CN104262212B - Continuous production 2, the method for 6-dinonylnaphthalene sulfonic acid - Google Patents
Continuous production 2, the method for 6-dinonylnaphthalene sulfonic acid Download PDFInfo
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Abstract
The invention discloses a kind of continuous production 2, the method of 6-dinonylnaphthalene sulfonic acid, the method is to realize the continuous production of 2,6-dinonylnaphthalene sulfonic acid by falling film sulfonation reactor, by 2,6-dinonyl naphthalene and sulfur trioxide gas carry out falling film sulfonation reaction by passing into continuously in falling film sulfonation reactor, sulfonating reaction product goes out after acid sludge through aging, sedimentation separation, and extract and separate separates afterproduct after concentrated, acidifying, washing, steaming desolventize, obtain 2,6-dinonylnaphthalene sulfonic acid; The method is based on the continuous sulfonation 2 of falling film sulfonation reactor, 6-dinonyl naphthalene is realized high-purity 2,6-dinonylnaphthalene sulfonic acid high efficiency production, and it is easy that technological process is short, the reaction time is short, low for equipment requirements, product is purified, cost is low, meets demand of industrial production completely.
Description
Technical field
The present invention relates to continuous production 2, the method for 6-dinonylnaphthalene sulfonic acid, belongs to fine chemicals preparation field.
Background technology
Dinonyl naphthalene sulphur, for dark-brown or brown viscous liquid, has no irritating odor, not oxidizable, nondiscolouring,Good stability, is a kind of nontoxic, nonirritant, does not produce the anion surfactant of allergic reaction.
Dinonylnaphthalene sulfonic acid, because it has good physicochemical property, is widely used as the drier of baking vanish, hydrometallurgyThe extractant of middle synergic solvent extraction, lubricating oil, lubricating grease and lubricant additive, the auxiliary agent of dyestuff, resinAdditive.
At present, China produces the manufacturer of dinonyl naphthalene sulphur for counting seldom, and is all to adopt the concentrated sulfuric acid of being fuming to doSulfonating agent uses pot type method manufacture dinonylnaphthalene sulfonic acid, but this production method mainly exists following shortcoming:(1) oxidation reaction easily occurs in production process, cause accessory substance to increase, product is difficult to purifying; (2) produceIn process, equipment corrosion is serious, causes equipment to change frequent, and production cost increases; (3) in production process, produceA large amount of acid sludges, these acid sludges are difficult, contaminated environment; (4) in production process, producing a large amount of acid sludges fails to findSuitable method is carried out circular treatment, can not recycling utilization, increase production cost; (5) concentrated sulfuric acid withProduct is not easily separated, and the sedimentation time is long, postprocessing working procedures complexity, and production efficiency is low. In view of adopting pot type method profitMake the various drawbacks of sulfonating agent with oleum, seek the method for the green cleaner production of dinonyl naphthalene sulfonating reactionAnd technique, become the synthetic key technology of preparing dinonylnaphthalene sulfonic acid of current research exploitation.
In prior art, there is the report that adopts falling film reactor to prepare sulfonic acid analog anion surfactants, asPatent 201210421926.9 is mentioned and is adopted falling film reactor to prepare displacement of reservoir oil sulfonate, this method sulfonation efficiencyHeight, simple to operate. But adopt falling film reactor sulfonation, in sulfonation process, acutely, temperature is difficult to control in reactionSystem, reaction selectivity is poor, and sulfonation side reaction is many, Organic Ingredients cannot be carried out to selective sulfonation and prepare high-puritySingle product, is all at present to adopt the sulfonation reactor preparation product not high to sulfonated products purity requirement, asSulfonic acid analog anion surfactants etc.
Summary of the invention
Have for producing 2,6-dinonylnaphthalene sulfonic acid production technology in prior art that acid sludge amount is excessive, the sedimentation timeLength, the difficult separation of product, oleum are serious to equipment corrosion, and adopt in sulfonation reactor sulfonation process,The shortcomings such as reaction is difficult to control, and side reaction is many, and product purity is not high; The object of the invention is to be to provide a kind ofBased on falling film sulfonation reactor, continuous 2,6-dinonyl naphthalene sulfonation high yield is prepared to high-purity 2,6-dinonyl naphthaleneThe method of sulfonic acid, the method technological process is short, and the reaction time 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 for 6-dinonylnaphthalene sulfonic acid, the method is to pass through falling film typeSulfonation reactor is realized the continuous production of 2,6-dinonylnaphthalene sulfonic acid, on described falling film sulfonation inside reactorEnd is provided with uniform device, and central authorities are provided with nozzle; Described falling film sulfonation reactor outer setting two sections are coolingWater leg is controlled the temperature in falling film sulfonation reactor; While carrying out the continuous sulfonation of 2,6-dinonyl naphthalene,Between falling film sulfonation reactor wall and central nozzle, be filled with continuously dry air as protection gas; Control simultaneouslyIn epimere cooling water jecket, the temperature of cooling water is 20 DEG C～30 DEG C, the temperature of cooling water in hypomere cooling water jecketIt is 25 DEG C～35 DEG C; While carrying out the continuous production of 2,6-dinonylnaphthalene sulfonic acid, by 2,6-dinonyl naphthalene continuously from fallingIntroduce in falling film sulfonation reactor at film sulfonation reactor top, and by after the uniform dispersion of uniform device along fallingFilm sulfonation reactor inwall is membranaceous and flows down; Meanwhile, after sulfur trioxide gas dilutes by dry air, connectContinuous introducing in falling film sulfonation reactor, and spraying by central nozzle, protection gas pressure-acting under,Sulfur trioxide gas spreads downwards, extends along falling film sulfonation reactor wall, with 2,6-dinonyl naphthalene liquid filmThere is sulfonating reaction in contact, in sulfonating reaction process, maintaining falling film sulfonation reactor temperature is 45～55 DEG C;Sulfonating reaction product is drawn falling film sulfonation reactor, goes out after acid sludge through aging, sedimentation separation, and mixing material is logicalCross alkali and regulate behind pH to 9.5～10.5, adopt alcohol water mixed solution extract and separate, concentrated, obtain bis-ninth of the ten Heavenly Stems of 2,6-Base naphthalene sulfonate, gained 2, after 6-dinonylnaphthalene sulfonic acid salt is acidified, obtains 2,6-dinonylnaphthalene sulfonic acid; ItsIn, 2,6-dinonyl naphthalene and sulfur trioxide pass into speed in falling film sulfonation reactor to maintain falling film sulfonation anti-Answering the mol ratio of the interior dinonyl naphthalene of device and sulfur trioxide is 1:1～1.2.
Continuous production 2 of the present invention, the method for 6-dinonylnaphthalene sulfonic acid also comprises following preferred version:
In preferred scheme, in epimere cooling water jecket, the temperature of cooling water is 20 DEG C～25 DEG C, hypomere cooling water folderIn cover, the temperature of cooling water is 30 DEG C～35 DEG C.
In preferred scheme in epimere cooling water jecket the temperature of cooling water than cooling in hypomere cooling water jecketWater is low.
In preferred scheme, in sulfonating reaction process, maintaining falling film sulfonation reactor temperature is 48～52 DEG C.
In preferred scheme 2,6-dinonyl naphthalene and sulfur trioxide pass into the speed dimension in falling film sulfonation reactorThe mol ratio of holding the interior dinonyl naphthalene of falling film sulfonation reactor and sulfur trioxide is 1:1～1.1.
In preferred scheme, ageing time is 1.5～2.5h.
In preferred scheme 2,6-dinonylnaphthalene sulfonic acid salt adopts after petroleum ether dissolution, with acid for adjusting pH to 1 withUnder, isolate oil phase, oil phase is after washing, and evaporation benzinum, obtains 2,6-dinonylnaphthalene sulfonic acid.
In preferred scheme, sulfur trioxide is that oleum is heated to 145～155 DEG C, obtains by stripping tower air liftArrive.
In preferred scheme 2,6-dinonyl naphthalene is not diluted 2,6-dinonyl naphthalene, or by heptane, two2 of the dilution such as chloromethanes, dichloroethanes, 6-dinonyl naphthalene.
In preferred scheme, to be diluted to concentration be 4.5wt%～5.5wt% to sulfur trioxide; Most preferably be 4.8wt%～5.0wt％。
In preferred scheme, alcohol water mixed solution is that mass fraction is that the mixing of 40%～60% second alcohol and water is moltenLiquid.
In preferred scheme, reuse from falling film sulfonation reactor sulfur trioxide tail gas recycle out.
In preferred scheme, dry air is in air compressor air process out, to fill out the dry of discolour silica gelAfter dry device, obtain, dry air divides two-way, and a road is after metering as SO3The diluent of gas, another road warpProtective gas as sulfonating reaction after metering enters sulfonation reactor.
Falling film sulfonation reactor of the present invention is falling film sulfonation reactor conventional in prior art.
Of the present invention 2, the synthetic route of 6-dinonylnaphthalene sulfonic acid is as follows:
Beneficial effect of the present invention: the present invention is by the strict sulfonating reaction temperature of controlling falling film sulfonation reactorDegree, the conditions such as reacting material ratio, successfully use falling film sulfonation reactor the sulfonation of 2,6-dinonyl naphthalenePreparation 2,6-dinonylnaphthalene sulfonic acid technique; 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 amount is excessive, sedimentationLong, the difficult separation of product of time, oleum are to the defect such as equipment corrosion is serious. Successfully high yield obtains high-purityDegree 2,6-dinonylnaphthalene sulfonic acid product. Prior art relatively, technical advantage of the present invention is:
1, can carry out serialization production, by controlling reaction temperature and reaction raw materials concentration, sulfonating reaction be obtainedTo metastable control, the reaction time is short, and production efficiency is high, and product purity is high.
2, utilize falling film type reaction unit to carry out the sulfonating reaction of 2,6-dinonyl naphthalene, conduct heat, mass transfer effect is good,Technological process is short, and gas-liquid separation is fast, has reduced the sedimentation time, easily realizes industrialization.
3, low for equipment requirements, prior art has greatly reduced the corrosion of oleum to equipment, equipment relativelyMaintenance and operation expense is low.
4, raw material sources are wide, and utilization rate is high, excessive SO after sulfonating reaction3Easily reclaim, reusable edible,Without acid sludge pollute, have cleaner production feature.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is carried out to a step description, but protection scope of the present invention not only forIn this.
Purity in the embodiment of the present invention and comparative example all adopts analysis chromatogram to record by conventional method. AdoptWith raw material be all analyze pure raw material. The falling film sulfonation reactor using is conventional falling film reactor.
Embodiment 1
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 4.82wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1 (mol:mol) ratioExample, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, passes throughUniform device is membrane type along the inwall of sulfonation reactor and flows down, and gushes out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 22 DEG C of left and right, hypomere chuckTemperature is 31 DEG C of left and right, and makes to maintain 50 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 9.5; ProtectingIn temperature separatory funnel, with 50% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 86.18%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 94.5%.
Embodiment 2
Heat air stripper makes 20% oleum basin to 153 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 5.0wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1.2 (mol:mol) ratioExample, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, passes throughUniform device is membrane type along the inwall of sulfonation reactor and flows down, and gushes out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 24 DEG C of left and right, hypomere chuckTemperature is 33 DEG C of left and right, and makes to maintain 52 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2.2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 10; ProtectingIn temperature separatory funnel, with 40% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 88.48%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 96.15%.
Embodiment 3
Heat air stripper makes 20% oleum basin to 148 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 4.5wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1.1 (mol:mol) ratioExample, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, passes throughUniform device is membrane type along the inwall of sulfonation reactor and flows down, and gushes out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 24 DEG C of left and right, hypomere chuckTemperature is 32 DEG C of left and right, and makes to maintain 48 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 1.8h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 10; ProtectingIn temperature separatory funnel, with 50% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 86.48%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 93.5%.
Embodiment 4
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 4.52wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1.1 (mol:mol)Ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, logicalCross uniform device and be membrane type along the inwall of sulfonation reactor and flow down, and gush out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 23 DEG C of left and right, hypomere chuckTemperature is 32 DEG C of left and right, and makes to maintain 52 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 9.5; ProtectingIn temperature separatory funnel, with 50% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 85.01%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 92.8%.
Comparative example 1
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 8.0wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1 (mol:mol) ratioExample, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, passes throughUniform device is membrane type along the inwall of sulfonation reactor and flows down, and gushes out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 35 DEG C of left and right, hypomere chuckTemperature is 40 DEG C of left and right, and makes to maintain 60 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 9.5; ProtectingIn temperature separatory funnel, with 50% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 88.18%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 75.45%.
Comparative example 2
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 3.6wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1 (mol:mol) ratioExample, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, passes throughUniform device is membrane type along the inwall of sulfonation reactor and flows down, and gushes out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 15 DEG C of left and right, hypomere chuckTemperature is 25 DEG C of left and right, and makes to maintain 35 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 9.5; ProtectingIn temperature separatory funnel, with 50% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 60.18%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 92.5%.
Comparative example 3
Heat air stripper makes 20% oleum basin to 150 ± 2 DEG C, with dried air, sulfur trioxide is rareRelease to average gas concentration be 4.82wt%, by 2,6-dinonyl naphthalene: sulfur trioxide=1:1.8 (mol:mol)Ratio, introduces falling film sulfonation reactor upper end by 2,6-dinonyl naphthalene, and 2,6-dinonyl naphthalene after metering, logicalCross uniform device and be membrane type along the inwall of sulfonation reactor and flow down, and gush out from sulfonation reactor central nozzleSO3, on the inwall of sulfonating reaction, there is membrane-type sulfonation reaction in dry air mixture, reaction is to downward-extension,And avoid hot-spot. Reactor external refrigeration water leg, epimere jacket temperature is 32 DEG C of left and right, hypomere chuckTemperature is 45 DEG C of left and right, and makes to maintain 60 DEG C in reactor. Mix from falling liquid film sulfonation reactor product outThing, aging 2h, sedimentation separation acid sludge; Being neutralized to pH value with 20% sodium hydroxide solution is 9.5; ProtectingIn temperature separatory funnel, with 70% ethanol water extract and separate unsulfonated reactant, ethanol water extract layer is2,6-dinonylnaphthalene sulfonic acid salting liquid, obtains dinonylnaphthalene sulfonic acid salt product after second alcohol and water is removed in decompression; By twoNonylnaphthalene sulfonates petroleum ether dissolution, is acidified to pH value with acid and is less than 1, point oil-yielding stratum, washing oil reservoirFree acid, then steam except benzinum, residue is 2,6-dinonylnaphthalene sulfonic acid. The conversion ratio of 2,6-dinonyl naphthaleneBe 90.18%, in product 2, the content of 6-dinonylnaphthalene sulfonic acid is 81.3%.
From comparative example 1～3, too high when reaction temperature, or sulfur trioxide reaction density is excessive, notThe sulfonating reaction that is beneficial to 2,6-dinonyl naphthalene is selective. Reaction temperature is too low, or sulfur trioxide concentration is too low anti-Answer conversion ratio too low.
Claims (8)
1. continuous production 2, the method for 6-dinonylnaphthalene sulfonic acid, is characterized in that, real by falling film sulfonation reactorThe continuous production of existing 2,6-dinonylnaphthalene sulfonic acid, described falling film sulfonation inside reactor upper end is provided with uniformDevice, central authorities are provided with nozzle; Described falling film sulfonation reactor outer setting two sections cooling water jecket is controlledTemperature in falling film sulfonation reactor processed; While carrying out the continuous sulfonation of 2,6-dinonyl naphthalene, at falling film sulfonationDry air is filled with continuously as protection gas between reactor wall and central nozzle; Control epimere cooling water simultaneouslyIn chuck, the temperature of cooling water is 20 DEG C ~ 25 DEG C, in hypomere cooling water jecket the temperature of cooling water be 30 DEG C ~35 DEG C; When carrying out the continuous seepage of 2,6-dinonylnaphthalene sulfonic acid, by 2,6-dinonyl naphthalene continuously from falling film sulfonationReactor head is introduced in falling film sulfonation reactor, and by after the uniform dispersion of uniform device along falling film sulfonationReactor wall flows down in membranaceous; Meanwhile, after sulfur trioxide gas is diluted by dry air, introduce and fall continuouslyIn film sulfonation reactor, and sprayed by central nozzle, under the pressure effect of protection gas, sulfur trioxide gasBody spreads downwards along falling film sulfonation reactor wall, extends, and with the contact of 2,6-dinonyl naphthalene liquid film, sulphur occursChange reaction, in sulfonating reaction process, maintaining falling film sulfonation reactor temperature is 48 ~ 52 DEG C; Sulfonating reaction is producedThing is drawn falling film sulfonation reactor, and after aging, sedimentation separation go out acid sludge, mixing material is regulated by alkaliBehind pH to 9.5 ~ 10.5, adopt alcohol water mixed solution extract and separate, concentrated, obtain 2,6-dinonylnaphthalene sulfonic acidSalt, gained 2, after 6-dinonylnaphthalene sulfonic acid salt is acidified, obtains 2,6-dinonylnaphthalene sulfonic acid; Wherein, 2,6-The speed that dinonyl naphthalene and sulfur trioxide pass in falling film sulfonation reactor maintains in falling film sulfonation reactorThe mol ratio of dinonyl naphthalene and sulfur trioxide is 1:1 ~ 1.2.
2. the method for claim 1, is characterized in that, described ageing time is 1.5～2.5h.
3. the method for claim 1, is characterized in that, described 2, and 6-dinonylnaphthalene sulfonic acid salt adopts stoneAfter oil ether dissolves, with below acid for adjusting pH to 1, isolate oil phase, oil phase, after washing, evaporates benzinum,Obtain 2,6-dinonylnaphthalene sulfonic acid.
4. the method for claim 1, is characterized in that, described sulfur trioxide is that oleum is heatedTo 145～155 DEG C, obtain by stripping tower air lift.
5. the method for claim 1, is characterized in that, described 2, and 6-dinonyl naphthalene is not diluted2,6-dinonyl naphthalene, or by 2 of heptane, carrene or dichloroethanes dilution, 6-dinonyl naphthalene.
6. the method for claim 1, is characterized in that, described sulfur trioxide is diluted to concentration and is 4.5wt％～5.5wt％。
7. the method for claim 1, is characterized in that, described alcohol water mixed solution is that mass fraction isThe mixed solution of 40%～60% second alcohol and water.
8. the method for claim 1, is characterized in that, from three oxidations out of falling film sulfonation reactorSulphur tail gas recycle is reused.
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| CN111302316B (en) * | 2020-03-05 | 2023-01-31 | 中国日用化学研究院有限公司 | Method and device for continuously preparing sulfamic acid |
| CN112694422B (en) * | 2021-01-14 | 2023-01-31 | 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3075005A (en) * | 1959-10-05 | 1963-01-22 | Continental Oil Co | Production of dinonylnaphthalene sulfonates |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3075005A (en) * | 1959-10-05 | 1963-01-22 | Continental Oil Co | Production of dinonylnaphthalene sulfonates |
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| Title |
|---|
| α-萘磺酸的合成;李慧芳 等;《印染助剂》;20130831;第30卷(第8期);摘要，第17页第1段，第18页左栏倒数第8行至倒数第5行 * |
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