CN100348512C - Technique for reclaiming ethylene alkali-washing waste liquid - Google Patents
Technique for reclaiming ethylene alkali-washing waste liquid Download PDFInfo
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- CN100348512C CN100348512C CNB2005101221854A CN200510122185A CN100348512C CN 100348512 C CN100348512 C CN 100348512C CN B2005101221854 A CNB2005101221854 A CN B2005101221854A CN 200510122185 A CN200510122185 A CN 200510122185A CN 100348512 C CN100348512 C CN 100348512C
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- alkali
- waste liquid
- alkali lye
- washing waste
- causticization
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Abstract
The present invention relates to a technology for reclaiming ethylene alkali-washing waste liquid, which comprises the following operation steps: oil removal, causticization, desulphurization, etc., are carried out in waste alkali liquid and in the operation steps, substances, such as a load carrying solid flocculating agent, metal oxide, etc., are successively added. The present invention has the advantages of simple technological process and obvious oil removing effect, and obtained regeneration alkali liquid completely conforms to the technological requirements of an ethylene alkali-washing process. S<2-> of side products obtained by the processes of the causticization and the desulphurization is converted into sulfide with a high added value by a sulfide conversion method, and the sulfide can be all used as commodities and can be sold. The present invention simplifies the treating process of the waste alkali liquid and also brings high economic benefit to the treatment of the waste alkali liquid.
Description
Technical field
The invention belongs to light industry, chemical waste liquid improvement field, particularly a kind of technique for reclaiming ethylene alkali-washing waste liquid.
Background technology
In ethylene production, splitting gas need be with the NaOH solution washing of high density to remove CO wherein
2, H
2Sour gas such as S.The remaining NaOH solution of alkaline cleaning procedure except that containing remaining NaOH, also contains the Na that generates as discharging of waste liquid in this class alkali-washing waste liquid in alkaline cleaning procedure
2CO
3, Na
2The sodium salt and the neutral oils of inorganic salts such as S and a small amount of organism such as mercaptan, thioether, phenols and naphthenic acid etc.The processing of this class alkali-washing waste liquid is the difficult problem of ethylene production always.
Na in the alkali-washing waste liquid
2CO
3, Na
2The content of material such as S, NaOH is relevant with the operational condition of ethylene unit raw material properties and alkaline cleaning procedure.Because the difference of each factory's cracking stock and operational path causes the composition of ethene cracking gas sour gas and content difference bigger, and then causes the composition of alkali-washing waste liquid that very big-difference is also arranged, its typical component and quality group become NaOH1%～3%, Na
2CO
33.1%～10%, Na2S1.5%～2.0%, dissolved hydro carbons 0.1%～0.3%.Therefore the comprehensive regulation of alkali-washing waste liquid or the route of utilization generally will be selected according to concrete ethylene alkali-washing waste liquid, just can obtain effect preferably.In recent decades, developed the kinds of processes route at the comprehensive regulation of ethylene alkali-washing waste liquid both at home and abroad.
Research that alkali-washing waste liquid is handled and industrialization starting abroad early, representative technology is nineteen sixties U.S.'s atmospheric oxidation law technology of at first proposing and using.This technical finesse is more thorough, but capital cost and working cost are all very high.Japan has proposed to utilize carbonic acid gas and sulfuric acid neutralisation after a while, and this method can reclaim elemental sulfur, but the alkali-washing waste liquid after the neutralization still need be handled.
The method of at present domestic each ethylene production factory and office reason alkali-washing waste liquid mainly contains following several:
1. sulfuric acid acidation-vaporizing extract process
What the ethylene unit that a collection of annual output that China's the eighties is built is 130,000 tons generally adopted is that sulfuric acid acidation-stripping (burning) route is administered alkali-washing waste liquid.
This method be earlier with 98% the vitriol oil with the ethylene alkali-washing waste liquid acidifying after, send into stripping tower again, the H that stripping comes out
2S, CO
2Burn Deng sending into torch.Acidizing fluid behind the stripping in overcooling and after, deliver to Sewage Plant and carry out biochemical treatment.This is a route that is purpose with thorough improvement alkali-washing waste liquid.Characteristics are that technology is simple, and treatment effect is good, but high to the corrosion-resistant requirement of equipment.
2.CO
2Neutralisation
The CO that Yanshan Petrochemical company utilizes intra-company's glycol unit to produce
2Waste gas and ethylene alkali-washing waste liquid reaction make the Na in the alkali-washing waste liquid
2S, NaOH etc. change into Na
2CO
3Thereby, reach remove sulfide and in and the purpose of salkali waste.Ethylene alkali-washing waste liquid is after this method is handled, and sulfide concentration can drop to below the 40mg/L.In addition, Na in the alkali lye after this method is handled
2CO
3And NaHCO
3Concentration can reach about 20%, can replace calcined soda for industry to use.
CO
2Neutralisation is a treatment of wastes with processes of wastes against one another, the technology of comprehensive utilization, and flow process is short, and equipment is simple, and equipment material requires low, does not produce advantages such as secondary pollution, but prerequisite has cheap CO near being
2Waste gas.
3.H
2The S neutralisation
H
2The S neutralisation is a purpose with the sodium sulphite that reclaims in the alkali-washing waste liquid.This technology can be produced Na from alkali-washing waste liquid
2S.But the Na that makes like this
2Contain partial organic substances in the S product, influence quality product.
4. be used for pulping and paper-making
NaOH in the ethylene waste lye and Na
2S is the effective constituent of alkaline process cooking liquor, but oily substance wherein is difficult to Ex-all, and paper surface often is with oil drop, and influences paper quality.
5. oxide treatment method
This method mainly is that the oxygenizement by various oxygenants is converted into harmless vitriol, thiosulphate, sulphite etc. to the sulfide in the alkali-washing waste liquid.Difference according to employed oxygenant and treatment process is divided into air oxidation process, wet air oxidation, chlorine oxidation process and supercritical oxidation process, these methods all have speed to handle advantage completely soon, but all shortcoming is difficult to be accepted by manufacturer because its complex process, processing cost height, facility investment be big etc.
Summary of the invention
Problem to be solved by this invention: at the problems referred to above, processing method of the present invention attempts to make alkali-washing waste liquid can recycle after treatment, in the alkali-washing waste liquid treating processes, at first remove the oils organism in the alkali-washing waste liquid, remove the CO in the alkali-washing waste liquid then
3 2-And S
2-, the alkali-washing waste liquid after the processing can be recycled.Simultaneously with CO
3 2-And S
2-Become the high salt of added value, the back of purifying is as commodity selling.
Technical scheme of the present invention is: a kind of technique for reclaiming ethylene alkali-washing waste liquid, and its operation steps is as follows: a kind of technique for reclaiming ethylene alkali-washing waste liquid, it is as follows to it is characterized by operation steps:
(1) oil removing: waste lye is heated to 20～60 ℃, stirs and drop into supported solid flocculation agent O down
x, wherein flocculant addition is 3～12g/100ml alkali lye, continues to stir 20min, has flocks to produce in the alkali lye, stops to stir, and solution is separated with supercentrifuge, floss falls to container bottom, inclines to the faint yellow transparent alkali lye in upper strata;
Supported solid flocculation agent O recited above
XBe load Mg
2+, Al
3+Or Fe
2+The ionic macroporous anion exchange resin;
(2) causticization: under agitation alkaline earth metal oxide or corresponding metal oxyhydroxide are added the filtrate of having passed through step (1) oil removing;
(3) desulfurization: add CuO, ZnO, FeO or CoO under stirring in the filtrate of passing through step (2) causticization, add-on is 1～5g/100ml alkali lye, when being heated to 30～90 ℃, continues to stir 20～60min, filters, and obtains clarifying regeneration alkali lye.
In technique for reclaiming ethylene alkali-washing waste liquid of the present invention, the alkaline earth metal oxide that uses in the described causticization process is calcium oxide or magnesium oxide.
In technique for reclaiming ethylene alkali-washing waste liquid of the present invention, the alkali lye that carries out causticization in the step (2) is through the one or many oil removing.
In technique for reclaiming ethylene alkali-washing waste liquid of the present invention, described macroporous anion exchange resin is 201 * 4,201 * 7,001 * 7,7170, D001, D101, D201, D301,330 or 110 resins.
The supported solid flocculation agent of Shi Yonging in the present invention, obtained by following preparation method: will drop in 10% metal salt solution with 1: 1 (volume ratio) through the activatory macroporous anion exchange resin, 30～60 ℃ were soaked 4 hours down, afterwards drop water purification solution, take out resin, make O
xLoad series type solid flocculation agent.
This supported solid flocculation agent oil removing is after regeneration can treatedly be reused, and renovation process is: the 1%H that uses equal volume after water washing
2O
2Normal temperature soaks 30～60min down, takes out the back and prepares the supported solid flocculation agent again with top supported solid flocculation agent preparation method.This flocculation agent uses the back deoiling effect not have considerable change through 80 reprocessing cycle.
Beneficial effect:
1, deoiling effect is obvious: the use of flocculation agent makes deoiling effect obvious: the solid flocculation agent has overcome the shortcoming that the liquid flocculation agent need dilute, the alkali lye after this method is handled, and color obviously shoals, and viscosity obviously reduces.And, follow-up causticization and sweetening process provide guarantee for obtaining the fine product.Adopt the waste lye after deoiling method of the present invention is handled to detect through Environment Monitor Center, Tianjin City, its oil-contg drops to 0.69mg/L from 14.6mg/L.
2, technological process is simple, and productive expense is low, removes CO
3 2-And S
2-Respond well Deng impurity, gained regeneration alkali lye meets the processing requirement of ethylene alkali-washing fully, only need replenish small amount of N aOH and just can recycle in alkali washing process.
3, by product is recycling, helps environment: the by product among the present invention comprises that adding metal oxide in the alkali lye that adopts after the causticization makes wherein S
2-Be converted into the materials such as CuS, ZnS of high added value, can be used as the medicine industry raw material and use after purifying, the forward price value is far above Na
2S, and removed crystallisation by cooling process in the existing crystallization processes from, greatly reduce running cost, also brought high economic benefit for spent lye treatment.
Embodiment
Embodiment 1:
In the 100ml beaker, add the 10%Al (NO that has configured
3)
3Aqueous solution 25ml drops into 20g macroporous anion exchange resin 201 * 7 in the solution again, and normal temperature soaked 4 hours down, took out, and drop water purification solution makes supported solid flocculation agent O
1
Embodiment 2:
In the 100ml beaker, add the 10%Mg (NO that has configured
3)
2Aqueous solution 25ml drops into 20g macroporous anion exchange resin 201 * 4 in the solution again, and normal temperature soaked 4 hours down, took out, and drop water purification solution makes supported solid flocculation agent O
2
Embodiment 3:
In the 100ml beaker, add the 10%MgSO that has configured
4Aqueous solution 25ml drops into 20g macroporous anion exchange resin D301 in the solution again, and normal temperature soaked 4 hours down, took out, and drop water purification solution makes supported solid flocculation agent O
3
Embodiment 4:
In the 100ml beaker, add the 10%FeCl that has configured
2Aqueous solution 25ml drops into 20g macroporous anion exchange resin D201 in the solution again, and normal temperature soaked 4 hours down, took out, and drop water purification solution makes supported solid flocculation agent O
4
Embodiment 5:
With Al (NO
3)
3The aqueous solution changes AlCl into
3The aqueous solution, other operation steps make supported solid flocculation agent O with embodiment 1
5
Embodiment 6:
(1) oil removing: in the 200ml flask, drop into the 100ml waste lye, be heated to 40 ℃, stir and drop into the supported solid flocculation agent O that makes among the 10g embodiment 1 down
1, continue to stir 20min, promptly there is flocks to produce in the alkali lye.Stop to stir, in the special-purpose test tube of solution impouring, separate with supercentrifuge, floss falls to the test tube bottom, and inclining the faint yellow transparent alkali lye in upper strata, is the alkali lye after the oil removing.The cotton-shaped oily substance otherwise processed of test tube bottom.
(2) causticization: in the alkali lye input 200ml flask through step 1 oil removing, be heated to 90 ℃, under agitation 5g MgO added wherein, continue to stir 30min.Filter out the MgCO of generation with B
3White precipitate otherwise processed, filtrate are carried out next step sulfur removal technology operation.
(3) desulfurization: in the alkali lye input 200ml flask through step 2 causticization, when being heated to 60 ℃, stir down and continue to stir 50～60min to wherein adding 3.5gCuO, promptly there is sulfuration CuS powder from solution, to be precipitated out in the alkali lye, filter except that copper sulfide precipitation with B, filtrate promptly is to remove S
2-Regeneration alkali lye.
Product is pressed the content check of GB/T16488-1996 through infrared spectrophotometric determination water PetroChina Company Limited.'s class and vegetable and animals oils, and oil-contg is 6.9mg/L in the regeneration alkali lye; With [Ca in the GB/T 14848-93 standard
2+] check of the concentration method of inspection, [Ca in the solution
2+] be 12mg/L; Titration method detects [S in the solution
2-] be 2mg/L.All meet the ethylene alkali-washing processing requirement.Gained by product MgCO
3Better with the CuS quality, but the peculiar smell of oily substance slightly, roasting can be eliminated under vacuum.
Embodiment 7
With in embodiment 6 steps (1) through the alkali lye of an oil removing, drop into once more in the 200ml flask, in kind carry out the secondary oil removing.Other operation stepss are with embodiment 6.
With the method for inspection check identical with embodiment 6, oil-contg in the regeneration alkali lye is reduced to 1.9mg/L, outward appearance clarity is significantly better than the effect of an oil removing among the embodiment 1, in application process, alkaline cleaning procedure requires the height repeatedly oil removing that can circulate to deoiling effect, but only needs 1～2 oil removing to meet the demands fully for the requirement of general soda-wash tower.The by product MgCO that obtains
3Quality is better, the peculiar smell of basically eliminate oily substance.CuS promptly can improve more than the purity to 99% through roasting under the vacuum.
Embodiment 8
(1) oil removing: in the 200ml flask, drop into the 100ml waste lye, be heated to 40 ℃, stir and drop into the supported solid flocculation agent O that makes among the 10g embodiment 2 down
2, continue to stir 20min, promptly there is flocks to produce in the alkali lye.Stop to stir, in the special-purpose test tube of solution impouring, separate with supercentrifuge, floss falls to the test tube bottom, and inclining the faint yellow transparent alkali lye in upper strata, is the alkali lye after the oil removing.The cotton-shaped oily substance otherwise processed of test tube bottom.
(2) causticization: in the alkali lye input 200ml flask through step 1 oil removing, be heated to 90 ℃, under agitation 5g MgO added wherein, continue to stir 30min.Filter out the MgCO of generation with B
3The white precipitate otherwise processed is taken out filtrate and is carried out next step sulfur removal technology operation.
(3) desulfurization: in the alkali lye input 200ml flask through step 2 causticization, when being heated to 60 ℃, stir down and continue to stir 50～60min to wherein adding 3.5gCuO, promptly there is sulfuration CuS powder from solution, to be precipitated out in the alkali lye, filter except that copper sulfide precipitation with B, filtrate promptly is to remove S
2-Regeneration alkali lye.
With the method for inspection check identical with embodiment 6, oil-contg, [Ca in the regeneration alkali lye
2+], [S
2-] all the result with embodiment 6 is suitable for value, meets the ethylene alkali-washing processing requirement.
Embodiment 9
(1) oil removing: in the 200ml flask, drop into the 100ml waste lye, be heated to 40 ℃, stir and drop into the supported solid flocculation agent O that makes among the 10g embodiment 3 down
3, continue to stir 20min, promptly there is flocks to produce in the alkali lye.Stop to stir, in the special-purpose test tube of solution impouring, separate with supercentrifuge, floss falls to the test tube bottom, and inclining the faint yellow transparent alkali lye in upper strata, is the alkali lye after the oil removing.The cotton-shaped oily substance otherwise processed of test tube bottom.
(2) causticization: in the alkali lye input 200ml flask through step 1 oil removing, be heated to 90 ℃, under agitation 5g MgO added wherein, continue to stir 30min.Filter out the MgCO of generation with B
3The white precipitate otherwise processed is taken out filtrate and is carried out next step sulfur removal technology operation.
(3) desulfurization: in the alkali lye input 200ml flask through step 2 causticization, when being heated to 60 ℃, stirring down and continue to stir 50～60min, promptly have the CuS powder from solution, to be precipitated out in the alkali lye to wherein adding 3.5gCuO, filter except that copper sulfide precipitation with B, filtrate promptly is to remove S
2-Regeneration alkali lye.
Through check, the oil-contg in the regeneration alkali lye is identical with the deoiling effect among the embodiment 2, the by product CaCO that obtains
3Quality is better, the peculiar smell of basically eliminate oily substance.ZnS promptly can improve more than the purity to 99% through roasting under the vacuum.
Embodiment 10
Solid flocculation agent among the embodiment 9 is changed to the O that makes among the embodiment 4
4, to operate identical disposal methods waste lye with embodiment 9, the result who manages result and embodiment 6 through above-mentioned method of inspection master meter in the open is suitable.
Embodiment 11
With the supported solid flocculation agent O that makes among the embodiment 5
5, using and the identical disposal methods degree alkali lye of embodiment 9 operations, the result who manages result and embodiment 6 through above-mentioned method of inspection master meter in the open is suitable.
Embodiment 12
1. with the supported solid flocculation agent O that makes among the used embodiment 3
3Drop in the beaker, with the 1%H of equal volume
2O
2Solution soaked 4 hours for 50 ℃.
2. use with embodiment 1 in the identical method of step 1, with MgSO
4Preparation supported solid flocculation agent.
3. use with embodiment 3 in step 3,4 identical methods carry out causticization and desulfurization.
Detect supported solid flocculation agent O through the method for inspection identical with embodiment 6
3After recycling through 80 times, the spent lye treatment effect still can reach the deoiling effect identical with embodiment 7.
Claims (4)
1, a kind of technique for reclaiming ethylene alkali-washing waste liquid, it is as follows to it is characterized by operation steps:
(1) oil removing: waste lye is heated to 20～60 ℃, stirs and drop into supported solid flocculation agent O down
X, wherein flocculant addition is 3～12g/100ml alkali lye, continues to stir 20min, has flocks to produce in the alkali lye, stops to stir, and solution is separated with supercentrifuge, floss falls to container bottom, inclines to the faint yellow transparent alkali lye in upper strata;
Supported solid flocculation agent O recited above
XBe load Mg
2+, Al
3+Or Fe
2+The ionic macroporous anion exchange resin;
(2) causticization: under agitation alkaline earth metal oxide or the adding of corresponding metal oxyhydroxide have been passed through in the alkali lye of step (1) oil removing, add-on is 1～5g/100ml alkali lye, is heated to 40～90 ℃, continues to stir 30～80min, filters back taking-up filtrate;
(3) desulfurization: add CuO, ZnO, FeO or CoO under stirring in the filtrate of passing through step (2) causticization, add-on is 1～5g/100ml alkali lye, when being heated to 30～90 ℃, continues to stir 20～60min, filters, and obtains clarifying regeneration alkali lye.
2, technique for reclaiming ethylene alkali-washing waste liquid as claimed in claim 1 is characterized by the alkaline earth metal oxide that uses in the described causticization process and is calcium oxide or magnesium oxide.
3, technique for reclaiming ethylene alkali-washing waste liquid as claimed in claim 1 is characterized by the alkali lye process one or many oil removing of carrying out causticization in the step (2).
4, technique for reclaiming ethylene alkali-washing waste liquid as claimed in claim 1 is characterized by described macroporous anion exchange resin and is 201 * 4,201 * 7,001 * 7,7170, D001, D101, D201, D301,330 or 110 resins.
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|---|---|---|---|
| CNB2005101221854A CN100348512C (en) | 2005-12-06 | 2005-12-06 | Technique for reclaiming ethylene alkali-washing waste liquid |
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|---|---|---|---|
| CNB2005101221854A CN100348512C (en) | 2005-12-06 | 2005-12-06 | Technique for reclaiming ethylene alkali-washing waste liquid |
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| CN100348512C true CN100348512C (en) | 2007-11-14 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838073B (en) * | 2009-03-20 | 2012-10-10 | 宝山钢铁股份有限公司 | Silicon steel alkali rinse purification method and device |
| CN102452672B (en) * | 2010-11-01 | 2013-08-14 | 中国石油化工股份有限公司 | Method for recycling sodium sulfate from waste alkali liquor of ethylene unit |
| CN102452673B (en) * | 2010-11-01 | 2014-01-08 | 中国石油化工股份有限公司 | Recovery processing method of waste alkaline liquor in ethylene plant |
| CN102452674B (en) * | 2010-11-01 | 2013-11-06 | 中国石油化工股份有限公司 | Processing method for recycling sodium sulfate from waste alkali liquor in ethylene unit |
| CN102815812B (en) * | 2011-06-10 | 2013-11-06 | 中国石油化工股份有限公司 | Optimization process method for recovering sodium sulfate form ethylene waste alkali |
| CN102815815B (en) * | 2011-06-10 | 2013-11-06 | 中国石油天然气股份有限公司 | Method for processing acid gas alkali-wash waste liquor |
| CN102424498B (en) * | 2011-10-19 | 2013-09-25 | 谢辉灿 | Circular and comprehensive utilization method for ethylene alkali waste liquid |
| CN114605041B (en) * | 2022-04-01 | 2022-12-06 | 扬州工业职业技术学院 | Environment-friendly purification device and method for purifying industrial high-alkalinity wastewater |
| CN115155311A (en) * | 2022-07-11 | 2022-10-11 | 锦州泰丰精细化工有限公司 | Regeneration process of desulfurization waste alkali |
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|---|---|---|---|---|
| CN1205985A (en) * | 1997-07-22 | 1999-01-27 | 中国石油化工总公司 | Treatment process of naphthenic acid effluents in oil refinery |
| US6589427B2 (en) * | 2001-02-28 | 2003-07-08 | Council Of Scientific & Industrial Research | Process for treatment of mixture of spent wash from distillery and black liquor from pulp and paper industry |
| CN1544347A (en) * | 2003-11-19 | 2004-11-10 | �Ϻ���ͨ��ѧ | Processing method of cupric ion of phthalocyanine green waste water using 335 type alkalescence anion resin |
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2005
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1205985A (en) * | 1997-07-22 | 1999-01-27 | 中国石油化工总公司 | Treatment process of naphthenic acid effluents in oil refinery |
| US6589427B2 (en) * | 2001-02-28 | 2003-07-08 | Council Of Scientific & Industrial Research | Process for treatment of mixture of spent wash from distillery and black liquor from pulp and paper industry |
| CN1544347A (en) * | 2003-11-19 | 2004-11-10 | �Ϻ���ͨ��ѧ | Processing method of cupric ion of phthalocyanine green waste water using 335 type alkalescence anion resin |
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