CN108947777A - A kind of concentration and separation technique of the low concentration multicomponent containing phenol mixture - Google Patents
A kind of concentration and separation technique of the low concentration multicomponent containing phenol mixture Download PDFInfo
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Abstract
A kind of concentration and separation technique the present invention provides low concentration multicomponent containing phenol mixture, successively include comprising: 3, 5- xylenol purification process, 3, 4- xylenol and metacresol purification process, isophorone purification process, isopropylidene acetone and mesitylene purification process, described 3, 5- xylenol purification process includes crystallization and purification and decoloration rectifying, 3, 4- xylenol and metacresol purification process include alkalization split-phase, it is acidified split-phase, rectifying and secondary rectifying, isophorone purification process includes molecular distillation and the rectification under vacuum of phegma, isopropylidene acetone and mesitylene purification process include the rectification under vacuum of distillate.The depths that the present invention carries out high-efficiency cleaning to a variety of byproducts generated during isophorone aromatisation preparation 3,5-dimethylphenol is managed, and can be realized the maximization of raw material availability, has significant economic benefit and social benefit.
Description
Technical field
The invention belongs to process for separating and purifying fields, are more particularly to a kind of enrichment of the low concentration multicomponent containing phenol mixture
Separating technology.
Background technique
Isophorone (Isophorone, ISO) is the product of condensation of acetone, chemical name: 3,5,5- trimethyl -2- hexamethylenes
- 1 ketone of alkene, molecular formula: C9H14O, molecular weight: 138.21, appearance colorless or light yellow transparent liquid have higher, low suction
It is moist, solvability, dispersibility, good leveling property.Isophorone is the good solvent of high molecular material, can dissolve nitrocellulose
Element, acrylate, alkyd resin, polyester and epoxy resin etc..Since isophorone has the structure of beta-unsaturated ketone, double bond can be into
One step, which reacts, generates the staple products such as alcohol, acid, amine, ester and isocyanates, in the industry such as plastics, pesticide, medicine, coating
Tool has been widely used.
3,5-dimethylphenol is white crystal, molecular formula C8H10O, molecular weight 122.17, fusing point: 63-66 DEG C, boiling
Point: 222 DEG C, density: 0.968, CAS 108-68-9 is dissolved in water and ethyl alcohol.3,5- xylenol can be used for phenolic aldehyde tree processed
Rouge, medicine, insecticide, dyestuff and explosive are the intermediates for preparing carbamate insecticides methiocarb, it may also be used for production
Rubber accelerator, antiaging agent, drug, fragrance, phenolic resin etc..3,5- xylenol also serves as the addition of steel rolling cold-rolled lubricating oil
Agent can extend cold-rolled lubricating oil service life.
Isophorone aromatisation preparation 3,5-dimethylphenol reaction process is mainly to pass through the route progress of two competitions
's.One of process is the phenolic ketone rearrangement process after isophorone demethanation, mainly generates 3,5-dimethylphenol；Another mistake
Journey is isophorone decomposable process, and a variety of by-products, which can be generated, in this process 1,3,5- trimethylbenzenes, meta-xylene, first
Benzene, metacresol, diacetone alcohol, Mesityl oxide, acetone etc..
Under the conditions of 550 DEG C, being reset by isophorone demethanation and forming 3,5-dimethylphenol is main reaction, wherein 3,5-
The content of xylenol in the reactor can reach 90%, and light component and heavy constituent that various by-products are formed respectively account for 2% left side
It is right.
Main reaction equation are as follows:
It is as follows that isophorone aromatisation prepares 3,5-dimethylphenol reaction process:
It is being at present that raw material prepares 3,5- xylenol process aspect and had more documents and materials from isophorone
And patent report, the research of reaction process is focused on to improve yield and reduce consumption, but for generating in reaction process
By-product open source information it is less.A large amount of low-boiling point material research datas for especially being generated in reaction process or less, this
If a little low-boiling point materials are not subject to collection, processing can cause serious harm to environment, and can be with if carry out categorised collection recycling
It realizes making full use of for material, significantly improves economic benefit.
Summary of the invention
The object of the present invention is to provide the low concentration multicomponents of a kind of achievable material made full use of containing phenol mixture
Concentration and separation technique.
According to an aspect of the invention, there is provided a kind of concentration and separation technique of low concentration multicomponent containing phenol mixture,
Successively include comprising: 3,5- xylenol purification process, 3,4- xylenol and metacresol purification process, isophorone mention
Pure procedure, isopropylidene acetone and mesitylene purification process,
The 3,5-dimethylphenol purification process include crystallization and purification and decoloration rectifying,
The crystallization and purification contains phenol mixture as raw material using multicomponent, and the multicomponent is contained phenol using chilled brine as refrigerant
Mixture is down to 0-1 DEG C from room temperature with the speed of 5 DEG C/h, is separated by solid-liquid separation after cooling, and respectively obtaining mass content is
The solid crude product and secondary mother liquid of the 3,5-dimethylphenol of 96-98%,
Decoloration rectifying: the solid crude product will be obtained from crystallization and purification and will be carried out in rectifying column after heating is melted into decolourizing
Purification obtains the finished product of mass content >=98% of 3,5-dimethylphenol again,
3,4- xylenol and metacresol purification process include alkalization split-phase, acidification split-phase, a rectifying and secondary fine
It evaporates,
Alkalization split-phase: being reacted at normal temperature using the NaOH solution of 15% concentration as basifier with the secondary mother liquid,
Reaction generates the sodium phenolate being soluble in the aqueous phase, and respectively obtains water phase and organic phase by oil water separator after quaternization, controls
The pH for making the water phase is 9-10,
Acidification split-phase: by the hydrochloric acid solution of 15% concentration with the resulting water phase of the alkalization split-phase in normal temperature and pressure, react
PH is to carry out acid-base neutralization reaction under 5-6 to generate phenolic substances and water, then respectively obtained by oil water separator realization
Machine phase and water phase,
Rectifying: enter by the organic phase that the acidification split-phase obtains not high in bottom temperature in a rectifying tower reactor
It is not low for the mass content for producing metacresol under the conditions of -0.098Mpa not higher than 110 DEG C, vacuum degree in 130 DEG C, tower top temperature
In 98% finished product,
Secondary rectifying: by the resulting kettle liquid of a rectifying in 155 DEG C of kettle temperature, top warm 135-140 DEG C, vacuum degree-
The crude product for being 95-97% by the mass content that secondary rectifying produces 3,5-dimethylphenol under conditions of 0.098Mpa,
Isophorone purification process includes molecular distillation and the rectification under vacuum of phegma,
Molecular distillation: the organic phase that split-phase obtains that alkalized enters in molecular distillation equipment, respectively by molecular distillation
To phegma and distillate,
The rectification under vacuum of phegma: the phegma that molecular distillation is obtained is sent into vacuum rectifying tower in bottom temperature 145-
148 DEG C, 105-107 DEG C of tower top temperature, produce under the conditions of vacuum degree -0.098Mpa isophorone mass content >=98% at
Product,
Isopropylidene acetone and mesitylene purification process include the rectification under vacuum of distillate,
The rectification under vacuum of distillate: by the distillate Jing Guo molecular distillation by rectification under vacuum bottom temperature≤110 DEG C,
65-70 DEG C of tower top temperature, isopropylidene acetone is isolated under conditions of vacuum degree -0.085Mpa, it will distillating by molecular distillation
Liquid isolates mesitylene under conditions of bottom temperature≤130 DEG C, tower top temperature≤105 DEG C, vacuum degree -0.085Mpa.
In some embodiments, 3.66% isopropylidene third that the multicomponent includes by mass percentage containing phenol mixture
Ketone, 5.25% mesitylene, 9.83% metacresol, 6.55% isophorone, 68.9% 3,5- xylenol,
2.08% 3,4- xylenol, 3.73% other components.
In some embodiments, the qualitative character content of the secondary mother liquid are as follows: isopropylidene acetone 8.75%, equal front three
Benzene 12.55%, metacresol 23.51%, isophorone (IP) 15.65%, 3,5- xylenol (MX) 25.65%, 3,4- bis-
Methylphenol 4.97%, other components 8.92%.
In some embodiments, the technological parameter of the decoloration rectifying is bottom temperature≤130 DEG C, tower top temperature≤110
DEG C, rectifying tower vacuum is -0.098Mpa.
In some embodiments, the mass content of the alkalization resulting organic phase main component of split-phase is isopropylidene third
Ketone 19.43%, mesitylene 27.87%, isophorone 34.76% and other components 17.92%.
In some embodiments, the resulting water phase of the acidification split-phase then returns to dilute hydrochloric acid preparation workshop section and is applied,
The sewage-treatment plant that enterprise is sent into after repeatedly applying carries out desalination and biochemical treatment.
In some embodiments, the mass content of the main component of the acidification split-phase organic phase obtained are as follows:
Cresols 42.76%, 3,5- xylenol 46.65%, 3,4- xylenol 9.04%, other 1.55%.
In some embodiments, the mass content of the kettle liquid main component after a rectifying is 3,5- dimethyl benzene
Phenol 81.5%, 3,4- xylenol 15.8% and other 2.7%.
In some embodiments, the resulting crude product of the secondary rectifying and the crystallization and purification obtain crude product and enter together
It is purified again in decoloration rectifying column.
In some embodiments, the mass content of the phegma main component is isophorone 66%, other components
44%, the main component of the distillate is 41% isopropylidene acetone and 59% mesitylene.
It has the advantage that: the present invention is a variety of to what is generated during preparing 3,5-dimethylphenol by means of isophorone aromatization
Byproduct carries out the depths reason of high-efficiency cleaning, can be realized the maximization of raw material availability, has significant economic benefit and society
It can benefit.The present invention successively isolates and purifies the multicomponent after enriched containing phenol mixture, realizes the efficient utilization of raw material,
Has the characteristics that significant energy conservation and environmental protection.
Detailed description of the invention
Fig. 1 is a kind of process of the concentration and separation technique of low concentration multicomponent containing phenol mixture of an embodiment of the present invention
Schematic diagram.
Specific embodiment
Can generate during preparing 3,5- xylenol as raw material using isophorone a variety of can generate a variety of by-product ratios
As the product of 3,4- xylenol, metacresol, isopropylidene acetone, mesitylene etc., the reaction distinguishes washed, decoking and knot
It will form after crystalline substance and also have a large amount of low content multicomponent mixtures outside 3,5-dimethylphenol product, after the crystallized separation in this part
Substance system be referred to as multicomponent contain phenol mixture.This mixture has crystallization at normal temperature and proposes, temperature is risen to 40 DEG C
Left and right can all dissolve, and industrially also be commonly called as " mother liquor ".A mother liquor or multicomponent mentioned below is mixed containing phenol
Object each mean more than substance.The content of each component is mass percentage content below.
Mass percentage content of the multicomponent containing phenol mixture are as follows: isopropylidene acetone 3.66%, mesitylene 5.25%,
Cresols 9.83%, isophorone (IP): 6.55%, 3,5- xylenol (MX) 68.9%, 3,4- xylenol
2.08%, other components 3.73%.
Fig. 1 schematically illustrates the concentration and separation work of the low concentration multicomponent mixture of one embodiment of the present invention
Skill.As shown in Figure 1, concentration and separation technique of the low concentration multicomponent containing phenol mixture includes: 3,5-dimethylphenol (MX) mentions
Pure procedure, 3,4- xylenol and metacresol purification process, isophorone (IP) purification process, isopropylidene acetone and equal front three
Benzene purification process.3,5- xylenol (MX) purification process includes crystallization and purification and decolorization and purification；3,4- xylenol and
Metacresol purification process includes alkalization split-phase, acidification split-phase, a rectifying and secondary rectifying；Isophorone (IP) purification process packet
Include molecular distillation；Isopropylidene acetone and mesitylene purification process include rectification under vacuum.
3,5- xylenol (MX) purification process: the process mainly passes through crystallization and rectifying obtains 3,5- dimethyl benzene
Then phenol crude product passes through rectifying and decolourizes to obtain the process of finished product 3,5- xylenol (MX).Comprising containing phenol mixture to multicomponent
Carry out crystallization and purification obtain crude product and by crystallization and purification obtain crude product carry out decoloration rectifying obtain finished product 3,5- xylenol
(MX)。
Crystallization and purification process: using multicomponent containing phenol mixture as raw material, be refrigerant by the multicomponent containing phenol with chilled brine
Mixture is down to 0-1 DEG C from room temperature with the speed of 5 DEG C/h, is separated by solid-liquid separation, is respectively obtained containing 96-98% after cooling
3,5- xylenol solid crude product and liquid secondary mother liquid.The qualitative character content of secondary mother liquid are as follows: isopropylidene acetone
8.75%, mesitylene 12.55%, metacresol 23.51%, isophorone (IP) 15.65%, 3,5- xylenol (MX)
25.65%, 3,4- xylenol 4.97%, other components 8.92%.
Decolorization and purification: since 3,5-dimethylphenol its color obtained from crystallization and purification is poor, it is therefore desirable to be taken off
Color processing, and the requirement of finished product is not achieved in the total content of the crude product, therefore also needs to further increase its purity by rectifying
To reach the requirement of finished product.Crude product will be obtained from crystallization and purification to be purified again in rectifying column after heating is melted into decolourizing
Obtain 3,5- xylenol (MX) finished product of main content >=98%.The technological parameter of the decoloration rectifying is bottom temperature≤130
DEG C, tower top temperature≤110 DEG C, rectifying tower vacuum is -0.098Mpa.
2,3,4- xylenol and metacresol purification process: it is crystallized to purify obtained secondary mother liquid, pass through alkali first
Change split-phase the sodium phenolate that substance containing phenol therein generates after reacted is soluble in the aqueous phase, other organic matters pass through in organic phase
Water-oil separating respectively obtains water phase and organic phase and then is handled respectively.
The process mainly has alkalization split-phase, acidification split-phase, a rectifying and secondary rectifying.
Alkalization split-phase: it is reacted using the NaOH solution of 15% concentration as basifier with secondary mother liquid, reaction principle is
Phenolic substances is weakly acidic to carry out neutralization reaction generation sodium phenolate and water with NaOH, and water can be dissolved in by reacting the sodium phenolate generated
Phase, the water-oil separating of secondary mother liquid.The alkalinization is controlled the PH=9-10 of water phase after reaction at normal temperatures and pressures
, water phase and organic phase are respectively obtained by oil water separator after alkalization.The mass content of organic phase main component is
Isopropylidene acetone 19.43%, mesitylene 27.87%, isophorone 34.76% and other components 17.92%.Organic phase into
Enter molecular distillation operation, and water phase then enters acidification phase process.
Acidification split-phase: sodium phenolate can react in water phase for weak acid strong alkali salt with strong acid, with the salt of 15% concentration
Acid solution and previous step alkalization split-phase and the water phase come carries out acid-base neutralization reaction and generates phenolic substances and water.Phenolic substances can be with
It floats on above water phase, organic phase and water phase is respectively obtained by oil water separator realization.Organic phase is mainly phenols crude product
It is purified into a rectifying, water phase then returns to dilute hydrochloric acid preparation workshop section and applied, and the dirt of enterprise is sent into after repeatedly applying
Water treatment facilities carries out desalination and biochemical treatment.It is acidified the mass content of the main component of split-phase organic phase obtained are as follows:
Cresols 42.76%, 3,5- xylenol 46.65%, 3,4- xylenol 9.04%, other 1.55%.Main control ginseng
Number is normal temperature and pressure, reaction PH=5-6.
Rectification and purification: the organic phase that acidification split-phase obtains enters in a rectifying tower reactor to be not higher than in bottom temperature
130 DEG C, tower top temperature not higher than 110 DEG C, vacuum degree be -0.098Mpa under the conditions of extraction metacresol content not less than 98% at
Product.Since the molten boiling point of metacresol is lower therefore is easiest to preferentially separate extraction when rectifying, after a rectifying
Kettle liquid enters secondary rectifying and separates again.The mass content of kettle liquid main component after rectifying is 3,5- xylenol
81.5%, 3,4- xylenol 15.8% and other 2.7%.
Secondary rectification and purification: by the kettle liquid of a rectifying in 155 DEG C of kettle temperature, top warm 135-140 DEG C, vacuum degree-
The crude product that 3,5-dimethylphenol content is 95-97%, the crude product and certainly crystallization are produced by rectifying under conditions of 0.098Mpa
Purification obtains crude product and is purified again in rectifying column into decolourizing together.And what is obtained after secondary purification is rich in 3,4- bis-
The substance of methylphenol crude product is purified to obtain 3,4- xylenol finished product directly in tower reactor again.Secondary rectification and purification
Process can complete purification operations in a rectifying column, which is gap operating, and purification first obtains 3,5- bis-
Methylphenol crude product then proceedes to qualified 3, the 4- xylenol finished product of rectifying extraction.
Isophorone (IP) purification process: the organic phase that split-phase obtains that alkalized enters in molecular distillation, utilizes isopropylidene
The difference of acetone, mesitylene and isophorone molecular tools realizes the separation of substance, which is mainly
Isopropylidene acetone and mesitylene separated from organic phase system, in order to separate in next step.The molecular distillation
Device model is MK/FEEL-6.0, vacuum degree 0.13Pa, respectively obtains phegma and distillate by molecular distillation, reflux
Liquid is also referred to as heavy constituent, and distillate is also referred to as light component.The mass content of phegma main component is isophorone 66%, other components
44%；The main component of distillate is 41% and mesitylene 59%.
There is up to tens kinds of component since the component of organic phase is especially complex, is difficult to realize group using conventional rectification means
The purifying divided, it is therefore desirable to use and be different from tradition by the method for boiling-point difference separation.
The rectification under vacuum of phegma: the phegma that molecular distillation is obtained is sent into vacuum rectifying tower in bottom temperature 145-
148 DEG C, 105-107 DEG C of tower top temperature, produce under the conditions of vacuum degree -0.098Mpa isophorone mass content >=98% at
Product.
After isophorone produces, in 155-160 DEG C of kettle temperature, warm 120-125 DEG C, vacuum degree -0.098Mpa condition are pushed up
Under continue to produce organic phase, which can be used as high boiling solvent.Its component of the high boiling solvent is more miscellaneous, more mainly
Virtue, ketone compounds.
Isopropylidene acetone and mesitylene purification process: the distillate obtained after molecular distillation is purer different
The mixture of propylidene acetone and mesitylene.The larger feature of boiling-point difference according to both components, can pass through traditional vacuum
The separation of rectifying realization component.Isopropylidene acetone distillation process specific process parameter is bottom temperature≤110 DEG C, tower top temperature
65-70 DEG C, vacuum degree -0.085Mpa；Mesitylene rectification process parameter is bottom temperature≤130 DEG C, tower top temperature≤105
DEG C, vacuum degree -0.085Mpa.It is higher than 98% finished product isopropyl by the mass content that rectification under vacuum respectively obtains main component
Pitch two kinds of valuable constituents of acetone and mesitylene.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, it is not taking off
Under the premise of from the invention design, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.
Claims (10)
1. a kind of concentration and separation technique of low concentration multicomponent containing phenol mixture, which is characterized in that successively include comprising: 3,5- bis-
Methylphenol purification process, 3,4- xylenol and metacresol purification process, isophorone purification process, isopropylidene acetone and
Mesitylene purification process,
The 3,5-dimethylphenol purification process include crystallization and purification and decoloration rectifying,
The crystallization and purification contains phenol mixture as raw material using multicomponent, mixes the multicomponent containing phenol using chilled brine as refrigerant
Object is down to 0-1 DEG C from room temperature with the speed of 5 DEG C/h, is separated by solid-liquid separation after cooling, and respectively obtaining mass content is 96-
The solid crude product and secondary mother liquid of 98% 3,5-dimethylphenol,
Decoloration rectifying: the solid crude product will be obtained from crystallization and purification and will be carried out again in rectifying column after heating is melted into decolourizing
Purification obtains the finished product of mass content >=98% of 3,5-dimethylphenol,
3,4- xylenols and metacresol purification process include alkalization split-phase, are acidified split-phase, a rectifying and secondary rectifying,
Alkalization split-phase: being reacted at normal temperature using the NaOH solution of 15% concentration as basifier with the secondary mother liquid, is reacted
The sodium phenolate being soluble in the aqueous phase is generated, water phase and organic phase are respectively obtained by oil water separator after quaternization, controls institute
The pH for stating water phase is 9-10,
Acidification split-phase: by the hydrochloric acid solution of 15% concentration and the resulting water phase of the alkalization split-phase in normal temperature and pressure, react pH and be
Acid-base neutralization reaction is carried out under 5-6 and generates phenolic substances and water, then organic phase is respectively obtained by oil water separator realization
And water phase,
Rectifying: enter in a rectifying tower reactor by the organic phase that the acidification split-phase obtains and be not higher than in bottom temperature
130 DEG C, tower top temperature not higher than 110 DEG C, vacuum degree be -0.098Mpa under the conditions of extraction metacresol content not less than 98% at
Product,
Secondary rectifying: by the resulting kettle liquid of a rectifying in 155 DEG C of kettle temperature, top warm 135-140 DEG C, vacuum degree-
The crude product for being 95-97% by the mass content that secondary rectifying produces 3,5-dimethylphenol under conditions of 0.098Mpa,
Isophorone purification process includes molecular distillation and the rectification under vacuum of phegma,
Molecular distillation: the organic phase that split-phase obtains that alkalized enters in molecular distillation equipment, is respectively obtained back by molecular distillation
Flow liquid and distillate,
The rectification under vacuum of phegma: the phegma that molecular distillation is obtained is sent into vacuum rectifying tower in bottom temperature 145-148
DEG C, produce under the conditions of 105-107 DEG C of tower top temperature, vacuum degree -0.098Mpa isophorone mass content >=98% finished product,
Isopropylidene acetone and mesitylene purification process include the rectification under vacuum of distillate,
The rectification under vacuum of distillate: by the distillate Jing Guo molecular distillation by rectification under vacuum in bottom temperature≤110 DEG C, tower top
65-70 DEG C of temperature, isopropylidene acetone is isolated under conditions of vacuum degree -0.085Mpa, the distillate Jing Guo molecular distillation is existed
Mesitylene is isolated under conditions of vacuum degree -0.085Mpa in bottom temperature≤130 DEG C, tower top temperature≤105 DEG C.
2. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
3.66% isopropylidene acetone that multicomponent includes by mass percentage containing phenol mixture, 5.25% mesitylene, 9.83%
Metacresol, 6.55% isophorone, 68.9% 3,5- xylenol, 2.08% 3,4- xylenol, 3.73%
Other components.
3. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
The qualitative character content of secondary mother liquid are as follows: isopropylidene acetone 8.75%, mesitylene 12.55%, metacresol 23.51%, different Buddhist
That ketone 15.65%, 3,5- xylenol 25.65%, 3,4- xylenol 4.97%, other components 8.92%.
4. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that this is de-
The technological parameter of color rectifying is bottom temperature≤130 DEG C, and tower top temperature≤110 DEG C, rectifying tower vacuum is -0.098Mpa.
5. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
Alkalize the resulting organic phase of split-phase main component mass content be isopropylidene acetone 19.43%, mesitylene 27.87%,
Isophorone 34.76% and other components 17.92%.
6. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
The acidification resulting water phase of split-phase then returns to dilute hydrochloric acid preparation workshop section and is applied, and the sewage treatment dress of enterprise is sent into after repeatedly applying
It sets and carries out desalination and biochemical treatment.
7. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
It is acidified the mass content of the main component of split-phase organic phase obtained are as follows: metacresol 42.76%, 3,5- xylenol
46.65%, 3,4- xylenol 9.04%, other 1.55%.
8. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
The mass content of the main component of kettle liquid after rectifying is 3,5- xylenol 81.5%, 3,4- xylenol
15.8% and other 2.7%.
9. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that described
The secondary resulting crude product of rectifying and the crystallization and purification obtain crude product and are purified again in rectifying column into decolourizing together.
10. concentration and separation technique of the low concentration multicomponent according to claim 1 containing phenol mixture, which is characterized in that institute
The mass content for stating phegma main component is isophorone 66%, and the main component of other components 44%, the distillate is
41% isopropylidene acetone and 59% mesitylene.
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| CN115108888A (en) * | 2022-07-05 | 2022-09-27 | 山东奥友化学有限责任公司 | Separation and purification method of byproducts in 4-chloro-3-methylphenol production and mildew-proof antibacterial liquid containing byproducts |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417248A (en) * | 2010-09-27 | 2012-04-18 | 新奥科技发展有限公司 | Method for processing and recycling waste water containing phenolic compounds |
| CN104151143A (en) * | 2014-07-24 | 2014-11-19 | 连云港科铭化工有限公司 | Paracresol production crude distillation residue recovery treatment method |
| CN104230669A (en) * | 2014-09-11 | 2014-12-24 | 苏州飞翔新材料研究院有限公司 | Separation and purification method of m-cresol |
| CN107573227A (en) * | 2017-08-30 | 2018-01-12 | 中国石油大学(华东) | Acetone vapour phase condensation prepares the device and method of isophorone |
| CN107721826A (en) * | 2017-10-27 | 2018-02-23 | 陕西煤业化工集团神木天元化工有限公司 | The method and device of a variety of phenol is separated in a kind of therefrom coalite tar crude phenols |
-
2018
- 2018-05-31 CN CN201810547922.2A patent/CN108947777B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417248A (en) * | 2010-09-27 | 2012-04-18 | 新奥科技发展有限公司 | Method for processing and recycling waste water containing phenolic compounds |
| CN104151143A (en) * | 2014-07-24 | 2014-11-19 | 连云港科铭化工有限公司 | Paracresol production crude distillation residue recovery treatment method |
| CN104230669A (en) * | 2014-09-11 | 2014-12-24 | 苏州飞翔新材料研究院有限公司 | Separation and purification method of m-cresol |
| CN107573227A (en) * | 2017-08-30 | 2018-01-12 | 中国石油大学(华东) | Acetone vapour phase condensation prepares the device and method of isophorone |
| CN107721826A (en) * | 2017-10-27 | 2018-02-23 | 陕西煤业化工集团神木天元化工有限公司 | The method and device of a variety of phenol is separated in a kind of therefrom coalite tar crude phenols |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115108888A (en) * | 2022-07-05 | 2022-09-27 | 山东奥友化学有限责任公司 | Separation and purification method of byproducts in 4-chloro-3-methylphenol production and mildew-proof antibacterial liquid containing byproducts |
| CN115108888B (en) * | 2022-07-05 | 2024-05-17 | 山东奥友化学有限责任公司 | Separation and purification method of byproducts in production of 4-chloro-3-methylphenol and mildew-proof antibacterial liquid containing byproducts |
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