CN102020596A - Desalination refining method in production of petroleum sulfonate - Google Patents
Desalination refining method in production of petroleum sulfonate Download PDFInfo
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- CN102020596A CN102020596A CN201010592365XA CN201010592365A CN102020596A CN 102020596 A CN102020596 A CN 102020596A CN 201010592365X A CN201010592365X A CN 201010592365XA CN 201010592365 A CN201010592365 A CN 201010592365A CN 102020596 A CN102020596 A CN 102020596A
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Abstract
The invention discloses a desalination refining method in the production of petroleum sulfonate, wherein a separating method of phase separation by adding organics is used to precipitate the organic salts and the inorganic salts in the salt-containing solution of the petroleum sulfonate or enrich the organic salts and the inorganic salts in another liquid phase, and lower the petroleum sulfonate concentration in the new phase of the enriched salts, thereby realizing the purposes of desalination and maximum recovery and refining of the petroleum sulfonate. The mixture of one or more materials of ketone, alcohol, ester, aldehyde, organic acid and the like is used as the extracting agent or the assistant to separate the organic salts, the inorganic salts and the like in the salt-containing solution of the petroleum sulfonate, thereby realizing the purpose of separating the components. The separated surface-active product without the organic salts and the inorganic salts can be used in the tertiary oil recovery, has better compatibility with the oil field and can reduce the interfacial tension more efficiently. The method of the invention has simple process and low operation cost, and can well solve the problems of long time consumption, insufficient desalination and the environment pollution of the waste water generated during production of the precipitation desalination method in the traditional production process of the petroleum sulfonate. The obtained active matter with higher purity can be used as the main raw material of the oil field chemical in the tertiary oil recovery, and has better compatibility with the oil field and high industrial application value.
Description
Technical field
The present invention relates to the desalting refinement method in a kind of sulfonated petro-leum production, mainly be to realize that by adding organism the isolating method of phase-splitting removes organic salt except that sulfonated petro-leum and inorganic salt in the sulfonated petro-leum salt-containing solution, make organic salt and inorganic salt except that sulfonated petro-leum be settled out or be enriched in another liquid phase, and make the mahogany acid salt concn in the cenotype of enrichment salt lower, thereby reclaim, the purification sulfonated petro-leum.Belong to petrochemical industry.
Background technology
Along with the exploitation of oil, the deficiency of the exhausted year by year and reserved resources of resource, improving oil recovery is the important topic of studying both at home and abroad.Petroleum sulfonate for tertiary oil recovery is one of important chemical agent that improves oil recovery factor, belongs to anion surfactant, can reduce oil water interfacial tension, reduces the work of adhesion effect, reaches crude oil is peeled off from the stratum, drives the purpose of extraction.Along with improving going deep into of recovery efficiency technique research, the performance and the adaptability of tensio-active agent all there has been higher requirement.
At present, preparation sulfonated petro-leum analog anion surfactants be with fraction oil of petroleum for being sulfonated the agent thing, the employing vitriol oil is the liquid phase still formula of sulphonating agent or with SO
3Gas for sulphonating agent---the preparation of liquid film type process for sulfonation.Its operational path is: at first stock oil and solvent ethylene dichloride are preheating to temperature of reaction, under agitation slowly drip sulphonating agent, and sulfonation process is carried out acid number monitoring, stopped reaction after its value reaches requirement.The sulfonated products mahogany acid is neutralized with ammonia soln or other alkali, and the system PH of making is 7～9, thereby obtains containing the thick product of sulfonated petro-leum of aqueous solvent, inorganic salt and organic salt.The thick product working substance of the sulfonated petro-leum of present various sulfonated petro-leum explained hereafter (sulfonate that wetting ability and lipophilicity are suitable) content is lower, wherein contains a large amount of inorganic salt and unsulfonated oil and moisture or volatile matter.Directly as the oil-displacing agent of tertiary oil recovery, the effect that reduces interfacial tension is undesirable for this thick product.
Patent CN1203935A discloses a kind of petroleum sulfonate for tertiary oil recovery, method for making and application.This invention product is to be raw material with natural oil or distillate, uses SO
3Sulfonation is produced, and the reactant after the sulfonation reaction feeds water miscible sulfonated petro-leum slurry tank, and the throw out of bottom is pumped into neutralization tank, add the alkali neutralization, mix, sedimentation is more than 4 hours, top solution adds alkali and is neutralized to PH 7～9, promptly produces water miscible sulfonated petro-leum; Use alcoholic extract behind the slurry tank middle and upper part acid coil neutralization, after the sedimentation phase-splitting, the oil-soluble sulfonated petro-leum in bottom is separated, behind the recovery of alcohol distillation, promptly produce oil-soluble sulfonated petro-leum.Oil-soluble sulfonated petro-leum and water miscible sulfonated petro-leum are in harmonious proportion the sulfonated petro-leum of promptly producing used for tertiary oil recovery by a certain percentage.The component of this sulfonated petro-leum (weight %) is an oil soluble sulfonated petro-leum 2～60%, salt 5～15%.Unsulfonated oil 10～20%, water 15～30%.This invention separates oil-soluble sulfonated petro-leum and water miscible sulfonated petro-leum respectively, and target product can ratio on demand be in harmonious proportion.But the sulfonated petro-leum sepn process is consuming time longer, and salts contg is higher in the product, and standard is used in the oil field at present head and shoulders above.
Patent CN1327979A relates to a kind of petroleum sulfonate used in oil field technology that is made through sulfonation by the distillate of aryl crude oil, particularly separates the technology of sulfonated petro-leum after sulfonation the mixture.Patent adopts the sulfonation of three grades of continuous pot group type sulfonation reactors, and the mix products that makes after the sulfonation separates with alcohol extraction earlier, use in the NaOH aqueous solution again and sulfonic acid to PH10, concentrate then, reclaim ethanol, promptly get the mahogany acid product salt.Though product main component mahogany acid salts contg of the present invention increases substantially, guaranteed quality product, but raffinate promptly contains in the salt-containing solution of sulfonated petro-leum and still contains a large amount of table beings, not mentionedly in the patent how to recycle table being wherein and removes wherein organic salt and inorganic salt.
Patent CN1230420C discloses a kind of sulfonated petro-leum continuous preparation method, be 2-8 placed in-line sulfonation reaction jar generation sulfonation reaction, the sulfonic acid that comes out from last sulfonation jar is after ammoniacal liquor is neutralized to PH=7,130 ℃ of distillations down, divide the branch that anhydrates, the ethylene dichloride re-injection that steams, the inorganic salt in the filtration product will be purpose product sulfonated petro-leum behind the filtrate evaporate to dryness fugitive constituent ethylene dichloride.Ethylene dichloride can not dissolve sulfonated petro-leum well in the desalting method that this invention relates to, and carries a large amount of sulfonated petro-leums in the inorganic salt that this step can cause telling, and product loss is more serious.
The sulfonated petro-leum salt-containing solution comprises: the solution that 1. contains the sulfonate of solvent (as ethylene dichloride), sulfonated petro-leum, unsulfonated oil, water, inorganic salt and strong water-soluble; 2. after removing solvent, contain the sulfonate of inorganic salt, unsulfonated oil, water, strong water-soluble and the solution of bulk petroleum sulfonate; 3. the waste water that contains sulfonated petro-leum, inorganic salt and strong water-soluble sulfonate.Because salt (inorganic salt except that sulfonated petro-leum and organic salt) content is higher in the sulfonated petro-leum, and is relatively poor with the compatibleness in oil field, makes it that many limitation be arranged in use.Simultaneously, contain a large amount of sulfonated petro-leums in the brine waste that preparation produces during sulfonated petro-leum, removing wherein salt, to reclaim tensio-active agent simultaneously be present important research project.
Summary of the invention
The objective of the invention is to overcome the above-mentioned defective of prior art, a kind of method that removes the inorganic salt except that sulfonated petro-leum and organic salt in the sulfonated petro-leum saline solns is provided.It is higher to reach the active principle content that makes in the sulfonated petro-leum by method provided by the invention, with the better purpose of oil field compatibleness.
The present invention solves the technological line that its desalting technology problem adopted: adopt to add organism and reach the isolating method of phase-splitting and realize separation to each component in the sulfonated petro-leum saline solns.Promptly in the sulfonated petro-leum saline solns, add one or more organic mixtures and carry out desalination, make organic salt and inorganic salt except that sulfonated petro-leum be settled out or be enriched in another liquid phase, and make the mahogany acid salt concn in the cenotype of enrichment salt lower, thereby finally reach desalination, reclaim the purpose of turpentole sulfonate to greatest extent.
Concrete technical scheme is: add organism and separate in the sulfonated petro-leum saline solns, raw material and organic mass ratio are: 100: (1～10000), organism comprises ketone, alcohol, ester, aldehyde, organic acid etc., and organic adding method is that one or more join in the stirring tank after mixing in the above-mentioned organism.Organism stirs after adding, mixture was reacted in still after 0.001～6 hour can realize making inorganic salt and organic salt in the sulfonated petro-leum salt-containing solution to be settled out or to be enriched in another liquid phase in static again 0.001～10 hour, and make the mahogany acid salt concn in the cenotype of enrichment salt lower, thereby realize desalination or reclaim the purpose of turpentole sulfonate product.
The present invention is because the separation method that adopts the adding organism to reach phase-splitting has been realized the desalination or the recovery of sulfonated petro-leum salt-containing solution refining preferably, and facility investment and running cost are cheap, and resulting higher degree actives is used for tertiary oil recovery and the oil field compatibleness is better.
Compared with prior art the present invention has the following advantages: (one) has solved traditional settling desalting method long and inadequate problem of desalination consuming time; (2) brine waste problem of environment pollution caused (three) the present invention who has solved the table being that produces in the mahogany acid technology of threonates can make the saltiness that reclaims in the purified sulfonated petro-leum drop to below 4%; (4) mahogany acid product salt after the desalination of the present invention and oil field compatibleness are better, can more effectively reduce interfacial tension; (5) technical process of the present invention is simple, easy to operate, and one-time investment is little, and running cost is low; (6) after the present invention separates inorganic salt in the sulfonated petro-leum brine waste (salt-containing solution), actives, ethylene dichloride, waste residue wet goods component, further reclaim and to have obtained the quality water of actives and low COD preferably.
Embodiment
Describe the present invention in detail below in conjunction with embodiment.
Embodiment 1: alcohol mixeding liquid is handled the sulfonated petro-leum brine waste
Use raw material: the sulfonated petro-leum brine waste that raw material provides as Shengli Oilfield Zhongsheng Environmental Protection Co., Ltd..Wherein showing the being mass content is 8～10%, and inorganic salt ammonium sulfate mass content is 30～35%, and quality content is 50～55%, and the sulfonate mass content of strong water-soluble is 1～12%.
Concrete steps:
1. take by weighing raw material sulfonated petro-leum brine waste 101 grams and place beaker;
2. under stirring condition, add alcohol mixeding liquid 300 grams, and continue to stir 20 minutes down at 30 ℃;
3. leave standstill a moment, be settled out inorganic salt and organic salt in the solution, filter, and carry out the salt that repeatedly washing precipitation goes out with dehydrated alcohol, and with dry 2 hours of the salt that is settled out, weighing, get salt dry weight 32 grams, the massfraction that accounts for the sulfonated petro-leum brine waste is 32%;
4. filtrate is transferred in the flask, distilled, reclaim ethanol;
5. the dope after distilling with 100 gram hot ethanol mixed solution dissolution extraction filters, and filtrate is repeated operation in 4, dry 2 hours of gained reddish-brown dope, and weighing gets surface-active substance product 9 grams.
Embodiment 2: the Virahol mixed solution is handled sulfonated petro-leum brine waste I
Use raw material: identical with embodiment 1
Concrete steps:
1. take by weighing raw material sulfonated petro-leum brine waste 109 grams, add H
2SO
4Solution neutralizes;
2. add 220 gram Virahol mixed solutions, stirred 4 hours, leave standstill, be settled out inorganic salt and organic salt in the solution, filter, dry that salt dry weight 32.9 restrains, the massfraction that accounts for the sulfonated petro-leum brine waste is 30%.
3. filter the filtrate 260 gram branch two-phases that obtain.Tell upper strata liquid and subnatant with separating funnel.
4. upper strata liquid is distilled, separate out a spot of salt, wash material in the flask with the hot ethanol mixed solution, get salt 1.1 grams after filtration, the drying, the massfraction that accounts for the sulfonated petro-leum brine waste is 1%, and the filtrate evaporate to dryness is weighed to such an extent that actives 7.3 restrains.
5. subnatant is distilled, separate out more salt, with the flushing of hot ethanol mixed solution, get white crystals 11.6 grams after filtration, the drying, the massfraction that accounts for the sulfonated petro-leum brine waste is 10%.
6. ethanol washing lotion baking in 5 is removed fugitive constituent, dry actives 0.85 gram.
Embodiment 3: the Virahol mixed solution is handled sulfonated petro-leum brine waste II
Use raw material: identical with embodiment 1
Concrete steps:
1. take by weighing raw material sulfonated petro-leum brine waste 122.5 grams, add H
2SO
4Solution neutralizes;
2. add 490 gram Virahol mixed solutions, stirred 4 hours, leave standstill, be settled out inorganic salt and organic salt in the solution, filter, dry that salt dry weight 43.0 restrains, the massfraction that accounts for the sulfonated petro-leum brine waste is 35%.
3. filter the filtrate 400 gram branch two-phases that obtain.Tell upper strata liquid and subnatant with separating funnel.
4. upper strata liquid is distilled, separate out a spot of salt, wash material in the flask with the hot ethanol mixed solution, get salt 1.93 grams after filtration, the drying, the massfraction that accounts for the sulfonated petro-leum brine waste is 2%, and the filtrate evaporate to dryness is weighed to such an extent that actives 7.9 restrains.
5. subnatant is distilled, separate out a spot of salt, with the flushing of hot ethanol mixed solution, get white crystals 0.5 gram after filtration, the drying, the massfraction that accounts for the sulfonated petro-leum brine waste is 0.4%.
6. ethanol washing lotion baking in 5 is removed fugitive constituent, dry actives 0.38 gram.
Embodiment 4: the Virahol mixed solution is handled saliniferous sulfonated petro-leum neutralizer I
Use raw material: the sulfonated petro-leum neutralizer that raw material provides as Shengli Oilfield Zhongsheng Environmental Protection Co., Ltd..Wherein showing the being mass content is 15～18%, the ethylene dichloride mass content is 48～55%, and inorganic salt ammonium sulfate mass content is 6～9%, and quality content is 15～18%, the mass content of unsulfonated oil is 10～15%, the sulfonate 1～10% of strong water-soluble.
Concrete steps:
1. take by weighing bed blending liquid 98.5 grams, place 105 ℃ oil bath to reclaim the solvent ethylene dichloride;
2. add 116.5 gram Virahol mixed solutions, stirred 4 hours, leave standstill, be settled out inorganic salt and organic salt in the solution, filter, dry that salt dry weight 12.8 restrains, the massfraction that accounts for neutralizer is 13.0%;
3. filter filtrate 217.5 grams that obtain, analyze to such an extent that table being 15.3 restrains, accounting for the neutralizer massfraction is 15.5%;
4. filter residue PetroChina Company Limited. sulfonate 1.5 restrains, inorganic salt except that sulfonated petro-leum and organic salt 11.3 grams, and accounting for the neutralizer massfraction is 11.5%.
Embodiment 5: the Virahol mixed solution is handled saliniferous mahogany acid neutralizer II
Use raw material: identical with embodiment 4
Concrete steps:
1. take by weighing bed blending liquid 74.1 grams, place 105 ℃ oil bath to reclaim the solvent ethylene dichloride;
2. add 82.1 gram Virahol mixed solutions, stirred 4 hours, leave standstill, be settled out inorganic salt and organic salt in the solution, filter, dry that salt dry weight 12.3 restrains, the massfraction that accounts for neutralizer is 16.5%;
3. filter filtrate 202.5 grams that obtain, analyze to such an extent that table being 11.8 restrains, accounting for the neutralizer massfraction is 16.0%;
4. filter residue PetroChina Company Limited. sulfonate 0.8 restrains, inorganic salt except that sulfonated petro-leum and organic salt 11.5 grams, and accounting for the neutralizer massfraction is 15.5%.
Claims (6)
1. the desalting method during a sulfonated petro-leum is produced, be in sulfonated petro-leum table being saline solns, to add organism to carry out desalination, make organic salt and inorganic salt except that sulfonated petro-leum be settled out or be enriched in another liquid phase, and make the mahogany acid salt concn in the cenotype of enrichment salt lower, thereby reach desalination, reclaim turpentole sulfonate to greatest extent.
2. method according to claim 1 is characterized in that: described salt-containing solution comprises the sewage that solvent reaches not solvent-laden mahogany acid salt brine solution and contains sulfonated petro-leum that contains in the sulfonated petro-leum production process.Wherein water-content is 0～99%, and table being content is 1～80%, and salt (comprising inorganic salt and organic salt except that sulfonated petro-leum) content is 1～60%.
3. according to arbitrary described method among the claim 1-2, it is characterized in that: salt comprises inorganic salt and organic salt, and described inorganic salt comprise vitriolate of tartar, ammonium sulfate, sodium sulfate, calcium sulfate, barium sulfate, sal epsom; Organic salt comprises water-soluble very strong but be insoluble to the organic polysulfonate of alcoholic acid, does not comprise the water-soluble sulfonated petro-leum suitable with oil soluble.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the temperature of described desalination is 0～300 ℃; The pressure of desalination comprises decompression, normal pressure and pressurization, and absolute pressure is 0～10Mpa.
5. according to the described method of claim 1-4, it is characterized in that: described organism comprises ketone, alcohol, ester, aldehyde, organic acid etc.
6. method according to claim 5 is characterized in that: ketone comprises acetone, butanone, methyl tertbutyl ketone, pentanone, heptanone etc.; Alcohol comprises methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, amylalcohol, enanthol, octanol, ethylene glycol, propylene glycol, butyleneglycol etc.; Ester comprise methyl-formiate, ethyl formate,, propyl formate, butyl formate, methyl acetate, ethyl acetate, propyl acetate, n-butyl acetate, methyl propionate, ethyl propionate, butyl propionate, isoamyl butyrate, ethyl hexanoate etc.; Aldehyde comprises formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, isobutyric aldehyde, valeral, enanthaldehyde, oxalic dialdehyde etc.; Organic acid comprises aliphatic monobasic, binary, polycarboxylic acid, as formic acid, acetate, propionic acid, oxalic acid, propanedioic acid, Succinic Acid etc. and aromatic organic acid such as phenylformic acid, tolyl acid, toluylic acid, Whitfield's ointment etc.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271586A (en) * | 2014-06-12 | 2016-01-27 | 山东大明精细化工有限公司 | Apparatus and method for processing wastewater containing active organics and inorganics |
| CN106810475A (en) * | 2015-11-27 | 2017-06-09 | 中国石油天然气股份有限公司 | Method for removing inorganic salt from petroleum sulfonate |
| CN110523440A (en) * | 2019-08-28 | 2019-12-03 | 华南理工大学 | A kind of desalination method of purification of water-solubility chitosan derivative |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271586A (en) * | 2014-06-12 | 2016-01-27 | 山东大明精细化工有限公司 | Apparatus and method for processing wastewater containing active organics and inorganics |
| CN106810475A (en) * | 2015-11-27 | 2017-06-09 | 中国石油天然气股份有限公司 | Method for removing inorganic salt from petroleum sulfonate |
| CN106810475B (en) * | 2015-11-27 | 2018-09-04 | 中国石油天然气股份有限公司 | Method for removing inorganic salt from petroleum sulfonate |
| CN110523440A (en) * | 2019-08-28 | 2019-12-03 | 华南理工大学 | A kind of desalination method of purification of water-solubility chitosan derivative |
| CN110523440B (en) * | 2019-08-28 | 2022-04-22 | 华南理工大学 | Desalination purification method of water-soluble chitosan derivative |
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Application publication date: 20110420 |