
Room temperature, pressure 30Bar, filtration flux 35LMH.In this application embodiment, the tetrahydrofuran permeated is recycled, directly
Connect back to the first order separator surge tank, isolate shut off liquid back to the second level surge tank in, carry out into
The solvent recovery of one step, until the rate of recovery reaches 98%, i.e. the concentration of pentaerythritol tetraacrylate is increased to 98%.Meanwhile
The liquid that shuts off generated in first order separation similarly returns to the surge tank of the first order, and then carries out secondary separation.Due to second
The pure tetrahydrofuran that grade membrane separation device is isolated rejoins in first order surge tank, and the concentration of pentaerythrite is further
Decline, impurity and microgel of macromolecule etc. will not be adsorbed on film surface, and after separating for the second time, the liquid that shuts off is mainly high viscous
The impurity of degree, the penetrating fluid containing pentaerythritol tetraacrylate go successively to second level membrane separation device and are separated.It is overall
For, by second level UF membrane, the recycled of 95% tetrahydrofuran may be implemented, the separation yield of subject monomers is similarly
95%.
Application Example 4: waste lubricant oil regeneration pretreatment
Lubricating oil is essential lubricant during all kinds of mechanical movements, and the regeneration of waste lubricating oil is always people
Hot issue of interest because there was only about 10%-20% in waste lubricating oil is non-renewable impurity, rest part still may be used
It is oily based on regeneration.The base oil not gone bad in waste lubricating oil is subject to recycling and reusing, protection environment is not only improved, subtracts
Of low pollution can also push the sound development of environmental protection industry.At a kind of waste lubricating oil based on membrane separation technique described herein
Reason method can handle macromolecular substances in waste lubricating oil, additive, colloid, the impurity such as asphalitine.Obtained yellow is to brown
Color product can be applied to further refine.
By by the waste lubricating oil of thermal precipitation removing mechanical admixture and moisture, shown in the left side Fig. 2, it is used as first to be separated
Organic liquid separated, create PuraMem Flux membrane module using winning, which can retain macromolecular colloid, pitch
The impurity such as matter simultaneously penetrate lube base oily substance, are 60 degrees Celsius into film liquid temperature to realize the removal of impurity, pressure
Power is 50bar, filtration flux 5LMH, and macromolecular colloid, asphalitine removal rate are greater than 95%.Obtained yellow to brown is permeated
Liquid can be used as the raw material of further purification Reclaimed Base Oil, since Fig. 2 is artwork master, without display infiltration on the right side of Fig. 2
The true color of liquid.The key technical index for separating front and back is as shown in table 1.
1 waste lubricating oil of table and penetrating fluid key index compare
| Waste lubricating oil | Penetrating fluid | |
| Carbon residue | 1.72% | 0.02% |
| Calcium | 230ppm | 19.2ppm |
| Manganese | 365ppm | 40.3ppm |
| Chromium | 129ppm | 11.8ppm |
To sum up, this application discloses the solid particle polluters for removing superfine, super low loading in organic solvent；Natural
Foreign pigment is removed in product recycling；It is removed in macromolecule impurity and preparation process in temperature sensitive polymerisable monomer
The method of microgel impurity, recrystallization are eutectoid out the separation such as impurity；And waste lubricant oil regeneration pretreatment etc..And rely on these realities
It tests, has invented whole device, the corollary equipments such as from the pre-treatment of separation component to the subsequent purification of concentrate and penetrating fluid.Entirely
Plant area is small, and energy conservation, high-efficient, applicability is wide, has wide answer in general chemical and electron level chemical raw material field
Use prospect.It uses, cannot especially heat and very low to impurity content requirement to realize in the production of particular/special requirement organic matter
Product impurity removal process of the purification production either in the very high situation of conventional method energy consumption improvement.
The above-mentioned description to embodiment is that this Shen can be understood and used for the ease of those skilled in the art
Please.Those skilled in the art obviously readily can make various modifications to these embodiments, and described herein one
As principle be applied in other embodiments, without having to go through creative labor.Therefore, the application is not limited to the above embodiments.
Those skilled in the art do not depart from improvement that the scope of the application is made and modification all should be at these according to the principle of the application
Within the protection scope of application.
Claims (10)
1. it is a kind of separate organic liquid impurities device, it is characterised in that: including pass sequentially through piping connection head tank (1),
Surge tank (2), feed pump (3), membrane separation plant (4)；
Wherein, head tank (1) is to store organic liquid to be separated (11)；Surge tank (2) is to by organic liquor to be separated
Body (11), which directly forms feeding liquid (21) or organic solvent is added, is diluted to feeding liquid (21) for organic liquid (11) to be separated；
Feed pump (3) is used for according to the size of organic nanofiltration membrane, the temperature and pressure of flow adjustment feeding liquid (21) in membrane separation plant (4)
Power is formed into film liquid (31)；Organic nanofiltration membrane is provided in membrane separation plant, separating-purifying will be carried out simultaneously into film liquid (31)
Form trapped fluid (41) and penetrating fluid (42).
2. the device of separation organic liquid impurities according to claim 1, it is characterised in that: the infiltration of membrane separation plant (4)
End and/or retention end are connect by pipeline with surge tank (2) thoroughly, make membrane separation plant (4), surge tank (2), feed pump (3) it
Between further constitute multi-cycle separation system, return to penetrating fluid (42) and/or trapped fluid (41) from membrane separation plant (4)
Formation feeding liquid (21) again is mixed in surge tank (2) with organic liquid (11) to be separated, feeding liquid (21) is using charging
It is formed after pump (3) adjustment temperature and pressure into film liquid (31), membrane separation plant (4) is entered back into film liquid (31), in organic nanofiltration
Trapped fluid (41) and penetrating fluid (42) are formed under film effect.
3. the device of separation organic liquid impurities according to claim 1, it is characterised in that: the pipeline is special steel
The special steel material of material or inner liner polytetrafluoroethylene is prepared.
4. a kind of method for separating organic liquid impurities characterized by comprising
S1. material liquid is removed into big particulate matter by common filter device and obtains organic solvent to be separated, to avoid
Organic nanofiltration membrane is destroyed；
S2. organic solution to be separated described in step S1 is directly formed into feeding liquid, or under organic solvent effect as requested
It is diluted to form feeding liquid；
S3. the feeding liquid that step S2 is obtained is adjusted to be formed into film liquid by feed pump progress temperature and pressure；
S4. separating-purifying is carried out by organic nanofiltration membrane into film liquid by what step S3 was obtained, obtains trapped fluid and penetrating fluid.
5. the method for separation organic liquid impurities according to claim 4, it is characterised in that: after step S4 further include:
The obtained penetrating fluid of step S4 and/or trapped fluid are back in step S2, further with it is to be separated described in step S2
Organic solution carries out being mixed to form feeding liquid.
6. the method for separation organic liquid impurities according to claim 4, it is characterised in that: after step S4 further include:
The obtained penetrating fluid of step S4 and/or trapped fluid are passed through into distillation or rectifying or fractionation or molecular distillation or recrystallization
Mode further purify.
7. the method for separation organic liquid impurities according to claim 4, it is characterised in that: described to be separated organic molten
Liquid is in the organic solutions of formation such as pure solvent or the mixed solvent of the solid particle polluter containing superfine, super low loading；
Or the polymerizable type monomer solution containing the high molecular weight impurity such as oligomer, microgel；Or contain the organic of natural products
Solvent extractable matter solution；Or the organic solution containing waste lubricating oil etc. with a large amount of impurity.
8. the method for separation organic liquid impurities according to claim 7, it is characterised in that: described to be separated organic molten
The weight percent of organic compound is at least 80% in liquid.
9. the method for separation organic liquid impurities according to claim 4, it is characterised in that: temperature of the step S3 into film liquid
It is -30 DEG C to 100 DEG C.
10. the method for separation organic liquid impurities according to claim 4, it is characterised in that: pressure of the step S3 into film liquid
Power is 5bar to 70bar.
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| CN111573950A (en) * | 2020-05-29 | 2020-08-25 | 盛隆资源再生（无锡）有限公司 | Method for recycling and treating wastewater containing organic solvent |
| CN113088324A (en) * | 2021-04-14 | 2021-07-09 | 山东英可利新材料技术有限公司 | Method for extracting carbon nano material from waste lubricating oil, heavy oil or asphalt |
| CN113209824A (en) * | 2021-04-29 | 2021-08-06 | 南京威尔生物科技有限公司 | Method for removing macromolecular substances in polysorbate80 |
| WO2021237841A1 (en) * | 2020-05-26 | 2021-12-02 | 桂林莱茵生物科技股份有限公司 | Use of organic membrane in hemp extraction |
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Application publication date: 20191115 |