CN106986739A - The production technology that a kind of phenol raffinate is recycled - Google Patents
The production technology that a kind of phenol raffinate is recycled Download PDFInfo
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- CN106986739A CN106986739A CN201710221289.3A CN201710221289A CN106986739A CN 106986739 A CN106986739 A CN 106986739A CN 201710221289 A CN201710221289 A CN 201710221289A CN 106986739 A CN106986739 A CN 106986739A
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- phenol
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention belongs to environmental protective chemical industry field, more particularly to the production technology that a kind of phenol raffinate is recycled.It is made up of storage tank, delivery pump, bottom of towe kettle, electric heater, rectifying column, condenser, vavuum pump, reflux ratio controller, collecting tank, Venturi tube blender, phenol collecting tank, extract and separate tank, circulating pump, Forced Mixing device, static mixer, compression pump, emulsifying agent holding vessel, fuel oil holding vessel, emulsified fuel oil collecting tank, cryogenic system, absorbent charcoal adsorber；Thick cut is broadly divided into from the technical process that, rectifying separation, phenol purification, exhaust-gas treatment, residue are recycled, this technical process takes Batch Process mode.
Description
Technical field
The invention belongs to environmental protective chemical industry field, more particularly to the production technology that a kind of phenol raffinate is recycled.
Background technology
Phenol raffinate refers in cumene oxidation legal system phenol manufacturing process, isolates remaining part mixing after phenol
Thing；Its main component has α-methylstyrene, paraxylene, isopropylbenzene, phenol, acetophenone etc., wherein α-methylstyrene most
It is many.Acetophenone is used for perfumed soap processed and cigarette, also serves as the plasticising in the solvent and plastics industry production of cellulose esters and resin etc.
Agent etc..It can be made, or be made by ethylbenzene oxidation with acetic anhydride by benzene, it is also possible to which chloroacetic chloride is with benzene under alchlor effect
It is made through Friedel-crafts reaction；Isopropylbenzene is a kind of colourless liquid for having a special aromatic odor.Be mainly used as production phenol and acetone, α-
Methyl styrene etc., it is also possible to make organic synthesis raw material and improve the additive of engine fuel octane, be important industry
Raw material.Industrially, isopropylbenzene is prepared mainly using benzene and propylene as raw material in the presence of catalyst through alkylated reaction.Pass
System method prepares isopropylbenzene, though can largely produce, because of the different choice of catalyst, can cause equipment corrosion, production environment
It is seriously polluted, in addition cause isopropylbenzene purity it is not high a series of problems, such as.Meanwhile, production process is cumbersome, produces complicated；
α-methylstyrene, which is called, does α-phenylethylene or propyloxy phenyl alkene, is a kind of colourless or lurid transparent liquid in appearance
Body, is commonly used for monomer or modified monomer that polymerisation produces adhesive base-material, be synthetic resin and plastics important monomer it
One, it is also the modifying agent of polyester resin, alkyd resin and ABS resin.It can be additionally used in production coating, plasticizer etc., be a kind of weight
The industrial chemicals wanted.Therefore phenol, acetophenone, α-methylstyrene and isopropylbenzene these four materials are reclaimed from phenol raffinate is
It is very necessary, be conducive to resource reclaim and environmental protection.
According to documents, the recycling of original phenol raffinate has only reclaimed the thing of two kinds of useful constituents of phenol and acetophenone
Matter, and removal process need to add catalyst and high-temperature solvent oil, and this process is without catalyst and technological operation is simple,
And phenol, acetophenone, four kinds of utilities of α-methylstyrene and isopropylbenzene can be reclaimed simultaneously, and purity is very high.
Documents：Invention is authorized：A kind of method that phenol and acetophenone are reclaimed from phenol tar,
2012101176825；The method and apparatus that phenol tar refines p -cumylphenol, 2012103221007.
The content of the invention
The production technology that a kind of phenol raffinate is recycled, by storage tank, delivery pump, bottom of towe kettle, electric heater, rectifying
Tower, condenser, vavuum pump, reflux ratio controller, collecting tank, Venturi tube blender, phenol collecting tank, extract and separate tank, circulation
Pump, Forced Mixing device, static mixer, compression pump, emulsifying agent holding vessel, fuel oil holding vessel, emulsified fuel oil collecting tank, depth
Device for cooling, absorbent charcoal adsorber composition；It is broadly divided into thick cut from, rectifying separation, phenol purification, exhaust-gas treatment, residue again
The technical process utilized.This technical process takes Batch Process mode；
（1）Thick cut from：Phenol raffinate in head tank is pumped into bottom of towe kettle, 210 DEG C are heated to by phenol and acetophenone
Mixed vapour is separated, after condenser cools, by after reflux ratio controller respectively with 5:1 ratio is delivered to reaction
In tower and collecting tank A；Through after a period of time, then bottom of towe kettle is heated to 150 DEG C mixes α-methylstyrene and isopropylbenzene
Steam is separated, after condenser cools, by after reflux ratio controller respectively with 5:1 ratio be delivered to reaction tower and
In collecting tank B；Phenol in collecting tank A and acetophenone mixture pump are sent in bottom of towe kettle and carry out rectifying, by α-first in collecting tank B
Base styrene and isopropylbenzene mixture pump are sent to head tank and wait rectifying；During this using vavuum pump make in device keep-
0.1MPa vacuum, improves gas rate flow.
（2）Rectifying is separated：Phenol and acetophenone mixture pump are sent to after bottom of towe kettle, are kept at bottom of towe temperature in the kettle
160 DEG C and 200 DEG C, phenol and acetophenone are separated in two collecting tanks, produced acetophenone after separation completely, phenol is carried out
Purify again；Then α-methylstyrene and isopropylbenzene mixture pump are sent to bottom of towe kettle, bottom of towe kettle temperature degree is kept at 130
DEG C and 150 DEG C, α-methylstyrene and isopropylbenzene is separated in two collecting tanks, separation completely after produce；It is sharp during this
Make holding -0.1MPa vacuums in device with vavuum pump, improve gas rate flow.
（3）Phenol is purified：Still there is acetophenone in phenol after rectifying, must be purified, it is beaten using delivery pump
Enter and uniformly mixed in Venturi tube blender, the liquid after having mixed is entered in extract and separate tank and is layered, then will layering
The phenol extraction in solution, which comes out, afterwards is stored in phenol collecting tank, and this process can make phenol purity reach 99.5%.
（4）Exhaust-gas treatment：Slightly evaporating and its is kept negative pressure, the gas so extracted using vavuum pump in rectifying separation process
It can be discharged after need to handling, the waste gas of extraction is passed sequentially through into cryogenic system and absorbent charcoal adsorber, cryogenic system setting temperature
Degree -10 DEG C or so by portion be changed into waste collection extraction, can re-start thick cut from；Remainder of exhaust gas will pass through activity
Charcoal adsorbent equipment can be discharged into air after being adsorbed.
（5）Residue is recycled：The residue after rectifying and fuel oil, emulsifying agent are thrown into Forced Mixing by delivery pump respectively
Device carries out Forced Mixing, enters after having mixed in static mixer, and incorporation time is 15 ~ 30min, and mixing temperature is 60 ~ 80
℃；By compression pump forced circulation, finally throw emulsified fuel oil into static mixer by delivery pump and stored up again to emulsified fuel oil
Deposit tank.
Fig. 1 is the structural representation of phenol raffinate reuse means；
1 is storage tank in figure, and 2 be delivery pump, and 3 be bottom of towe kettle, and 4 be electric heater, and 5 be rectifying column, and 6 be condenser, and 7 are
Vavuum pump, 8 be reflux ratio controller, and 9 be collecting tank, and 10 be Venturi tube blender, and 11 be phenol collecting tank, and 12 be extract and separate
Tank, 13 be circulating pump, and 14 be Forced Mixing device, and 15 be static mixer, and 16 be pump, and 17 be emulsifying agent holding vessel, and 18 be fuel
Oily holding vessel, 19 be emulsified fuel oil collecting tank, and 20 be cryogenic system, and 21 be absorbent charcoal adsorber.
Embodiment
The production technology that a kind of phenol raffinate is recycled, by storage tank, delivery pump, bottom of towe kettle, electric heater, rectifying
Tower, condenser, vavuum pump, reflux ratio controller, collecting tank, Venturi tube blender, phenol collecting tank, extract and separate tank, circulation
Pump, Forced Mixing device, static mixer, compression pump, emulsifying agent holding vessel, fuel oil holding vessel, emulsified fuel oil collecting tank, depth
Device for cooling, absorbent charcoal adsorber composition；It is broadly divided into thick cut from, rectifying separation, phenol purification, exhaust-gas treatment, residue again
The technical process utilized.This technical process takes Batch Process mode.
（1）Thick cut from：Phenol raffinate in head tank is pumped into bottom of towe kettle, 210 DEG C are heated to by phenol and benzene
Ethyl ketone mixed vapour is separated, after condenser cools, by after reflux ratio controller respectively with 5:1 ratio is delivered to
In reaction tower and collecting tank A；150 DEG C are heated to by α-methylstyrene and isopropylbenzene through after a period of time, then by bottom of towe kettle
Mixed vapour is separated, after condenser cools, by after reflux ratio controller respectively with 5:1 ratio is delivered to reaction
In tower and collecting tank B；Phenol in collecting tank A and acetophenone mixture pump are sent in bottom of towe kettle and carry out rectifying, by collecting tank B
α-methylstyrene and isopropylbenzene mixture pump are sent to head tank and wait rectifying；Make guarantor in device using vavuum pump during this
- 0.1MPa vacuum is held, gas rate flow is improved；
（2）Rectifying is separated：Phenol and acetophenone mixture pump are sent to after bottom of towe kettle, bottom of towe temperature in the kettle is kept at 160
DEG C and 200 DEG C, phenol and acetophenone are separated in two collecting tanks, separation completely after acetophenone is produced, phenol carry out again
Purification；Then α-methylstyrene and isopropylbenzene mixture pump are sent to bottom of towe kettle, bottom of towe kettle temperature degree is kept at 130 DEG C
With 150 DEG C, α-methylstyrene and isopropylbenzene is separated in two collecting tanks, separation completely after produce；Utilized during this
Vavuum pump makes the vacuum of holding -0.1MPa in device, improves gas rate flow.
（3）Phenol is purified：Still there is acetophenone in phenol after rectifying, must be purified, it is beaten using delivery pump
Enter and uniformly mixed in Venturi tube blender, the liquid after having mixed is entered in extract and separate tank and is layered, then will layering
The phenol extraction in solution, which comes out, afterwards is stored in phenol collecting tank, and this process can make phenol purity reach 99.5%.
（4）Exhaust-gas treatment：Slightly evaporating and its is kept negative pressure, the gas so extracted using vavuum pump in rectifying separation process
It can be discharged after need to handling, the waste gas of extraction is passed sequentially through into cryogenic system and absorbent charcoal adsorber, cryogenic system setting temperature
Degree -10 DEG C or so by portion be changed into waste collection extraction, can re-start thick cut from；Remainder of exhaust gas will pass through activity
Charcoal adsorbent equipment can be discharged into air after being adsorbed.
（5）Residue is recycled：The residue after rectifying and fuel oil, emulsifying agent are thrown into Forced Mixing by delivery pump respectively
Device carries out Forced Mixing, and incorporation time is 15 ~ 30min, and temperature is 60 ~ 80 DEG C；Enter after having mixed in static mixer, lead to
Excess pressure pump forced circulation, finally throws emulsified fuel oil into static mixer again to emulsified fuel oil holding vessel by delivery pump.
By said process, phenol, acetophenone, four kinds of materials of α-methylstyrene and isopropylbenzene are obtained, its data is as follows：
Table 1 is the analysis result table for reclaiming phenol
| Peak number | Component | Peak height（uV） | Retention time（min） | Peak area（*#） | Area % | Content % |
| 1 | 94 | 2.375 | 139 | 0.00225 | 0.00225 | |
| 2 | 12 | 2.786 | 14 | 0.00023 | 0.00023 | |
| 3 | 174 | 4.016 | 361 | 0.00583 | 0.00583 | |
| 4 | 288 | 4.232 | 776 | 0.01255 | 0.01255 | |
| 5 | 13 | 4.378 | 44 | 0.00071 | 0.00071 | |
| 6 | 1325733 | 4.599 | 6176267 | 99.66908 | 99.66908 | |
| 7 | 10802 | 4.696 | 17919 | 0.28917 | 0.28917 | |
| 8 | 59 | 4.808 | 157 | 0.00263 | 0.00263 | |
| 9 | 322 | 4.871 | 594 | 0.00959 | 0.00959 | |
| 10 | 30 | 6.071 | 30 | 0.00048 | 0.00048 | |
| 11 | 6 | 10.095 | 470 | 0.00759 | 0.00759 | |
| Amount to | 1337633 | 6196774 | 100 | 100 |
Table 2 is the analysis result table for reclaiming acetophenone
| Peak number | Component | Peak height（uV） | Retention time（min） | Peak area（*#） | Area % | Content % |
| 1 | 13 | 2.356 | 42 | 0.00141 | 0.00141 | |
| 2 | 61 | 2.523 | 248 | 0.00823 | 0.00823 | |
| 3 | 235 | 2.861 | 479 | 0.01594 | 0.01594 | |
| 4 | 382 | 3.222 | 855 | 0.02845 | 0.02845 | |
| 5 | 27 | 3.603 | 65 | 0.00216 | 0.00216 | |
| 6 | 163 | 3.588 | 335 | 0.01113 | 0.01113 | |
| 7 | 132 | 3.625 | 347 | 0.01153 | 0.01153 | |
| 8 | 737 | 3.74 | 1831 | 0.06089 | 0.06089 | |
| 9 | 338 | 3.953 | 927 | 0.03082 | 0.03082 | |
| 10 | 275 | 4.209 | 777 | 0.02585 | 0.02585 | |
| 11 | 541283 | 4.547 | 2980639 | 98..42692 | 98..42692 | |
| 12 | 3336 | 4.745 | 693 | 0.26241 | 0.26241 | |
| 13 | 662 | 5.187 | 1843 | 0.06145 | 0.06145 | |
| 14 | 270 | 5.618 | 0.02655 | 0.02655 |
Table 3 is the analysis result table for reclaiming α-methylstyrene
| Peak number | Component | Peak height（uV） | Retention time（min） | Peak area（*#） | Area % | Content % |
| 1 | 15 | 0.173 | 44 | 0.00302 | 0.00302 | |
| 2 | 31 | 0.321 | 62 | 0.00421 | 0.00421 | |
| 3 | 24 | 0.611 | 58 | 0.00397 | 0.00397 | |
| 4 | 690 | 3.199 | 1556 | 0.1059 | 0.1059 | |
| 5 | 54 | 3.45 | 119 | 0.00811 | 0.00811 | |
| 6 | 29 | 3.645 | 73 | 0.00494 | 0.00494 | |
| 7 | 739 | 3.876 | 2107 | 0.14341 | 0.14341 | |
| 8 | 45 | 4.08 | 62 | 0.00423 | 0.00423 | |
| 9 | 458802 | 4.37 | 1462293 | 99.5265 | 99.5265 | |
| 10 | 697 | 4.679 | 1872 | 0.12744 | 0.12744 | |
| 11 | 29 | 7.337 | 129 | 0.00878 | 0.00878 | |
| 12 | 12 | 7.837 | 33 | 0.00228 | 0.00228 | |
| 13 | 47 | 9.256 | 368 | 0.02505 | 0.02505 | |
| 14 | 34 | 9.617 | 196 | 0.01332 | 0.01332 |
Table 4 is the analysis result table for reclaiming isopropylbenzene
| Peak number | Component | Peak height（uV） | Retention time（min） | Peak area（*#） | Area % | Content % |
| 1 | 17 | 0.951 | 18 | 0.00036 | 0.00036 | |
| 2 | 177 | 3.507 | 322 | 0.00646 | 0.00646 | |
| 3 | 1361 | 3.706 | 2682 | 0.05391 | 0.05391 | |
| 4 | 30 | 3.785 | 93 | 0.00188 | 0.00188 | |
| 5 | 1325416 | 3.972 | 4970463 | 99.90978 | 99.90978 | |
| 6 | 400 | 4.151 | 779 | 0.01566 | 0.01566 | |
| 7 | 363 | 4.194 | 594 | 0.01194 | 0.01194 | |
| Amount to | 1327764 | 4974951 | 100 | 100 |
Claims (1)
1. the production technology that a kind of phenol raffinate is recycled, by storage tank, delivery pump, bottom of towe kettle, electric heater, rectifying
Tower, condenser, vavuum pump, reflux ratio controller, collecting tank, Venturi tube blender, phenol collecting tank, extract and separate tank, circulation
Pump, Forced Mixing device, static mixer, compression pump, emulsifying agent holding vessel, fuel oil holding vessel, emulsified fuel oil collecting tank, depth
Device for cooling, absorbent charcoal adsorber composition；It is broadly divided into thick cut from, rectifying separation, phenol purification, exhaust-gas treatment, residue again
The technical process utilized；This technique takes Batch Process mode；Concrete mode is as follows：
（1）Thick cut from when the phenol raffinate in head tank be pumped into bottom of towe kettle be heated to 210 DEG C and mix phenol and acetophenone
Steam is closed to separate；Bottom of towe kettle is heated into 150 DEG C again to separate α-methylstyrene and isopropylbenzene mixed vapour；
Holding -0.1MPa vacuums in device during this；
（2）Rectifying makes bottom of towe temperature in the kettle be kept at 160 DEG C and 200 DEG C when separating, and phenol and acetophenone are separated；Then
Bottom of towe kettle temperature degree is kept at 130 DEG C and 150 DEG C, α-methylstyrene and isopropylbenzene are separated；During this in device
Holding -0.1MPa vacuums, improve gas rate flow；
（3）Phenol is uniformly mixed with acetophenone therein using Venturi tube blender；
（4）Waste gas passes sequentially through cryogenic system and absorbent charcoal adsorber, and cryogenic system design temperature is at -10 DEG C；
（5）Residue after rectifying and fuel oil, emulsifying agent are subjected to Forced Mixing by Forced Mixing device, incorporation time is
20min, temperature is 70 DEG C；Enter after having mixed in static mixer.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110054340A (en) * | 2019-05-27 | 2019-07-26 | 太仓塑料助剂厂有限公司 | The waste water adsorption method of cumyl peroxide |
| CN112142545A (en) * | 2020-09-29 | 2020-12-29 | 浙江大学 | Method for separating isopropyl benzene and alpha-methyl styrene |
| CN112778096A (en) * | 2021-02-24 | 2021-05-11 | 乐陵力维化学品有限责任公司 | Method for efficiently recycling phenol residual liquid |
| CN113511959A (en) * | 2020-04-10 | 2021-10-19 | 上海寰球工程有限公司 | System for separating phenol and acetophenone from tar |
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| CN112142545B (en) * | 2020-09-29 | 2021-08-31 | 浙江大学 | Method for separating isopropyl benzene and alpha-methyl styrene |
| CN112778096A (en) * | 2021-02-24 | 2021-05-11 | 乐陵力维化学品有限责任公司 | Method for efficiently recycling phenol residual liquid |
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