CN107512751A - A kind of concentration technology of cyclohexanone saponification waste lye - Google Patents

A kind of concentration technology of cyclohexanone saponification waste lye Download PDF

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Publication number
CN107512751A
CN107512751A CN201610439353.0A CN201610439353A CN107512751A CN 107512751 A CN107512751 A CN 107512751A CN 201610439353 A CN201610439353 A CN 201610439353A CN 107512751 A CN107512751 A CN 107512751A
Authority
CN
China
Prior art keywords
salkali waste
evaporating column
lye
compressor
saponification
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610439353.0A
Other languages
Chinese (zh)
Inventor
黎树根
刘洪武
李勇华
龙伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Baling Co
Original Assignee
China Petroleum and Chemical Corp
Sinopec Baling Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Sinopec Baling Co filed Critical China Petroleum and Chemical Corp
Priority to CN201610439353.0A priority Critical patent/CN107512751A/en
Publication of CN107512751A publication Critical patent/CN107512751A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/041Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds

Abstract

The invention discloses a kind of concentration technology of cyclohexanone saponification waste lye, cyclohexanone saponification waste lye evaporation gas phase is compressed using compressor, as the thermal source of cyclohexanone saponification waste lye concentration, the consumption of steam during so as to which concentration is greatly reduced.Energy consumption of the invention is low, good economy performance, is not in foaming and crystallization.

Description

A kind of concentration technology of cyclohexanone saponification waste lye
Technical field
The invention belongs to cyclohexanone saponification waste lye process field, and in particular to a kind of concentration work of cyclohexanone saponification waste lye Skill.
Background technology
Cyclohexanol and cyclohexanone are prepared, typically with the gas oxidizing ethyle alkyl of molecule-containing keto, firstly generates peroxide containing cyclohexyl Change the oxidation mixture (being commonly called as cyclohexane oxide solution) of hydrogen, cyclohexanol and cyclohexanone, then with 30% sodium hydroxide liquid caustic soda This oxidation mixture is handled, cyclohexyl hydroperoxide therein is decomposed generation cyclohexanol and cyclohexanone.Due in cyclohexyl Liquid caustic soda is introduced in hydrogen peroxide decomposable process, thus the saponification waste lye of high COD concentration can be produced, every about 1 ton of ring of production Hexanone can produce 0.8 ton of saponification waste lye.This saponification waste lye is because COD concentration is high, pH value reaches 10-14 and comparison is difficult Processing, if directly discharging, it will cause serious environmental pollution.
Current cyclohexanone saponification waste lye handling process is burning method at present, if the solid contents in saponification waste lye is too If low, fuel is on the one hand consumed more, incinerator flame on the other hand can be caused unstable, flame-out risk be present.So soap Changing before spent lye enters incinerator needs to carry out concentration.The concentration of common saponification waste lye is to take steam distillation shape in industry Formula, 1 ton of steam will be consumed by often steaming 1 ton of water, even if using double-effect evaporation, 0.6 ton of steam will be consumed by often steaming 1 ton of water. And due in the saponification waste lye in addition to containing sodium hydroxide, sodium carbonate, it is also existing containing a certain amount of carboxylic acid sodium, use Method for concentration is easy to make whole thing system bubble, plus easily crystallization again after concentration, when solid content has been begun to up to 45% or so Crystallization separates out and grain diameter is larger, easy blocking pipeline, is not easy to concentrate the technique conveying of spent lye, influences the length of device Periodic duty, therefore, cyclohexanone saponification waste lye condensing mode and power saving, which seem, to become more and more important.
The content of the invention
The invention aims to solve high energy consumption, foaming and Crystallization Plugging pipeline in cyclohexanone saponification waste lye concentration process The problem of, and propose that a kind of energy consumption is low, good economy performance, be not in the cyclohexanone saponification waste lye of foaming and pipe plugging by crystallization Concentration technology.
Problem solved by the invention can be realized using following technical scheme:
A kind of concentration technology of cyclohexanone saponification waste lye, the saponification waste lye after oxidizing cyclohexanone decomposition process enter useless Alkali evaporating column, gained evaporation gas phase enters pressure after salkali waste evaporates the foam removal of column overhead demister and cyclone hydraulic separators separation after evaporation Contracting machine compresses, and gained compression gas phase exchanges heat with the saponification waste lye of evaporator shell side and tube side after compression, compression gas phase cooling Liquid phase afterwards is discharged into water treatment system as lime set, the water in saponification waste lye vaporized after being heated obtained water evaporation gas phase from The tower top discharge of salkali waste evaporating column.
The present invention further comprises following preferable technical scheme:
In preferable scheme, ultrasonic cleaner is set in salkali waste evaporating column tower reactor and pump inlet pipeline.Utilize ultrasound The percussion of ripple, crystallization is set not form large-sized particle.
By above-mentioned setting, cyclohexanone saponification waste lye does not have large particle crystal precipitation and blocked after can further making concentration Pipeline.
In preferable scheme, the salkali waste evaporating column tower reactor liquid phase uses circulating pump forced circulation between evaporator and tower reactor.
In preferable scheme, the salkali waste evaporating column is tower structure, and demister is arranged on salkali waste evaporating column top, the rotation Liquid/gas separator is arranged on top gaseous phase pipeline, for carrying out gas-liquid phase separation.
In preferable scheme, compressor used is that compression ratio is less than 2.
In preferable scheme, compressor used is one kind in lobed rotor compressor, centrifugal compressor or air blower.
In preferable scheme, the salkali waste evaporation column overhead temperatures are 95-100 DEG C.
In preferable scheme, the salkali waste evaporating column bottom temperature is 95-105 DEG C.
In preferable scheme, the compressor exit temperature is 105-115 DEG C.
In preferable scheme, water evaporation gas phase is from the saponification waste lye after remaining concentration after the tower top discharge of salkali waste evaporating column In, solids content 50-60%.
Present invention contrast prior art has following progressive:
1st, the thermal efficiency is high, it is low to save the energy, unit work consumptiom.Evaporation 1 ton of water energy consumption be converted to mark coal be only equivalent to tradition it is general / 10 to ten/9ths of logical evaporation, energy-saving effect is notable.
2nd, clean environment firendly, new pollution is not produced.
3rd, it is suitable for easy to foaming, easy crystallizing system.
4th, in the saponification waste lye after concentrating, solids content is high, is easy to further carry out subsequent treatment.
Although compressor compresses are a kind of compress modes more conventional in mechanical field, use it for concentrating cyclohexanone saponification Spent lye is very difficult to expect, during inventor is engaged in research and development throughout the year, not yet someone carries out this kind of trial, because It is too wide in the gap for field.And inventor is had found by the way that compressor is used for into cyclohexanone saponification salkali waste in once accidental trial When in liquor treating process, discovery can obtain the unexpected effect got twice the result with half the effort.And inventor is complete in order to obtain one , handling process achievable, effect is good, continuous improvement has been carried out to technical process, has not only obtained various heats Effective recycling, has saved resource, and solve and easily go out in conventional cyclohexanone saponification waste lye handling process Existing easy to foaming, the problems such as easily crystallizing.The present invention each process seem simple, actually its combine be very cleverly, Also solve the problems, such as long-standing problem technical staff, consume the substantial amounts of energy of inventor, by small-scale practical application, It was found that it has very strong practicality, huge economic benefit can be brought.
Brief description of the drawings
Fig. 1 is the schematic diagram of the process chart of the present invention.
Wherein:1- cyclone hydraulic separators, 2- salkali waste evaporating columns, 3- lobed rotor compressors, 4- evaporators, 5- circulating pumps
Embodiment
The present invention will be further described with reference to the accompanying drawings and examples, but the present invention is not limited to following embodiments.
Embodiment 1
10t/h cyclohexanone saponification waste lye (solids content 30%) enters salkali waste evaporating column 2 by pressure difference, Evaporated in salkali waste evaporating column 2,95-100 DEG C of evaporation gas phase passes through the rotary filter press of cyclone hydraulic separators 1, and then gas phase enters sieve Recompressed in thatch compressor 3, the exit gas phase temperature of lobed rotor compressor 3 is 105-115 DEG C, and compression gas phase is re-used as thermal source Carry out cyclohexanone saponification waste lye in heating evaporation salkali waste evaporating column 2, compression gas phase is condensed into liquid in circulating pump 4.
The amount of liquid discharged from cyclone hydraulic separators 1 and circulating pump 4 is 4t/h, and the power consumption of lobed rotor compressor 3 is 350Kw/h, The solids content of cyclohexanone saponification waste lye after concentration is 50%.
The embodiment of the present invention is described above in association with accompanying drawing, but these explanations can not be considered as limiting this The scope of invention, protection scope of the present invention are limited by appended claims, any on the basis of the claims Change is all protection scope of the present invention.

Claims (10)

  1. A kind of 1. concentration technology of cyclohexanone saponification waste lye, it is characterised in that the saponification after oxidizing cyclohexanone decomposition process Spent lye enters salkali waste evaporating column, and gained evaporation gas phase evaporates the foam removal of column overhead demister through salkali waste after evaporation and cyclone hydraulic separators separates Enter compressor compresses afterwards, gained compression gas phase exchanges heat with the saponification waste lye of evaporator shell side and tube side after compression, compresses gas phase Liquid phase after cooling is discharged into water treatment system as lime set, the water in saponification waste lye vaporized after being heated obtained water evaporation gas phase from The tower top discharge of salkali waste evaporating column.
  2. 2. technique according to claim 1, it is characterised in that in salkali waste evaporating column tower reactor with being set on pump inlet pipeline Ultrasonic cleaner.
  3. 3. technique according to claim 1, it is characterised in that the salkali waste evaporating column tower reactor liquid phase is between evaporator and tower reactor With circulating pump forced circulation.
  4. 4. according to any one of the claim 1-3 techniques, it is characterised in that the salkali waste evaporating column is tower structure, demister Salkali waste evaporating column top is arranged on, the cyclone hydraulic separators is arranged on top gaseous phase pipeline, for carrying out gas-liquid phase separation.
  5. 5. technique according to claim 1, it is characterised in that compressor used is that compression ratio is less than 2.
  6. 6. according to the technique of claim 1 or 5, it is characterised in that compressor used is lobed rotor compressor, centrifugal compressor One kind in machine or air blower.
  7. 7. according to any one of the claim 1-3 techniques, it is characterised in that the salkali waste evaporation column overhead temperatures are 95-100 DEG C.
  8. 8. according to any one of the claim 1-3 techniques, it is characterised in that the salkali waste evaporating column bottom temperature is 95-105 DEG C.
  9. 9. according to any one of claim 1-3 or 5 techniques, it is characterised in that the compressor exit temperature is 105-115 DEG C.
  10. 10. according to any one of the claim 1-3 techniques, it is characterised in that evaporation gas phase is discharged from the tower top of salkali waste evaporating column Afterwards in the saponification waste lye after remaining concentration, solids content 50-60%.
CN201610439353.0A 2016-06-17 2016-06-17 A kind of concentration technology of cyclohexanone saponification waste lye Pending CN107512751A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610439353.0A CN107512751A (en) 2016-06-17 2016-06-17 A kind of concentration technology of cyclohexanone saponification waste lye

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610439353.0A CN107512751A (en) 2016-06-17 2016-06-17 A kind of concentration technology of cyclohexanone saponification waste lye

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CN107512751A true CN107512751A (en) 2017-12-26

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110759406A (en) * 2019-12-06 2020-02-07 岳阳才益精细化工有限公司 High-temperature concentration device for saponified waste alkali liquor

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007033443A1 (en) * 2005-09-22 2007-03-29 Vlaamse Instelling Voor Technologisch Onderzoek N.V. (Vito) Installation for the treatment of liquid
WO2010112673A1 (en) * 2009-03-31 2010-10-07 Hsp Engineering Ab Oy A method for thermal concentration of a fluid
CN102923895A (en) * 2012-11-07 2013-02-13 江苏迈克化工机械有限公司 Method for disposing cyclohexanone saponified waste liquid
CN103585773A (en) * 2013-06-07 2014-02-19 佛山汉维科技有限公司 Vacuum agitation type energy-saving evaporation device
CN204380287U (en) * 2014-12-31 2015-06-10 山东圣琪生物有限公司 A kind of MVR evaporimeter

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007033443A1 (en) * 2005-09-22 2007-03-29 Vlaamse Instelling Voor Technologisch Onderzoek N.V. (Vito) Installation for the treatment of liquid
WO2010112673A1 (en) * 2009-03-31 2010-10-07 Hsp Engineering Ab Oy A method for thermal concentration of a fluid
CN102923895A (en) * 2012-11-07 2013-02-13 江苏迈克化工机械有限公司 Method for disposing cyclohexanone saponified waste liquid
CN103585773A (en) * 2013-06-07 2014-02-19 佛山汉维科技有限公司 Vacuum agitation type energy-saving evaporation device
CN204380287U (en) * 2014-12-31 2015-06-10 山东圣琪生物有限公司 A kind of MVR evaporimeter

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110759406A (en) * 2019-12-06 2020-02-07 岳阳才益精细化工有限公司 High-temperature concentration device for saponified waste alkali liquor

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Application publication date: 20171226