CN106810471A - Production method of petroleum sulfonate - Google Patents
Production method of petroleum sulfonate Download PDFInfo
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- CN106810471A CN106810471A CN201510866750.1A CN201510866750A CN106810471A CN 106810471 A CN106810471 A CN 106810471A CN 201510866750 A CN201510866750 A CN 201510866750A CN 106810471 A CN106810471 A CN 106810471A
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- Prior art keywords
- sulfonation
- oil
- production method
- petroleum sulfonate
- extractant
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 51
- 239000003208 petroleum Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 62
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims description 57
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000010025 steaming Methods 0.000 claims description 7
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 6
- 238000013517 stratification Methods 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- 239000010779 crude oil Substances 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 4
- 239000011552 falling film Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims 2
- 239000004575 stone Substances 0.000 claims 2
- 239000002253 acid Substances 0.000 abstract description 19
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000002378 acidificating effect Effects 0.000 abstract 2
- 239000010802 sludge Substances 0.000 description 14
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 10
- 238000006386 neutralization reaction Methods 0.000 description 5
- 229930195734 saturated hydrocarbon Natural products 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical class C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000158728 Meliaceae Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000005586 carbonic acid group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a production method of petroleum sulfonate, which comprises the following steps: and (3) after sulfonation is finished, extracting the sulfonated acidic oil by using a solvent insoluble in petroleum components as an extracting agent, standing for layering, returning the upper layer as raffinate oil to continue sulfonation, repeating the process until the content of aromatic hydrocarbon in the raw material is reduced to below 5%, distilling the lower layer as an extracting agent containing sulfonic acid, and distilling the extracting agent to obtain sulfonic acid which can be used for further preparing sulfonate, wherein the distilled extracting agent is recycled. The method uses a solvent insoluble in petroleum components as an extracting agent to extract sulfonated acidic oil, sulfonic acid after extraction and separation is directly neutralized into sulfonate, raffinate oil returns to be sulfonated continuously, and the raffinate oil does not contain the sulfonic acid and cannot be sulfonated into acid residue again when being contacted with a sulfonating agent again, so that the purpose of improving the yield of the sulfonate is achieved.
Description
Technical field
The present invention relates to sulfonate production field, more specifically to a kind of life of petroleum sulfonate
Product method.
Background technology
Petroleum sulfonate is the widely used anion surfactant of a class, in agent for improving oilfield recovery
Etc. aspect play an important role.
Petroleum component is complicated mixture, is had a very wide distribution, containing substantial amounts of gum asphalt and
Polycyclic aromatic hydrocarbon etc., contained aromatic hydrocarbons because of structure difference sulfonation process and asynchronous, with entering for sulfonating reaction
OK, the aromatic hydrocarbons of sulfonation at first is particularly easy to further sulfonation for many sulfonic acid, so as to influence the product of sulfonate
Quality, reduces the yield of petroleum sulfonate and produces the acid sludge of environmental pollution.
To avoid the sulfonation excessively of sample, existing processing method is roughly divided into two classes：The first kind, passes through
Reduce the generation of acid sludge to the improvement of equipment, such as CN00240550, CN85109591,
CN96107060、CN200510093638、CN200520118134、CN200610028680、
CN200610102153, CN201210262133, CN201320359754 etc., these methods are only capable of
A small amount of growing amount for reducing acid sludge, the raising influence on petroleum sulfonate yield is limited.Equations of The Second Kind, plus
The method for entering solvent dilution feedstock oil reduction acid sludge, CN201210384390 discloses a kind of by residual oil
The method that sulfonation prepares oil field sulfonate surfactant is carried out, in avoiding residual oil sulfonation process
Cross sulfonation problem, propose first to dilute residual oil and solvent in mass ratio 1: 2~5, then cool down,
After sulfonating agent and solvent in mass ratio 1: 1~3 dilute, the 1/2~1/20 of relative residual oil addition is taken
Complexing agent is added in residual oil, and then aging 0.5~2h is gradually added into 1~3 times of dilution of residual oil quality
Sulfonating agent, adds alkali to be neutralized afterwards, the sedimentation removing bottom aqueous solution, solvent is distilled off, finally
Can obtain mahogany acid product salt.CN201210235703 is disclosed with SO3As sulfonating agent, non-matter
Subtype alkyl halide is solvent, the method that sulfonation prepares sulfonated humic acid at a lower temperature.
CN201010271259 and CN201310660630, discloses a kind of petroleum sulfonate surfactant
Preparation method, it with 350~500 DEG C of crude oil fractions oil is raw material that the method is, with 60~120 DEG C
Solvent naphtha, chlorinated aromatic hydrocarbons or chloralkane be diluent, the sulfur trioxide with gas phase as sulfonating agent, and
Using falling film reactor, purpose product is obtained by controlling reaction temperature, aging temperature.CN
201210094872 disclose a kind of method that tapped oil alkylate sulfonation method prepares surfactant,
Alkylate with catalytic cracked oil pulp or recycle oil tapped oil as raw material, with the concentrated sulfuric acid, oleum
Acid or SO3It is sulfonating agent, with petroleum ether, dichloroethanes, nitrobenzene as solvent, carries out sulfonating reaction
Prepare sulfonate surfactant.Although above-mentioned these methods relax sulfonating conditions, but generation
Acid sludge is present in acid-soluble oil with dissolved state, have impact on the quality of sulfonate, in addition, what is added is molten
Agent such as halogenated hydrocarbons etc. is not only big to human body infringement, serious to atmospheric environment destruction, after being remained in oil
Will also cause the chloride ion corrosion during downstream oil refining working process.
Therefore, exploitation one kind is greatly lowered acid sludge yield, improves the sulfonation of aromatic hydrocarbons utilization rate in oil
Method is very necessary.
The content of the invention
It is an object of the invention in solving petroleum sulfonate production process, easily produce acid sludge so as to drop
The problem of low sulfonated efficiency, and then provide and a kind of prevent sulfonic acid excessive sulfonation, improve petroleum sulfonate
The production method of yield
Above-mentioned purpose of the invention is achieved in that a kind of production method of petroleum sulfonate, including
Following steps：It is extractant that the solvent insoluble in petroleum component is added in sulfonating reaction, to sulfonated acid
Property oil extracted after stratification, upper strata be raffinate oil return continue sulfonation, repeat said process,
Until the arene content in raw material is dropped into less than 5%, lower floor is the extractant containing sulfonic acid, by steaming
Evaporate and steam extractant, obtaining sulfonic acid can further prepare sulfonate, the extractant recycling for steaming makes
With.
Petroleum sulfonate production method of the present invention, wherein, the sulfonation acid-soluble oil is extracted and quiet
Put preferably 30-70 DEG C of the temperature of layering, when the extractant containing sulfonic acid distills, pressure is preferably 0~
- 0.08MPa, temperature is preferably below 92 DEG C.
Petroleum sulfonate production method of the present invention, wherein, the extractant is preferably carbonic acid two
Methyl esters, diethyl carbonate or dithyl sulfate.
Petroleum sulfonate production method of the present invention, wherein, the sulfonation process is particularly preferred as：
Sulfonation raw material be petroleum component, sulfonating agent be 98% the concentrated sulfuric acid, the oleum that concentration is 20% or
The SO3 of 3-5%, sulfonating agent is 0.1-0.6 with the aromatic hydrocarbons mol ratio in sulfonation raw material：1, sulfonation raw material
It is 1 with the volume ratio of extractant：0.2-2, reaction temperature is 10-80 DEG C.
Petroleum sulfonate production method of the present invention, it is characterised in that the sulfonation raw material and extraction
The volume ratio for taking agent is preferably 1：0.5-1.
Petroleum sulfonate production method of the present invention, it is characterised in that the sulfonating agent and raw material
Aromatic hydrocarbons mol ratio in oil is preferably 0.2-0.4：1.
Petroleum sulfonate production method of the present invention, it is characterised in that the reaction temperature is preferred
It is 20-60 DEG C.
Petroleum sulfonate production method of the present invention, it is characterised in that can in the petroleum component
The arene content of sulfonation is preferably more than 10%.
Petroleum sulfonate production method of the present invention, it is characterised in that the petroleum component is preferred
It is crude oil, straight-run, hydrofined oil or furfural extract oil.
Petroleum sulfonate production method of the present invention, it is characterised in that the sulfonating reaction mode
Preferably autoclave, falling film type or atomizing.
The present invention with the solvent insoluble in petroleum component be extractant, in time will be during sulfonating reaction
Separated after the sulfonic acid extraction of generation, it is to avoid the sulfonic acid for having generated is detained and is by excessive sulfonation in systems
Acid sludge, so as to reduce the yield of acid sludge, the yield of petroleum sulfonate is enhanced about more than once, extraction
Agent proceeds sulfonation extractive reaction after being processed through distillation.
Specific embodiment
The present invention is further illustrated by the following examples, but the present invention is not limited to these embodiments.
Embodiment 1：
In autoclave sulfonation reactor, input raw material is transformer oil furfural extract oil, saturated hydrocarbon content
31.58%, aromatic hydrocarbon content 66.28%, gum asphaltic content 2.14%, according to sulfonation raw material with
The volume ratio of extractant is 1：After 1 ratio adds dimethyl carbonate stirring, add under the conditions of 50 DEG C
Entering 20% oleum sulfonating agent carries out sulfonating reaction, the aromatic hydrocarbons mole in sulfonating agent and sulfonation raw material
Than being 0.4：1.After sulfonation terminates, by sulfonation acid-soluble oil stratification, the temperature of separation is 50 DEG C,
Upper strata is the raffinate oil for removing sulfonic acid, and aromatic hydrocarbon content is 45.26%, and lower floor is the extractant containing sulfonic acid,
By relative pressure -0.02MPa, distilled at 85 DEG C of temperature and steam extractant, obtaining sulfonic acid can enter one
Step neutralization prepares sulfonate, and the extractant for steaming returns to sulfonation dress together with the raffinate oil of removing sulfonic acid
Put repetition said process to continue to react, the arene content in second raffinate oil is 27.62%, third time
Arene content in raffinate oil is 15.73%, and the arene content in the 4th raffinate oil is 8.54%, the
Arene content in five raffinate oil is 3.28%.By after five sulfonation, the cumulative yield of acid sludge is
1.87%, the sum yield of sulfonate is 72.35%.
Embodiment 2：
In autoclave sulfonation reactor, input raw material is paraffinic base crude oil, wax content：5.42%, glue
Matter content：6.79%, asphalt content：0.58%, arene content：23.52%, it is former according to sulfonation
Material is 1 with the volume ratio of extractant：After 2 add diethyl carbonate stirring, 98% concentrated sulfuric acid is added
Sulfonating reaction is carried out under the conditions of 10 DEG C, sulfonating agent is 0.1 with the aromatic hydrocarbons mol ratio in sulfonation raw material：1,
After sulfonation terminates, by sulfonation acid-soluble oil stratification, the temperature of separation is 15 DEG C, and upper strata is removing sulphur
The raffinate oil of acid, aromatic hydrocarbon content is 20.56%, and lower floor is the extractant containing sulfonic acid, by relative pressure
Power -0.04MPa, distills at 72 DEG C of temperature and steams extractant, and obtaining sulfonic acid can further neutralize preparation
Sulfonate, the extractant for steaming returns to xanthator, sulfonating agent together with the raffinate oil of removing sulfonic acid
It is 0.3 with the aromatic hydrocarbons mol ratio in sulfonation raw material：1, repeat said process and continue to react, second extraction
Arene content in excess oil is 15.43%, steams extractant by distilling, and obtaining sulfonic acid can be further
Neutralization prepares sulfonate, and the extractant for steaming returns to xanthator together with the raffinate oil of removing sulfonic acid,
Sulfonating agent is 0.6 with the aromatic hydrocarbons mol ratio in sulfonation raw material：1, repeat said process and continue to react, the
Arene content in three raffinate oil is 7.89%, repeats said process and continues to react, the 4th raffinate
Arene content in oil is 2.14%, by after four sulfonation, the cumulative yield of acid sludge is 1.28%,
The sum yield of sulfonate is 25.37%.
Embodiment 3：
Falling film sulfonation reactor, raw material is cycloalkyl second line of distillation, saturated hydrocarbon content 70.82 in raw material
%, aromatic hydrocarbon content 20.82%, gum asphaltic content 8.36%, according to sulfonation raw material and extractant
Volume ratio be 1：After 0.2 ratio adds dithyl sulfate stirring, with 5% under the conditions of 80 DEG C
Gas phase sulfur trioxide sulfonating agent carries out sulfonating reaction, and sulfonating agent is with the aromatic hydrocarbons mol ratio in sulfonation raw material
0.6：1.After sulfonation terminates, by sulfonation acid-soluble oil stratification, the temperature of separation is 70 DEG C, upper strata
To remove the raffinate oil of sulfonic acid, aromatic hydrocarbon content is 10.67%, and lower floor is the extractant containing sulfonic acid, warp
92 DEG C of distillations of normal pressure are crossed, extractant is steamed, obtaining sulfonic acid further neutralization can prepare sulfonate, steam
The extractant for going out returns to xanthator together with the raffinate oil of removing sulfonic acid and repeats said process continuation instead
Should, the arene content in second raffinate oil is 4.38%, by after secondary sulfonation, the accumulation of acid sludge
Yield is 0.96%, and the sum yield of sulfonate is 21.74%.
Embodiment 4：
Spraying sulfonation reactor, input raw material is the paraffinic base line that subtracts three, saturated hydrocarbon content 89.63%, virtue
Fragrant hydrocarbon content 9.53%, gum asphaltic content 0.84%, according to sulfonation raw material and dimethyl carbonate
Volume ratio is 1：After 0.5 ratio adds dimethyl carbonate stirring, 5% is passed through under the conditions of 40 DEG C
Gas phase sulfur trioxide sulfonating agent carries out sulfonating reaction, and sulfonating agent is with the aromatic hydrocarbons mol ratio in sulfonation raw material
0.2：1.After sulfonation terminates, by sulfonation acid-soluble oil stratification, the temperature of separation is 40 DEG C, upper strata
To remove the raffinate oil of sulfonic acid, aromatic hydrocarbon content is 7.56%, and lower floor is the extractant containing sulfonic acid, warp
Cross under relative pressure -0.08MPa, temperature 45 C to distill and steam extractant, obtaining sulfonic acid can be further
Neutralization prepares sulfonate, and the extractant for steaming returns to xanthator together with the raffinate oil of removing sulfonic acid
Repeat said process to continue to react, the arene content in second raffinate oil is 5.89%, and third time extracts
Arene content in excess oil is 3.24%, by after three sulfonation, the cumulative yield of acid sludge is 0.64%,
The sum yield of sulfonate is 10.71%.
Comparative example 1：
Spraying sulfonation reactor, input raw material is the paraffinic base line that subtracts three, saturated hydrocarbon content 89.63%, virtue
Fragrant hydrocarbon content 9.53%, gum asphaltic content 0.84% is passed through 5% gas phase under the conditions of 40 DEG C
SO 3 sulfonated dose carries out sulfonating reaction, and sulfonating agent is 0.6 with the aromatic hydrocarbons mol ratio in sulfonation raw material.
After sulfonation terminates, sulfonation acid-soluble oil is carried out into neutralization extraction, acid sludge yield is 6.49%, sulfonate
Yield is 4.32%.
Certainly, the present invention can also have other various embodiments, without departing substantially from spirit of the invention and its essence
In the case of, those of ordinary skill in the art can make various corresponding changes and change according to the present invention
Shape, but these corresponding changes and deformation should all belong to protection scope of the present invention.
Claims (10)
1. a kind of production method of petroleum sulfonate, it is characterised in that comprise the following steps：In sulfonation
It is extractant that the solvent insoluble in petroleum component is added in reaction, quiet after being extracted to sulfonation acid-soluble oil
Layering is put, upper strata is that raffinate oil is returned and continues sulfonation, repeats said process, until by the virtue in raw material
Hydrocarbon content drops to less than 5%, and lower floor is the extractant containing sulfonic acid, steams extractant by distilling,
Obtaining sulfonic acid can further prepare sulfonate, and the extractant for steaming is recycled.
2. petroleum sulfonate production method according to claim 1, it is characterised in that the sulphur
The temperature for changing acid-soluble oil extraction and stratification is 30-70 DEG C, when the extractant containing sulfonic acid distills,
Pressure is 0~-0.08MPa, and temperature is below 92 DEG C.
3. petroleum sulfonate production method according to claim 1, it is characterised in that the extraction
Agent is taken for dimethyl carbonate, diethyl carbonate or dithyl sulfate.
4. the petroleum sulfonate production method according to claim any one of 1-3, it is characterised in that
The sulfonation process is specially：Sulfonation raw material is petroleum component, and sulfonating agent is 98% concentrated sulfuric acid, dense
Spend the oleum or the SO of 3-5% for 20%3, sulfonating agent is with the aromatic hydrocarbons mol ratio in sulfonation raw material
0.1-0.6：1, sulfonation raw material is 1 with the volume ratio of extractant：0.2-2, reaction temperature is 10-80 DEG C.
5. petroleum sulfonate production method according to claim 4, it is characterised in that the sulphur
It is 1 to change raw material with the volume ratio of extractant：0.5-1.
6. petroleum sulfonate production method according to claim 4, it is characterised in that the sulphur
Agent is 0.2-0.4 with the aromatic hydrocarbons mol ratio in feedstock oil：1.
7. petroleum sulfonate production method according to claim 4, it is characterised in that described anti-
It is 20-60 DEG C to answer temperature.
8. petroleum sulfonate production method according to claim 4, it is characterised in that the stone
In oil ingredient can sulfonation arene content more than 10%.
9. petroleum sulfonate production method according to claim 4, it is characterised in that the stone
Oil ingredient is crude oil, straight-run, hydrofined oil or furfural extract oil.
10. petroleum sulfonate production method according to claim 4, it is characterised in that described
Sulfonating reaction mode is autoclave, falling film type or atomizing.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745291A (en) * | 2018-08-13 | 2018-11-06 | 宁夏然尔特工业产业研究院（有限公司） | A kind of biomass carbon and its application based on furfural dregs |
| CN109265376A (en) * | 2018-10-22 | 2019-01-25 | 中石油克拉玛依石化有限责任公司 | The method and device of continous way production petroleum sulfonate |
| CN109824552A (en) * | 2019-01-28 | 2019-05-31 | 高路生 | A kind of petroleum sulfonate and preparation method thereof |
| CN114088797A (en) * | 2021-11-09 | 2022-02-25 | 中国石油大学(北京) | Sulfonation method and analysis method of aromatic hydrocarbon compounds in petroleum oil products |
| CN115974731A (en) * | 2022-12-02 | 2023-04-18 | 国家能源集团宁夏煤业有限责任公司 | Co-production process method and system of alpha-olefin sulfonate and alkane solvent oil |
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| CN1379076A (en) * | 2001-04-06 | 2002-11-13 | 天津开发区鑫淼工贸有限公司 | Process for preparing petroleum sulfonate dedicated for tertiary recovery of petroleum |
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