CN110156556A - A kind of coating solvent slop withdrawal technique - Google Patents

A kind of coating solvent slop withdrawal technique Download PDF

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Publication number
CN110156556A
CN110156556A CN201910475510.7A CN201910475510A CN110156556A CN 110156556 A CN110156556 A CN 110156556A CN 201910475510 A CN201910475510 A CN 201910475510A CN 110156556 A CN110156556 A CN 110156556A
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CN
China
Prior art keywords
toluene
technique
dimethylbenzene
solvent slop
coating
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CN201910475510.7A
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Chinese (zh)
Inventor
左姣
林辉荣
毛小英
阳杨
何睿明
陈国平
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XINZHONGTIAN ENVIRONMENTAL PROTECTION Co Ltd
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XINZHONGTIAN ENVIRONMENTAL PROTECTION Co Ltd
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Priority to CN201910475510.7A priority Critical patent/CN110156556A/en
Publication of CN110156556A publication Critical patent/CN110156556A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/58Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/10Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a kind of techniques of recycling design from coating solvent slop, the recycling design is toluene, butyl acetate and/or dimethylbenzene, the technique is extracted by extractant of desalted water, to remove ethyl alcohol, isopropanol, water and water-soluble resin, then it cleaned, take off light component, toluene rectifying and xylene distillation processing, recycling obtains the toluene, butyl acetate and/or dimethylbenzene for meeting GB standard, the technique is by coating waste recycled solvent, not only mitigate the environmental protection pressure of Chan Fei enterprise, while can also generate economic benefit.

Description

A kind of coating solvent slop withdrawal technique
Technical field
The invention belongs to field of environment engineering technology, a kind of specific coating solvent slop withdrawal technique.
Background technique
Modern times industry rapid development, anticorrosion with painting technology are also widely applied therewith, such as the spray of vehicle spray painting, steel construction Anticorrosion with painting technology is widely applied in painting, component of machine spraying etc..It is a large amount of to generate painting while anticorrosion with painting technology is widely applied Solvent slop is filled, based on the complexity of coating solvent slop, there are no perfect techniques to carry out returning for coating solvent slop currently on the market It receives and utilizes.
According to the market survey to coating solvent slop, selection has representative automobile industry coating solvent slop and is ground Study carefully, the composition of painting dressing automobiles solvent slop see the table below 1 at present:
1 automobile industry coating solvent slop of table composition
Note: this table information is obtained according to certain painting dressing automobiles solvent enterprise's sampling analysis.
Due to coating solvent slop contain a large amount of resin-oatmeal and other its film forming of guarantee, adhesion strength and add.Greatly Molecular organic causes coating waste solvent viscosity bigger, and simple recovery process and equipment cannot achieve high viscosity coating waste The recycling of solvent
Since coating waste solvent composition is complicated and recovery difficult is larger, coating solvent slop is mainly treated as hazardous waste at present Incineration disposal is carried out, not only causes the waste of valuable solvent resource, while increasing dangerous waste incineration disposal difficulty and incineration tail gas The difficulty of processing.
Present invention aims at a large amount of coating solvent slop efficient resource utilizations are solved, environmental protection is carried out for Chan Fei enterprise and is subtracted Pressure is not only reduced because burning the air pollution generated, can also obtain economic benefit because recycling.
Summary of the invention
The purpose of the present invention is to provide a kind of technique of recycling design from coating solvent slop, the solvent contains first Benzene, butyl acetate and/or dimethylbenzene pass through the stable operation of a whole set of continuous processing, separating-purifying coating solvent, respectively by content Higher and better economy toluene, butyl acetate, dimethylbenzene are recycled, and the quality for recycling product meets GB standard.
On the one hand, the technique of a kind of recycling design from coating solvent slop of the invention, the recycling design are toluene, second Acid butyl ester and/or dimethylbenzene, comprising the following steps:
(1) extraction is using desalted water as extractant, by ethyl alcohol, isopropanol, water and the water-soluble resin in coating solvent slop Extraction removes;
(2) removing impurities collects wiped film vaporization by the way that the solvent slop for removing water and resin is sloughed impurity by luwa evaporator Device top gas phase material;
(3) take off light component and the gaseous phase materials of collection entered into lightness-removing column, by boiling point lower than toluene boiling point substance all from Tower top abjection enters light component return tank after heat exchange condensation, and by reflux, extraction light component goes to burn as spent organic solvent Disposition;
(4) upper step is deviate from the coating waste solvent after light component and is pumped into toluene rectifying column by toluene rectifying, by toluene from tower Top abjection, enters refluxing toluene tank after heat exchange condensation, controls regurgitant volume and produced quantity by reflux ratio, produces toluene product;
(5) solvent slop after deviating from toluene is pumped into xylene distillation tower by xylene distillation, by butyl acetate from tower top Abjection enters butyl ester return tank after heat exchange condensation, controls regurgitant volume and produced quantity by reflux ratio, extraction butyl acetate produces Product leave as dimethylbenzene.
The technique of aforementioned present invention, it is preferred that step it is poly- 1) in, the volume flow ratio of desalted water and coating solvent slop controls In 1:4;Walk it is poly- 2) described in removal of impurities, including by coating solvent slop extracted and lightness-removing column top gaseous phase heat exchange after, enter Luwa evaporator is all deviate from the substance that boiling point is less than or equal to dimethylbenzene, boiling in a manner of gas phase from luwa evaporator top The substance and solid impurity that point is higher than dimethylbenzene are disposed, control knifing is steamed from luwa evaporator bottom discharge system as dangerous waste Device gaseous phase outlet temperature is sent out at 150 DEG C or so;In step 3), lightness-removing column uses vertical siphon reboiler, is saturated and is steamed using 6Bar Vapour is as reboiler heat source.6, technique as described in claim 1, step 3), 4) reflux ratio, 5) are 1.5-2;Step It 5) further comprise being adopted after the dimethylbenzene that will be left behind is delivered to the cooling of dimethylbenzene cooler by pump as xylene product in Out.
In one embodiment, the technique of a kind of recycling design from coating solvent slop of the invention, specifically includes Following procedure:
(1) it extracts
Using desalted water as extractant, by ethyl alcohol, isopropanol, water and the water-soluble resin extraction in coating solvent slop Out, by practical operation, the volume flow ratio of desalted water and coating solvent slop is controlled in 1:4;
(2) removing impurities
It is larger between coating solvent slop amount containing solid impurity, contain the high boiling organic matter in part simultaneously, therefore, using scraping Film evaporator removing impurities, concrete operations are as follows:
Coating solvent slop extracted lightness-removing column top gaseous phase heat exchange after, preheated device by its waste heat to 90 DEG C, then Into luwa evaporator, the substance that boiling point is less than or equal to dimethylbenzene is all taken off in a manner of gas phase from luwa evaporator top Out, the substance and solid impurity that boiling point is higher than dimethylbenzene are disposed from luwa evaporator bottom discharge system as dangerous waste, wherein Luwa evaporator, as heat source, controls luwa evaporator gaseous phase outlet temperature at 150 DEG C or so using 6Bar saturated vapor;
(3) light component is taken off
The gaseous phase materials that luwa evaporator top takes off are sent into lightness-removing column, and boiling point is whole lower than the substance of toluene boiling point Deviate from from tower top, enters light component return tank after heat exchange condensation, pass through reflux ratio control (preferably 1.5) regurgitant volume processed and extraction Amount produces light component as spent organic solvent and removes incineration disposal, wherein lightness-removing column uses vertical siphon reboiler, using 6Bar Saturated vapor is as reboiler heat source.
(4) toluene rectifying
Coating waste solvent after lightness-removing column deviates from light component is pumped into toluene rectifying column, toluene is deviate from from tower top, warp Enter refluxing toluene tank after heat exchange condensation, control regurgitant volume and produced quantity by reflux ratio (preferably 2), produce toluene product, In, toluene rectifying uses vertical siphon reboiler, using 6Bar saturated vapor as reboiler heat source;
(5) xylene distillation
Coating waste solvent after toluene rectifying column deviates from toluene is pumped into xylene distillation tower, by butyl acetate from tower top Abjection, enters butyl ester return tank after heat exchange condensation, controls regurgitant volume and produced quantity by reflux ratio (preferably 1.5), produces second Acid butyl ester product.
Tower reactor is the dimethylbenzene for meeting GB quality requirement after deviating from butyl acetate, and it is cold to be delivered to dimethylbenzene cooler by pump But it is produced afterwards as xylene product, wherein xylene distillation uses vertical siphon reboiler, using 6Bar saturated vapor conduct Reboiler heat source.
Advantage of the invention:
1, this technique is suitable for the separation of highly viscous coating solvent slop;
2, this technique is by the content in coating solvent slop is higher and the toluene of better economy, butyl acetate, dimethylbenzene point It is not recycled, by coating solvent slop maximum resource;
3, toluene, butyl acetate, the dimethylbenzene of this technique recycling are all satisfied the target level of product quality of GB, and product has and city The ability that field integrates with;
4, the toluene in coating solvent slop, butyl acetate, the dimethylbenzene rate of recovery reach 95% or more.
Detailed description of the invention
Fig. 1 coating waste solvent recovery process flow diagram.
Specific embodiment
Following embodiment does not limit this hair for furtheing elucidate and understanding Spirit Essence of the invention in any way Bright range.
Embodiment 1
Recovery process process is shown in Fig. 1, wherein
P1- feed pump;P2- dehydrogenation reflux pump;P3- dehydrogenation discharging pump;P4- refluxing toluene pump;P5- discharging pump;P6- butyl ester Reflux pump;P7- dimethylbenzene discharging pump;T1- extraction tower;T2- lightness-removing column;T3- toluene tower;T4- benzenol hydrorefining;E1- evaporator; E2- preheater;E3- dehydrogenation reboiler;E4- dehydrogenation condenser;E5- dehydrogenation cooler;E6- toluene reboiler;The condensation of E7- toluene Device;E8- dimethylbenzene reboiler;E9- diformazan benzene condenser;E10- dimethylbenzene cooler;V1- light component return tank;V2- toluene returns Flow tank;V3- butyl ester return tank.
Specific steps are as follows:
(1) it extracts
Using desalted water as extractant, by ethyl alcohol, isopropanol, water and the water-soluble resin extraction in coating solvent slop Out, by practical operation, the volume flow ratio of desalted water and coating solvent slop is controlled in 1:4.
(2) removing impurities
It is larger between coating solvent slop amount containing solid impurity, contain the high boiling organic matter in part simultaneously, this technique uses Luwa evaporator removing impurities, concrete operations are as follows:
Coating solvent slop extracted and lightness-removing column top gaseous phase heat exchange after, preheated device by its waste heat to 90 DEG C, then Into luwa evaporator, the substance that boiling point is less than or equal to dimethylbenzene is all taken off in a manner of gas phase from luwa evaporator top Out, the substance and solid impurity that boiling point is higher than dimethylbenzene are disposed from luwa evaporator bottom discharge system as dangerous waste.Knifing steams Device is sent out using 6Bar saturated vapor as heat source, controls luwa evaporator gaseous phase outlet temperature at 150 DEG C or so.
(3) light component is taken off
The gaseous phase materials that luwa evaporator comes out enter lightness-removing column, and the substance by boiling point lower than toluene boiling point is all from tower top Abjection, enters light component return tank after heat exchange condensation, controls regurgitant volume and produced quantity by reflux ratio 1.5, produces light component Incineration disposal is removed as spent organic solvent.
Lightness-removing column uses vertical siphon reboiler, using 6Bar saturated vapor as reboiler heat source.
(4) toluene rectifying
Coating waste solvent after lightness-removing column deviates from light component is pumped into toluene rectifying column, toluene is deviate from from tower top, warp Enter refluxing toluene tank after heat exchange condensation, regurgitant volume and produced quantity are controlled by reflux ratio 2, produce toluene product.
Toluene rectifying uses vertical siphon reboiler, using 6Bar saturated vapor as reboiler heat source.
(5) xylene distillation
Coating waste solvent after toluene rectifying column deviates from toluene is pumped into xylene distillation tower, by butyl acetate from tower top Abjection, enters butyl ester return tank after heat exchange condensation, controls regurgitant volume and produced quantity by reflux ratio 1.5, produces butyl acetate Product.
Tower reactor is the dimethylbenzene for meeting quality requirement after deviating from butyl acetate, and it is cooling to be delivered to dimethylbenzene cooler by pump It is produced afterwards as xylene product.
Xylene distillation uses vertical siphon reboiler, using 6Bar saturated vapor as reboiler heat source.
The above technique of the invention, toluene, butyl acetate, dimethylbenzene the rate of recovery reach 95% or more.Recycle product Quality, be up to state standards GB: toluene purity 99.5%GB/T2284-2009, butyl acetate purity 99%GB/T 3729- 2007, dimethylbenzene purity 99.5%GB/T 3407-2010.

Claims (8)

1. a kind of technique of the recycling design from coating solvent slop, the recycling design is toluene, butyl acetate and/or diformazan Benzene, comprising the following steps:
(1) extraction using desalted water as extractant, by coating solvent slop water and water-soluble resin extraction remove;
(2) removing impurities collects luwa evaporator top by the way that the solvent slop for removing water and resin is sloughed impurity by luwa evaporator Portion's gaseous phase materials;
(3) it takes off light component and the gaseous phase materials of collection is entered into lightness-removing column, the substance by boiling point lower than toluene boiling point is all from tower top Abjection, enters light component return tank, partial reflux after heat exchange condensation, and extraction light component is gone at burning as spent organic solvent It sets;
(4) the coating waste solvent after upper step abjection light component is pumped into toluene rectifying column by toluene rectifying, and toluene is taken off from tower top Out, enter refluxing toluene tank after heat exchange condensation, regurgitant volume and produced quantity are controlled by reflux ratio, produce toluene product;
(5) solvent slop after deviating from toluene is pumped into xylene distillation tower by xylene distillation, and butyl acetate is deviate from from tower top, Enter butyl ester return tank after heat exchange condensation, regurgitant volume and produced quantity are controlled by reflux ratio, butyl acetate product is produced, leaves As dimethylbenzene.
2. technique as described in claim 1, walk it is poly- 1) in, the volume flow ratio of desalted water and coating solvent slop is controlled 1: 8。
3. technique as described in claim 1, walk it is poly- 2) described in removal of impurities, including by coating solvent slop extracted and de- light After the heat exchange of column overhead gas phase, into luwa evaporator, by boiling point be less than or equal to the substance of dimethylbenzene all in a manner of gas phase from The abjection of luwa evaporator top, the substance and solid impurity that boiling point is higher than dimethylbenzene are made from luwa evaporator bottom discharge system For dangerous waste disposition.
4. technique as claimed in claim 3 controls luwa evaporator gaseous phase outlet temperature at 150 DEG C or so.
5. technique as described in claim 1, in step 3), lightness-removing column uses vertical siphon reboiler, is saturated and is steamed using 6Bar Vapour is as reboiler heat source.
6. technique as described in claim 1, step 3), 4) reflux ratio, 5) are 1.5-2.
It further comprise that the dimethylbenzene that will be left behind is delivered to diformazan by pump in step 5) 7. technique as described in claim 1 It is produced after benzene cooler is cooling as xylene product.
8. technique as described in claim 1, removing substance by extractant in step 1) further includes ethyl alcohol and isopropanol.
CN201910475510.7A 2019-06-03 2019-06-03 A kind of coating solvent slop withdrawal technique Pending CN110156556A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110483296A (en) * 2019-09-12 2019-11-22 新中天环保股份有限公司 A kind of recovery method of pharmacy class ethyl acetate solvent slop
CN110483230A (en) * 2019-09-12 2019-11-22 新中天环保股份有限公司 A method of recycling toluene from pharmacy class toluene solvent slop
CN113214061A (en) * 2021-05-27 2021-08-06 新中天环保股份有限公司 Process for recovering butanone from waste solvent in adhesive industry

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110483296A (en) * 2019-09-12 2019-11-22 新中天环保股份有限公司 A kind of recovery method of pharmacy class ethyl acetate solvent slop
CN110483230A (en) * 2019-09-12 2019-11-22 新中天环保股份有限公司 A method of recycling toluene from pharmacy class toluene solvent slop
CN113214061A (en) * 2021-05-27 2021-08-06 新中天环保股份有限公司 Process for recovering butanone from waste solvent in adhesive industry

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