CN104262212A - Method for continuously preparing 2,6-dinonyl naphthalene sulfonic acid - Google Patents
Method for continuously preparing 2,6-dinonyl naphthalene sulfonic acid Download PDFInfo
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Abstract
The invention discloses a method for continuously preparing a 2,6-dinonyl naphthalene sulfonic acid. The 2,6-dinonyl naphthalene sulfonic acid is continuously produced through a falling film sulfonation reactor, and the method comprises the specific steps: 2,6-dinonyl naphthalene and a sulfur trioxide gas are continuously introduced into the falling film sulfonation reactor to be subjected to a falling film sulfonation reaction, a sulfonation reaction product is aged, settled to separate out acid residues, extraction and separation are carried out, the separated product is concentrated, acidized, washed with water, evaporated to remove a solvent to obtain the 2,6-dinonyl naphthalene sulfonic acid. According to the method, the efficient production of the high-purity 2,6-dinonyl naphthalene sulfonic acid is realized based on the fact that the 2,6-dinonyl naphthalene is continuously sulfonated in the falling film sulfonation reactor, the process flow is short, the reaction time is short, the facility request is low, the purification of the product is easy, the cost is low, and the industrial production requirements are completely met.
Description
Technical field
The present invention relates to the method for continuous production 2,6-dinonylnaphthalene sulfonic acid, belong to fine chemicals preparation field.
Background technology
Dinonyl naphthalene sulphur, is dark-brown or brown viscous liquid, has no irritating odor, not oxidizable, nondiscoloration, good stability, is a kind of nontoxic, nonirritant, does not produce the anion surfactant of anaphylaxis.
Dinonylnaphthalene sulfonic acid has excellent physicochemical property because of it, is widely used as the siccative of baking vanish, the extraction agent of synergistic extraction in hydrometallurgy, lubricating oil, lubricating grease and lubricant additive, the auxiliary agent of dyestuff, the additive of resin.
At present, the manufacturer that China produces dinonyl naphthalene sulphur is few for counting, and be all adopt the vitriol oil of being fuming to make sulphonating agent to use pot type method manufacture dinonylnaphthalene sulfonic acid, but mainly there is following shortcoming in this production method: easily oxidizing reaction occurs in (1) production process, cause by product to increase, product is difficult to purifying; (2) in production process, equipment corrosion is serious, and cause equipment to change frequent, production cost increases; (3) produce a large amount of acid sludge in production process, these acid sludges are difficult, contaminate environment; (4) produce a large amount of acid sludge in production process to fail to find suitable method to carry out circular treatment, can not recycling utilization, add production cost; (5) vitriol oil and product are not easily separated, and the settling time is long, and postprocessing working procedures is complicated, and production efficiency is low.In view of employing pot type method utilizes oleum to make the various drawbacks of sulphonating agent, seek the Method and process of the green cleaner production of dinonyl naphthalene sulfonation reaction, become the gordian technique that dinonylnaphthalene sulfonic acid is prepared in current research exploitation synthesis.
Had the report adopting falling film reactor to prepare sulfonic acid analog anion surfactants in prior art, mention as patent 201210421926.9 and adopt falling film reactor to prepare displacement of reservoir oil sulfonate, this method sulfonation efficiency is high, simple to operate.But adopt falling film reactor sulfonation, in sulfonation process, reaction is violent, difficult control of temperature, reaction preference is poor, sulfonation side reaction is many, organic raw material cannot be carried out selectivity sulfonation and prepare highly purified single product, be all the product adopting sulfonation reactor preparation not high to sulfonated products purity requirement, as sulfonic acid analog anion surfactants etc. at present.
Summary of the invention
2 are produced in prior art, 6-dinonylnaphthalene sulfonic acid production technology exists that acid sludge amount is excessive, the settling time is long, the difficult separation of product, oleum are serious to equipment corrosion, and adopts in sulfonation reactor sulfonation process, and reaction is difficult to control, the shortcomings such as side reaction is many, and product purity is not high; The object of the invention is to be to provide one based on falling film sulfonation reactor by 2, the continuous sulfonation high yield of 6-dinonyl naphthalene prepares high purity 2, the method of 6-dinonylnaphthalene sulfonic acid, the method technical process is short, reaction times is short, low for equipment requirements, and product is purified easily, cost is low, meets demand of industrial production completely.
The invention provides a kind of continuous production 2, the method of 6-dinonylnaphthalene sulfonic acid, the method is the continuous seepage being realized 2,6-dinonylnaphthalene sulfonic acid by falling film sulfonation reactor, described falling film sulfonation inside reactor upper end is provided with uniform device, and central authorities are provided with nozzle; Described falling film sulfonation reactor outer setting two sections cooling water jecket controls the temperature in falling film sulfonation reactor; When carrying out the continuous sulfonation of 2,6-dinonyl naphthalene, between falling film sulfonation reactor wall and central nozzle, be filled with dry air continuously as protecting gas; The temperature simultaneously controlling water coolant in epimere cooling water jecket is 20 DEG C ~ 30 DEG C, and in hypomere cooling water jecket, the temperature of water coolant is 25 DEG C ~ 35 DEG C; When carrying out the continuous seepage of 2,6-dinonylnaphthalene sulfonic acid, 2,6-dinonyl naphthalene is introduced in falling film sulfonation reactor from falling film sulfonation reactor head continuously, and by after the uniform dispersion of uniform device along falling film sulfonation reactor wall be membranaceous flowing down; Simultaneously, after sulfur trioxide gas is diluted by dry air, in continuous introducing falling film sulfonation reactor, and sprayed by central nozzle, protection gas pressure effect under, sulfur trioxide gas spreads downwards along falling film sulfonation reactor wall, extends, with 2, there is sulfonation reaction in the contact of 6-dinonyl naphthalene liquid film, maintaining falling film sulfonation reactor temperature in sulfonation reaction process is 45 ~ 55 DEG C; Sulfonation reaction product draws falling film sulfonation reactor, through aging, settlement separate go out after acid sludge, after mixing liquid regulates pH to 9.5 ~ 10.5 by alkali, adopt alcohol water mixed solution extracting and separating, concentrated, obtain 2,6-dinonylnaphthalene sulfonic acid salt, after gained 2,6-dinonylnaphthalene sulfonic acid salt is acidified, obtain 2,6-dinonylnaphthalene sulfonic acid; Wherein, 2,6-dinonyl naphthalene and the sulphur trioxide speed passed in falling film sulfonation reactor maintains the mol ratio of dinonyl naphthalene and sulphur trioxide in falling film sulfonation reactor is 1:1 ~ 1.2.
The method of continuous production 2,6-dinonylnaphthalene sulfonic acid of the present invention also comprises following preferred version:
In preferred scheme, in epimere cooling water jecket, the temperature of water coolant is 20 DEG C ~ 25 DEG C, and in hypomere cooling water jecket, the temperature of water coolant is 30 DEG C ~ 35 DEG C.
In preferred scheme, in epimere cooling water jecket, the temperature of water coolant is lower than water coolant in hypomere cooling water jecket.
Maintaining falling film sulfonation reactor temperature in preferred scheme in sulfonation reaction process is 48 ~ 52 DEG C.
In preferred scheme, 2,6-dinonyl naphthalenes and the sulphur trioxide speed passed in falling film sulfonation reactor maintains the mol ratio of dinonyl naphthalene and sulphur trioxide in falling film sulfonation reactor is 1:1 ~ 1.1.
In preferred scheme, digestion time is 1.5 ~ 2.5h.
After 2,6-dinonylnaphthalene sulfonic acid salt adopt petroleum ether dissolution in preferred scheme, with below acid for adjusting pH to 1, isolate oil phase, oil phase is after washing, and evaporation sherwood oil, obtains 2,6-dinonylnaphthalene sulfonic acid.
In preferred scheme, sulphur trioxide is that oleum is heated to 145 ~ 155 DEG C, is obtained by gas stripping column air lift.
In preferred scheme, 2,6-dinonyl naphthalenes are 2,6-dinonyl naphthalenes of not diluted, or 2, the 6-dinonyl naphthalenes diluted by heptane, methylene dichloride, ethylene dichloride etc.
In preferred scheme, sulphur trioxide is diluted to concentration is 4.5wt% ~ 5.5wt%; Most preferably be 4.8wt% ~ 5.0wt%.
The mixing solutions of alcohol water mixed solution to be massfraction the be second alcohol and water of 40% ~ 60% in preferred scheme.
Reuse from falling film sulfonation reactor sulphur trioxide tail gas recycle out in preferred scheme.
In preferred scheme dry air be by air compressor air out through interior fill out the moisture eliminator of discolour silica gel after obtain, dry air divides two-way, and a road is after metering as SO
3the thinner of gas, another road enters sulfonation reactor as the shielding gas of sulfonation reaction after metering.
Falling film sulfonation reactor of the present invention is falling film sulfonation reactor conventional in prior art.
The synthetic route of 2,6-dinonylnaphthalene sulfonic acids of the present invention is as follows:
Beneficial effect of the present invention: the present invention is by the strict sulfonation reaction temperature controlling falling film sulfonation reactor, the conditions such as reacting material ratio, 2,6-dinonylnaphthalene sulfonic acid technique is prepared in the sulfonation successfully falling film sulfonation reactor being used 2,6-dinonyl naphthalene; Overcome falling film sulfonation reactor reaction difficult control of temperature, the defect of poor selectivity, and in prior art, 2,6-dinonylnaphthalene sulfonic acid production technology acid sludge amounts are excessive, the settling time is long, the difficult separation of product, oleum is to the defect such as equipment corrosion is serious.Successfully high yield obtains high purity 2,6-dinonylnaphthalene sulfonic acid product.Hinge structure, technical superiority of the present invention is:
1, can carry out continuous prodution, make sulfonation reaction obtain metastable control by control temperature of reaction and reaction raw materials concentration, the reaction times is short, and production efficiency is high, and product purity is high.
2, utilize falling film type reaction unit to carry out the sulfonation reaction of 2,6-dinonyl naphthalene, heat transfer, mass transfer effect is good, and technical process is short, and gas-liquid separation is fast, decreases the settling time, easily realizes industrialization.
3, low for equipment requirements, hinge structure greatly reduces the corrosion of oleum to equipment, maintenance of the equipment and process cost low.
4, raw material sources are wide, and utilization ratio is high, SO excessive after sulfonation reaction
3easy recovery, reusable edible, without acid sludge pollute, have cleaner production feature.
Embodiment
Below in conjunction with specific embodiment, one step description is carried out to the present invention, but protection scope of the present invention is not limited in this.
Purity in the embodiment of the present invention and comparative example is all adopted by ordinary method and analyzes chromatogram and record.The raw material adopted is all analytical pure raw material.The falling film reactor that the falling film sulfonation reactor used is routine.
Embodiment 1
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 4.82wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 22 DEG C, and hypomere jacket temperature is about 31 DEG C, and makes to maintain 50 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2h, settlement separate acid sludge; It is 9.5 that sodium hydroxide solution with 20% is neutralized to pH value; With 50% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 86.18%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 94.5%.
Embodiment 2
Heat air stripper makes 20% oleum basin to 153 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 5.0wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1.2 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 24 DEG C, and hypomere jacket temperature is about 33 DEG C, and makes to maintain 52 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2.2h, settlement separate acid sludge; It is 10 that sodium hydroxide solution with 20% is neutralized to pH value; With 40% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 88.48%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 96.15%.
Embodiment 3
Heat air stripper makes 20% oleum basin to 148 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 4.5wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1.1 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 24 DEG C, and hypomere jacket temperature is about 32 DEG C, and makes to maintain 48 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 1.8h, settlement separate acid sludge; It is 10 that sodium hydroxide solution with 20% is neutralized to pH value; With 50% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 86.48%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 93.5%.
Embodiment 4
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 4.52wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1.1 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 23 DEG C, and hypomere jacket temperature is about 32 DEG C, and makes to maintain 52 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2h, settlement separate acid sludge; It is 9.5 that sodium hydroxide solution with 20% is neutralized to pH value; With 50% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 85.01%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 92.8%.
Comparative example 1
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 8.0wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 35 DEG C, and hypomere jacket temperature is about 40 DEG C, and makes to maintain 60 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2h, settlement separate acid sludge; It is 9.5 that sodium hydroxide solution with 20% is neutralized to pH value; With 50% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 88.18%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 75.45%.
Comparative example 2
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 3.6wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 15 DEG C, and hypomere jacket temperature is about 25 DEG C, and makes to maintain 35 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2h, settlement separate acid sludge; It is 9.5 that sodium hydroxide solution with 20% is neutralized to pH value; With 50% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 60.18%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 92.5%.
Comparative example 3
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulphur trioxide being diluted to average gas concentration is 4.82wt%, by 2,6-dinonyl naphthalene: sulphur trioxide=1:1.8 (mol:mol) ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, 2,6-dinonyl naphthalene after metering, is that membrane type flows down by uniform device along the inwall of sulfonation reactor, with the SO gushed out from sulfonation reactor central nozzle
3, dry air mixture occur on the inwall of sulfonation reaction membrane-type sulfonation reaction, react to downward-extension, and avoid local superheating.Reactor exterior cooling water jacket, epimere jacket temperature is about 32 DEG C, and hypomere jacket temperature is about 45 DEG C, and makes to maintain 60 DEG C in reactor.From falling-film sulfonation reactor product mixtures out, aging 2h, settlement separate acid sludge; It is 9.5 that sodium hydroxide solution with 20% is neutralized to pH value; With 70% aqueous ethanolic solution extracting and separating unsulfonated reactant in insulation separating funnel, aqueous ethanolic solution extract layer is 2,6-dinonylnaphthalene sulfonic acid salts solution, obtains dinonylnaphthalene sulfonic acid salt product after decompression removing second alcohol and water; By dinonylnaphthalene sulfonic acid salt petroleum ether dissolution, be acidified to pH value be less than 1 with acid, point oil-yielding stratum, the free acid of water washed reservoir, then steam except sherwood oil, resistates is 2,6-dinonylnaphthalene sulfonic acid.The transformation efficiency of 2,6-dinonyl naphthalene is 90.18%, and in product, the content of 2,6-dinonylnaphthalene sulfonic acids is 81.3%.
From comparative example 1 ~ 3, when temperature of reaction is too high, or sulphur trioxide reaction density is excessive, is all unfavorable for the sulfonation reaction selectivity of 2,6-dinonyl naphthalene.Temperature of reaction is too low, or the too low then reaction conversion ratio of sulphur trioxide concentration is too low.
Claims (10)
1. the method for continuous production 2,6-dinonylnaphthalene sulfonic acid, is characterized in that, is realized the continuous seepage of 2,6-dinonylnaphthalene sulfonic acid by falling film sulfonation reactor, and described falling film sulfonation inside reactor upper end is provided with uniform device, and central authorities are provided with nozzle; Described falling film sulfonation reactor outer setting two sections cooling water jecket controls the temperature in falling film sulfonation reactor; When carrying out the continuous sulfonation of 2,6-dinonyl naphthalene, between falling film sulfonation reactor wall and central nozzle, be filled with dry air continuously as protecting gas; The temperature simultaneously controlling water coolant in epimere cooling water jecket is 20 DEG C ~ 30 DEG C, and in hypomere cooling water jecket, the temperature of water coolant is 25 DEG C ~ 35 DEG C; When carrying out the continuous seepage of 2,6-dinonylnaphthalene sulfonic acid, 2,6-dinonyl naphthalene is introduced in falling film sulfonation reactor from falling film sulfonation reactor head continuously, and by after the uniform dispersion of uniform device along falling film sulfonation reactor wall be membranaceous flowing down; Simultaneously, after sulfur trioxide gas is diluted by dry air, in continuous introducing falling film sulfonation reactor, and sprayed by central nozzle, protection gas pressure effect under, sulfur trioxide gas spreads downwards along falling film sulfonation reactor wall, extends, with 2, there is sulfonation reaction in the contact of 6-dinonyl naphthalene liquid film, maintaining falling film sulfonation reactor temperature in sulfonation reaction process is 45 ~ 55 DEG C; Sulfonation reaction product draws falling film sulfonation reactor, through aging, settlement separate go out after acid sludge, after mixing liquid regulates pH to 9.5 ~ 10.5 by alkali, adopt alcohol water mixed solution extracting and separating, concentrated, obtain 2,6-dinonylnaphthalene sulfonic acid salt, after gained 2,6-dinonylnaphthalene sulfonic acid salt is acidified, obtain 2,6-dinonylnaphthalene sulfonic acid; Wherein, 2,6-dinonyl naphthalene and the sulphur trioxide speed passed in falling film sulfonation reactor maintains the mol ratio of dinonyl naphthalene and sulphur trioxide in falling film sulfonation reactor is 1:1 ~ 1.2.
2. the method for claim 1, is characterized in that, in epimere cooling water jecket, the temperature of water coolant is 20 DEG C ~ 25 DEG C, and in hypomere cooling water jecket, the temperature of water coolant is 30 DEG C ~ 35 DEG C.
3. method as claimed in claim 1 or 2, it is characterized in that, maintaining falling film sulfonation reactor temperature in sulfonation reaction process is 48 ~ 52 DEG C.
4. the method for claim 1, is characterized in that, described digestion time is 1.5 ~ 2.5h.
5. the method for claim 1, is characterized in that, after 2,6-described dinonylnaphthalene sulfonic acid salt adopt petroleum ether dissolution, with below acid for adjusting pH to 1, isolates oil phase, and oil phase is after washing, and evaporation sherwood oil, obtains 2,6-dinonylnaphthalene sulfonic acid.
6. the method for claim 1, is characterized in that, described sulphur trioxide is that oleum is heated to 145 ~ 155 DEG C, is obtained by gas stripping column air lift.
7. the method for claim 1, is characterized in that, 2,6-described dinonyl naphthalenes are 2,6-dinonyl naphthalenes of not diluted, or 2, the 6-dinonyl naphthalenes diluted by heptane, methylene dichloride, ethylene dichloride etc.
8. the method for claim 1, is characterized in that, it is 4.5wt% ~ 5.5wt% that described sulphur trioxide is diluted to concentration.
9. the method for claim 1, is characterized in that, the mixing solutions of described alcohol water mixed solution to be massfraction the be second alcohol and water of 40% ~ 60%.
10. the method for claim 1, is characterized in that, reuses from falling film sulfonation reactor sulphur trioxide tail gas recycle out.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302316A (en) * | 2020-03-05 | 2020-06-19 | 中国日用化学研究院有限公司 | Method and device for continuously preparing sulfamic acid |
| CN111836799A (en) * | 2018-02-14 | 2020-10-27 | 阿科玛法国公司 | Industrial method for continuous synthesis of alkane sulfonic acid |
| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
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| US3075005A (en) * | 1959-10-05 | 1963-01-22 | Continental Oil Co | Production of dinonylnaphthalene sulfonates |
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| US3075005A (en) * | 1959-10-05 | 1963-01-22 | Continental Oil Co | Production of dinonylnaphthalene sulfonates |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111836799A (en) * | 2018-02-14 | 2020-10-27 | 阿科玛法国公司 | Industrial method for continuous synthesis of alkane sulfonic acid |
| CN111302316A (en) * | 2020-03-05 | 2020-06-19 | 中国日用化学研究院有限公司 | Method and device for continuously preparing sulfamic acid |
| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
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