CN108971200A - Rectifying, evaporated mother liquor and residue treatment process - Google Patents
Rectifying, evaporated mother liquor and residue treatment process Download PDFInfo
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- CN108971200A CN108971200A CN201810855459.8A CN201810855459A CN108971200A CN 108971200 A CN108971200 A CN 108971200A CN 201810855459 A CN201810855459 A CN 201810855459A CN 108971200 A CN108971200 A CN 108971200A
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- salt
- mother liquor
- residue
- cracking
- rectifying
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 102
- 238000010025 steaming Methods 0.000 claims abstract description 9
- 238000005336 cracking Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 20
- 239000005416 organic matter Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000003795 desorption Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 238000012962 cracking technique Methods 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000000706 filtrate Substances 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000004821 distillation Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000010815 organic waste Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002594 sorbent Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to dangerous waste process fields, and in particular to rectifying, evaporated mother liquor and residue treatment process, the treatment process of creative use plus salt absorption effectively solves the handling problems that smart (steaming) evaporates mother liquor and residue in conjunction with purified salt technique in the present invention.
Description
Technical field
The invention belongs to dangerous waste process fields, and in particular to rectifying, evaporated mother liquor and residue treatment process.
Background technique
Rectifying is to utilize a kind of separation process that each component volatility in mixture is different and is separated each component.Essence
It evaporates and is carried out usually in rectifying column, gas-liquid two-phase carries out interphase heat transfer mass transfer by counter current contacting.Volatile components in liquid phase
Into gas phase, the difficult volatile component in gas phase is transferred to liquid phase, almost pure volatile components then can be obtained in tower top, tower bottom can
Obtain almost pure difficult volatile component.
Distillation is a kind of thermodynamic (al) separating technology, it is different using each component boiling point in mixing liquid or liquid-solid system,
Low boiling component is evaporated, then is condensed to separate the unit process of entire component, is two kinds of unit operations of evaporation and condensation
Joint.By the way that liquid to be heated to boiling in distillation process, so that liquid is become steam, be condensed into steam cooling again
Liquid can also separate the different liquid mixture of boiling point so that volatile and not volatile substance be separated.
Rectifying mother liquor or evaporated mother liquor are inevitably generated during rectifying and distillation.In general, smart
(steaming) evaporates mother liquor and residue is the liquid or jelly of higher boiling, high organic concentrations, and COD is generally in 10000mg/L or more, because of it
The technique of generation is different, property and forms also different, generally can be divided into saliferous and salt-free.Smart (steaming) evaporate mother liquor and
Residue is a kind of hazardous waste for being put into National Hazard waste register, and such hazardous waste derives from chemical industry, medicine, agriculture extensively
The fields such as medicine, printing and dyeing, yield is big, and cost of disposal is high, it has also become how the bottleneck of enterprise development effectively handles such danger
Waste has become very urgent.
It is using works such as burning, landfills for the processing method of rectifying mother liquor or evaporated mother liquor in currently available technology
Skill, but these method Disposal Conditions are harsh, it is with high costs, it can not efficiently and effectively solve rectifying in industrial applications, distillation
The handling problems of mother liquor and residue.
Summary of the invention
How the technical problem to be solved by the present invention is to be effectively reduced rectifying mother liquor, evaporated mother liquor and distillation and essence
The processing cost of residue is generated during evaporating, with simpler process flow, inexpensive mode realizes rectifying mother liquor, distillation
The processing of waste residue in mother liquor and distillation and rectifying.
In order to realize the purpose, the invention discloses the treatment process of rectifying, evaporated mother liquor and residue, including following step
It is rapid:
(1): essence (steaming) being evaporated into mother liquor and residue by pretreatment, obtains the feed liquid with certain fluidity；
(2): the feed liquid that step (1) obtains by pump is transported to stirred tank, in mass ratio 1:(1~5) ratio be added salt, sufficiently
Slurry is separated by centrifuge after stirring, obtains the crude salt of adsorption organic matter, and the solution thrown away；
(3): the solution of step (2) is back to reuse in rapid (1)；
(4): the crude salt of step (2) being entered into pyrolysis furnace and is cracked, using the continuous cracking technique of high-temperature low-oxygen, cracking temperature
Control obtains cracking salt at 100~600 DEG C.
Wherein pretreatment described in step (1), which refers to, carries out rectifying or evaporated mother liquor or residue at dissolution
Reason, and after removing oil removal, obtain the feed liquid with certain fluidity.When needed, adjusting that pH is carried out to it, is adjusted to
Property.
Preferably, the salt is water soluble salt.
It is further preferred that the salt is hydrochloride, sulfate, one of phosphate.According to institute's saliferous in raw material
Type, selection are added a kind of identical salt, and not saliferous in raw material then may be optionally added any one salt, it is generally preferable to sodium chloride.
In another preferred technical solution, the cracking salt direct reuse that step (4) is obtained into step (2), and/or
By purified salt technique, the purified salt for meeting target level of product quality is obtained.
It here is mainly to consider in step (2) plus when salt treatment for the demand of salt amount.For example, for the essence of saliferous
(steaming) evaporates mother liquor and residue, due to itself saliferous, will necessarily generate in step (4) and be greater than processing requirement
Salt, therefore industrial salt product will be used as by purified salt technique after a part of salt refining.And salt-free smart (steaming) is evaporated
For mother liquor and residue, the salt amount generated in step (4) is substantially equal to salt amount required for handling in step (2), theoretically not
Purified salt out is needed, salt whole circulating and recovering is cracked.
It is further preferred that the preparation process of purified salt is also disclosed in the present invention are as follows: (5) cracking salt dissolved, filtered,
Removing impurities by oxidation, secondary crystallization, thermal desorption obtain the purified salt for meeting target level of product quality.
It should be noted that in the present invention, still needing to be able to maintain mixture after salt stirring is added to feed liquid in step (2)
Mobility, it is preferred that after centrifugation, feed liquid decrement 30~70%.
The discovery salt of the present inventor's creativeness, especially water soluble salt is at rectifying, evaporated mother liquor and residue
Tool has an unexpected effect during reason.By the way that salt is added into mother liquor, waste residue, so that it may inexpensive, efficient to essence
The mother liquor and residue evaporate, generated in distillation process is handled.Salt has meaning during rectifying, evaporated mother liquor and residue treatment
Unimaginable advantage:
1. the suction-operated of salt: smart (steaming) evaporates mother liquor and residue is that high concentrated organic waste liquid is transformed into and contains after adding salt to adsorb
The salt type solid substance of organic matter evaporates essence (steaming) disposition of mother liquor and residue, is transformed into from the disposition to waste liquid useless to solid-state
The disposition of salt.
2. the heat transfer of salt, catalytic action: the crude salt after absorption organic matter carries out continuous high temperature cracking, salt in pyrolysis furnace
As heat transfer carrier, it is heated evenly material in furnace, and because the specific surface of salt particle is larger, so as to promote to be adsorbed on salt table
The cracking of face organic matter.
3. the circulating and recovering of salt: continuous high temperature cracking can be such that most of organic cracking on salt surface removes, resulting to split
It is very low to solve salt content of organics, secondary pollution can not be generated directly as sorbent circulation reuse.
4. continuous high temperature cracking technology: using high-temperature low-oxygen flue gas, cracked, improved organic by the heating of multistage temperature control
The lysis efficiency of object, and can effectively control the generation of dioxin.
5. purified salt technique: for saliferous in raw material, need to discharge in entire technique, gained cracking after Pintsch process
A part of salt, by dissolution filter, removing impurities by oxidation, secondary crystallization obtains meeting product matter after the purified salts process such as thermal desorption
The product salt of amount standard.
Specific embodiment
In order to better understand the present invention, we in conjunction with specific embodiments further explain the present invention below
It states.
Embodiment 1
Rectifying mother liquor in this embodiment comes from certain insecticide factory, is the organic waste liquor of salt-free high concentration.It is highly concentrated for this
Organic waste liquor is spent to be handled.
Processing step includes:
(1): taking 100ml rectifying mother liquor, 150g sodium chloride salt is added, is sufficiently stirred, filter, obtain crude salt and filtrate；
(2): crude salt Pintsch process, must cracking salt, (after TOC detection, needing to configure according to salt treatment and forming concentration is 300g/L's
Solution)；
(3): being that filtrate and a certain amount of former rectifying mother liquor for the 45ml for obtaining step (1) are mixed specifically by filtrate recycle
It closes, obtains 100ml feed liquid, then add cracking salt 186g, stir, filtering obtains crude salt, filtrate；
(4): crude salt Pintsch process, must cracking salt, (after TOC detection, needing to configure according to salt treatment and forming concentration is 300g/L's
Solution)；
It (5) is that filtrate and a certain amount of former rectifying mother liquor for the 42ml for obtaining step (4) are mixed specifically by filtrate recycle
It closes, obtains 100ml feed liquid, then add cracking salt 187g, stir, filtering obtains crude salt, filtrate；Salt filtrate recycle will be cracked,
Specifically, it is the Pintsch process salting liquid of 45ml to be added to the former rectifying mother liquor of 55ml, then adds new cracking salt
186g is stirred, and filtering obtains crude salt, filtrate；
(6): crude salt Pintsch process, must cracking salt, (after TOC detection, needing to configure according to salt treatment and forming concentration is 300g/L's
Solution)；
……
Constantly repeat step (3) and (4)
Experimental procedure and treatment effect are shown in Table 1:
Table 1:
Content of organics is very high in original nut liquid it can be seen from the data in table 1, after adding salt absorption centrifuge separation, obtains surface
The salt type solid substance for having adsorbed organic matter, after high-temperature low-oxygen technique continuous cracking, the organic matter on salt surface is most of
It cracks, content of organics is very low in cracking salt, uses in systems as sorbent circulation, does not generate secondary pollution.
Embodiment 2
Rectification residue in the present embodiment comes from certain pharmaceutical factory, for the highly concentrated debirs containing 10% or so sodium chloride.The rectifying is residual
The original shape of slag is jelly, does not have mobility.
Processing step includes:
(1): rectification residue is diluted with water by 1:2, obtains flowable slurry；Take 500g rectification residue that 1000ml water, stirring is added
Dissolution adds the absorption of 2000g sodium chloride, stirs evenly；
(2): being centrifugated to obtain crude salt and filtrate；
(3): crude salt Pintsch process, after obtaining the cracking salt 1720g(TOC detection of removal most organic, according to salt treatment
Need to configure the solution to form that concentration is 300g/L)；Crack a part of reuse of salt, a part purification
(4) it by step (2) filtrate recycle, specifically, then takes 300g rectification residue that 600ml water is added and step (3) filtrate is added
680ml, stirring and dissolving add the cracking salt absorption that 1650g step 3 obtains, stir evenly；
(5) crude salt and filtrate are centrifugated to obtain
……
It constantly repeats step (3) and arrives (5)
It is the rectification residue containing 10% or so sodium chloride from certain pharmaceutical factory by rectification residue in this present embodiment, it is therefore, high
The yield of anneal crack solution salt can be continuously increased, we increase a purified salt technique in the present embodiment, specifically include following step
It is rapid:
(1) cracking salt 70g obtained by step 1 is dissolved in 300ml water, filters；
(2) filtrate carries out the clear solution after heterogeneous oxidation impurity removal process；
(3) thermal desorption obtains purified salt；
(4) purified salt detection (300g/L).
Experimental procedure and treatment effect are shown in Table 2:
Table 2
The saliferous and content of organics is very high in former rectification residue it can be seen from the data in table 2, and do not have mobility, add
After water dissolved dilution, the slurry of certain fluidity is obtained, after sodium chloride salt absorption centrifugation is added, is obtained containing the thick of organic matter
Salt, after high-temperature low-oxygen technique continuous cracking, the organic matter on salt surface is largely cracked, and has cracked in salt content of organics
It is material in balance system because of saliferous in former rectification residue through very low, needs a part cracking salt carrying out purification discharging, obtain
Product salt is refined, from experimental data, it can be seen that gained purified salt meets chlor-alkali industry salt standard.The cracking salt of another part exists
It is used in system as sorbent circulation, does not generate secondary pollution.
The foregoing is a specific embodiment of the present invention.It should be pointed out that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (5)
1. the treatment process of rectifying, evaporated mother liquor and residue, it is characterised in that: the following steps are included:
(1): essence (steaming) being evaporated into mother liquor and residue by pretreatment, obtains the feed liquid with certain fluidity；
(2): the feed liquid that step (1) obtains by pump is transported to stirred tank, in mass ratio 1:(1~5) ratio be added salt, sufficiently
Slurry is separated by centrifuge after stirring, obtains the crude salt of adsorption organic matter, and the solution thrown away；
(3): the solution of step (2) is back to reuse in rapid (1)；
(4): the crude salt of step (2) being entered into pyrolysis furnace and is cracked, using the continuous cracking technique of high-temperature low-oxygen, cracking temperature
Control obtains cracking salt at 100~600 DEG C.
2. the treatment process of rectifying according to claim 1, evaporated mother liquor and residue, it is characterised in that: the salt is water
Soluble.
3. the treatment process of rectifying according to claim 2, evaporated mother liquor and residue, it is characterised in that: the salt is salt
Hydrochlorate, sulfate, one of phosphate.
4. the treatment process of rectifying according to claim 1, evaporated mother liquor and residue, it is characterised in that: obtain step (4)
The cracking salt direct reuse arrived obtains the purification for meeting target level of product quality into step (2), and/or through purified salt technique
Salt.
5. the treatment process of rectifying according to claim 1, evaporated mother liquor and residue, which is characterized in that further include purification
The preparation process of salt:
(5) cracking salt is dissolved, is filtered, removing impurities by oxidation, secondary crystallization, thermal desorption obtains the purification for meeting target level of product quality
Salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810855459.8A CN108971200A (en) | 2018-07-31 | 2018-07-31 | Rectifying, evaporated mother liquor and residue treatment process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810855459.8A CN108971200A (en) | 2018-07-31 | 2018-07-31 | Rectifying, evaporated mother liquor and residue treatment process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108971200A true CN108971200A (en) | 2018-12-11 |
Family
ID=64552303
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810855459.8A Pending CN108971200A (en) | 2018-07-31 | 2018-07-31 | Rectifying, evaporated mother liquor and residue treatment process |
Country Status (1)
| Country | Link |
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| CN (1) | CN108971200A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607570A (en) * | 2018-12-30 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of recycling treatment process of ammonium chloride abraum salt |
| CN109607571A (en) * | 2018-12-31 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of disposal of resources technique of highly concentrated organic spent lye |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106424078A (en) * | 2016-09-26 | 2017-02-22 | 克雷伯氏环保科技（苏州）有限公司 | Refining method for salt containing organic matters |
| CN107903942A (en) * | 2017-12-27 | 2018-04-13 | 洛阳昊海工贸有限公司 | A kind of disposing technique of liquid state rectification residue |
-
2018
- 2018-07-31 CN CN201810855459.8A patent/CN108971200A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106424078A (en) * | 2016-09-26 | 2017-02-22 | 克雷伯氏环保科技（苏州）有限公司 | Refining method for salt containing organic matters |
| CN107903942A (en) * | 2017-12-27 | 2018-04-13 | 洛阳昊海工贸有限公司 | A kind of disposing technique of liquid state rectification residue |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607570A (en) * | 2018-12-30 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of recycling treatment process of ammonium chloride abraum salt |
| CN109607571A (en) * | 2018-12-31 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of disposal of resources technique of highly concentrated organic spent lye |
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Application publication date: 20181211 Assignee: Yancheng Guotou Environmental Technology Co.,Ltd. Assignor: NANJING GREEN-WATER ENVIRONMENT ENGINEERING LIMITED BY SHARE Ltd. Contract record no.: X2021980001429 Denomination of invention: Treatment process of distillation, mother liquor and residue License type: Exclusive License Record date: 20210304 |
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Application publication date: 20181211 |