CN103709078A - Preparation method of dioctyl sodium sulfosuccinate - Google Patents
Preparation method of dioctyl sodium sulfosuccinate Download PDFInfo
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Abstract
The invention belongs to the technical field of fine chemical production, and discloses a preparation method of dioctyl sodium sulfosuccinate. The preparation method mainly comprises the steps of an esterification stage: implementing alcoholysis reaction to isooctanol and maleic anhydride, adding a catalyst and a color fixative, implementing primary dual-esterification reaction at 115 DEG C, increasing temperature to 185-205 DEG C and carrying out reaction to generate diisooctyl maleate; and a sulfonation stage: implementing reflux reaction to diisooctyl maleate, sodium hydrogen sulfite and water, and removing residual isooctanol in a refluxing process to obtain dioctyl sodium sulfosuccinate. The preparation method disclosed by the invention is low in isooctanol addition, thus reducing raw material cost, and is free from vacuum reaction and isooctanol removal under high vacuum, so as to greatly reduce requirement on equipment; the isooctanol is removed in the sulfonation reaction, thus effectively reducing residue. The prepared dioctyl sodium sulfosuccinate is light in color, small in smell, good in wettability and low in isooctanol content.
Description
Technical field
The invention belongs to fine chemicals production technical field, be specifically related to a kind of preparation method of Aerosol OT.
Background technology
Aerosol OT is by the U.S., to be developed the earliest, and World War II just appears at tensio-active agent market with commercial form later.It is famous with high wetting power, has lower surface tension, and surfactivity, is fabulous permeate agent, wetting agent and dispersion agent preferably.Aerosol OT has a polar head and two alkyl, and itself do not need cosurfactant can form microemulsion yet, can also play that emulsification, solubilising, foaming, froth breaking, moisturizing are lubricated, a series of effects such as washing, antistatic, protection against corrosion, make it be widely used in the industries such as plastics, makeup, mining coating, papermaking, rubber, synthetic detergent, metallurgy, agricultural chemicals, oil, asbestos, building, medicine.Aerosol OT is generally dissolved in polar solvent, make certain density product, main as fabric quickly penetrating agent in printing and dyeing industry at present, the cotton of processing, fiber crops, viscose glue and blended product, can directly bleach or dye without boiling-off, both save operation, can help improve again because of dead cotton cause dye defect, after printing and dyeing, fabric feeling is also more soft and full.
The current research synthetic and application to Aerosol OT is more, as disclosed a kind of preparation method of Aerosol OT in the application number Chinese invention patent < < preparation process of diisooctyl sodium sulfosuccinate > > that is 96116865.X, the principle of this invention is that MALEIC ANHYDRIDE is reacted with isooctyl alcohol under Catalyzed by p-Toluenesulfonic Acid, obtains esterification products Maleic Acid Diisooctyl.Esterification by product is in alkali and generate the different monooctyl ester salt of maleic acid list and as the sulfonation phase-transfer catalyst of esterification products, and the sodium bisulfite of take reacts generation Aerosol OT as sulphonating agent with esterification products.
The synthesis step of Aerosol OT common method is that MALEIC ANHYDRIDE is reacted with isooctyl alcohol at present, introduces the dibasic acid esters group of oleophylic, forms Maleic Acid Diisooctyl, as shown in reaction formula (1); Carry out again sulfonation reaction and introduce hydrophilic radical, form Aerosol OT, as shown in reaction formula (2).
The subject matter that current industrial production technique exists is: for obtaining the Aerosol OT product compared with high-quality, during esterification, isooctyl alcohol charging capacity is still excessive, need to have high vacuum to take off isooctyl alcohol step, to equipment and working condition, requires high; If without de-isooctyl alcohol technique, the isooctyl alcohol residual quantity in product is difficult to again guarantee, causes pungent odour larger, can not be applied to, in low smell formula, cannot obtain the Aerosol OT product of high-quality, has limited the use range of permeate agent product.
Summary of the invention
In order to overcome the shortcoming and deficiency of prior art, primary and foremost purpose of the present invention is to provide a kind of preparation method of Aerosol OT, and this preparation method's raw materials cost is low, simple, not high to equipment requirements, product colour is shallow, smell is little, and isooctyl alcohol content is low.
Object of the present invention is achieved through the following technical solutions:
A preparation method for Aerosol OT, comprises the steps:
(1) Esterification Stage: in nitrogen atmosphere, different monooctyl ester and MALEIC ANHYDRIDE are dropped in reactor at 60 ℃～90 ℃ to alcoholysis reaction 1～2 hour, add again catalyzer and colour protecting agent, be warming up to 115 ℃ of insulation esterifications 1～3 hour, then be warming up to 185 ℃～205 ℃ insulation reaction 2～5 hours, obtain intermediate diisooctyl butenedioate;
(2) the sulfonation stage: the described diisooctyl butenedioate of step (1) is proceeded to sulfonation reaction still after filtering, adding sodium hydroxide that diisooctyl butenedioate is neutralized to acid number is 0～0.3mgKOH/g, add sodium bisulfite and water, be warming up to 110～115 ℃ and carry out back flow reaction 2～5 hours, obtain Aerosol OT.
Preferably, the mol ratio of the different monooctyl ester described in step (1) and MALEIC ANHYDRIDE is (2～2.1): 1.
Preferably, the described catalyzer of step (1) is more than one in zinc acetate, zinc oxide, sodium pyrosulfate, boric acid, oxalic acid, phosphoric acid, citric acid, load phosphotungstic acid, Witco 1298 Soft Acid, tosic acid or Dibutyltin oxide;
Preferred, the described catalyzer of step (1) is more than one in boric acid, phosphoric acid, load phosphotungstic acid, tosic acid or Dibutyltin oxide.
Preferably, the described colour protecting agent of step (1) is phosphorous acid, sodium phosphite, Hypophosporous Acid, 50 or sodium hypophosphite.
Preferably, the consumption of the described catalyzer of step (1) is 0.05%～1.5% of isooctyl alcohol and MALEIC ANHYDRIDE gross weight.
Preferably, the consumption of the described colour protecting agent of step (1) is 0.05%～1.5% of isooctyl alcohol and MALEIC ANHYDRIDE gross weight.
Preferably, in step (2), the mol ratio of diisooctyl butenedioate and sodium bisulfite is 1:(1.0～1.1).
Preferably, the water adding in step (2) accounts for sodium bisulfite and water always adds 20%～30% of weight.
In back flow reaction described in step (2), azeotrope, through condenser condenses, separates profit two-phase at backflow header tank, the lower layer of water that only refluxes, the isooctyl alcohol of the oil reservoir that do not reflux.
Principle of the present invention:
In the synthesis step of aforesaid Aerosol OT common method, in fact esterification shown in reaction formula (1) does not settle at one go, and MALEIC ANHYDRIDE is easy to occur as the hydrolysis reaction of reaction formula (3) with as the alcoholysis reaction of reaction formula (4).Therefore, some MALEIC ANHYDRIDE of Esterification Stage can first generate butene dioic acid, just with isooctyl alcohol, carries out esterification, as shown in reaction formula (5).
The alcoholysis of MALEIC ANHYDRIDE directly generates that the speed of the different monooctyl ester of butene dioic acid list is fast, and temperature requirement is low, is far superior to generate after MALEIC ANHYDRIDE hydrolysis after butene dioic acid and isooctyl alcohol esterification again.Therefore in Esterification Stage in earlier stage, suppressing the generation of water, control the amount of MALEIC ANHYDRIDE hydrolysis, is favourable to whole double esterification reaction.Production method of the present invention is decomposed into the alcoholysis reaction of catalyst-free esterification and has the esterification of catalyzer.Alcoholysis reaction mainly forms the different monooctyl ester of butene dioic acid list; Esterification is by adjusting reaction conditions, the different monooctyl ester of butene dioic acid list further being formed to diisooctyl butenedioate.
Isooctyl alcohol and water have azeotropism, in the water that reaction system evaporates, can contain a certain proportion of isooctyl alcohol.Utilize this feature, Esterification Stage isooctyl alcohol is taken water azeotropic out of, promotes esterification to carry out; Sulfonation stage water is taken isooctyl alcohol azeotropic out of, and the isooctyl alcohol that can effectively remove in material is residual.
The present invention has following advantage and effect with respect to prior art:
(1) the esterification initial stage of the present invention does not add catalyzer, reduces the generation of water, suppresses hydrolysis reaction, allow it mainly carry out alcoholysis reaction, can also prevent that the azeotropic that is heated causes isooctyl alcohol premature loss because generating after water, thereby reduced the total charging capacity of isooctyl alcohol, improved isooctyl alcohol utilization ratio.
(2) under the protection of colour protecting agent, esterification is able to carry out under the high temperature of 185 ℃～205 ℃, is difficult for occurring variable color; improved the transformation efficiency of esterification; the alcoholysis reaction of comprehensive leading portion, conversion rate of esterification is 92～98%, obtains light-colored diisooctyl butenedioate.
(3) after the minimizing of isooctyl alcohol charging capacity and utilization ratio increase make esterification complete, without high vacuum, remove isooctyl alcohol, without vacuum extractor, also can produce this product, reduced the requirement to production unit.
(4) utilize the feature of isooctyl alcohol and water azeotropic, de-isooctyl alcohol step is combined with sulfonation procedure, the isooctyl alcohol that also can effectively reduce in product without vacuum unit in the situation that is residual.The back flow reaction solid content in sulfonation stage is high, and the minimizing of water-content can improve reflux temperature, when promoting sulfonation reaction, can strengthen and reflux except alcohol effect.In Aerosol OT after sulfonation, isooctyl alcohol content is less than or equal to 0.8% mass percent.
(5) adopt method provided by the invention, without vacuum requirement, required equipment is simple, and cost is low, and producing the Aerosol OT obtain, of light color (color and luster: pt-co≤50), smell is low, wettability is good.
Accompanying drawing explanation
Fig. 1 is sulfonation reaction device schematic diagram.Wherein, 1 is sulfonation reaction still, and 2 is condenser, and 3 is backflow header tank, and 4 is backflow controlled value.
Fig. 2 is the gas chromatogram of product Aerosol OT of the present invention.
Fig. 3 is the gas chromatogram of commercially available certain company's fast penetrant T.
Fig. 4 is the infrared spectrogram of product Aerosol OT of the present invention and commercially available certain company's fast penetrant T.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
By 267Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, starts stirring, be warming up to 80 ℃ of insulations 1.5 hours, add 4Kg Dibutyltin oxide, 3Kg sodium phosphite, is warming up to 115 ℃ of insulations 1.5 hours, continue to heat up, after reaching 200 ℃, be incubated 4 hours, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtain diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 130Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 108Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.The device of sulfonation reaction as shown in Figure 1, liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 4 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
Embodiment 2
By 273Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, start stirring, be warming up to 90 ℃ of insulations 1 hour, add 3Kg boric acid, 1Kg phosphoric acid, 3Kg sodium hypophosphite, be warming up to 115 ℃ of insulations 2 hours, continue heat up, be incubated 4.5 hours after reaching 200 ℃, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtains diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 120Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 110Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 3 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
By 260Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, start stirring, be warming up to 60 ℃ of insulations 2 hours, add 0.1Kg tosic acid, 0.1Kg load phosphotungstic acid, 2Kg Hypophosporous Acid, 50, be warming up to 115 ℃ of insulations 3 hours, continue heat up, be incubated 5 hours after reaching 185 ℃, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtains diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 89Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 104.1Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 2 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
Embodiment 4
By 265Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, start stirring, be warming up to 80 ℃ of insulations 1 hour, add 1Kg oxalic acid, 0.5Kg citric acid, 1Kg zinc oxide, 5.4Kg phosphorous acid, is warming up to 115 ℃ of insulations 3 hours, continue to heat up, after reaching 205 ℃, be incubated 2.5 hours, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtain diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 111Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 105Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 5 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
Embodiment 5
By 270Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, starts stirring, be warming up to 70 ℃ of insulations 1.5 hours, add 1.4Kg boric acid, 1Kg Witco 1298 Soft Acid, 3.6Kg Hypophosporous Acid, 50 is warming up to 115 ℃ of insulations 2 hours, continue to heat up, after reaching 190 ℃, be incubated 3 hours, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtain diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 134Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 107Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 3 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
By 273Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, starts stirring, be warming up to 85 ℃ of insulations 1.5 hours, add 1Kg boric acid, 1Kg sodium hypophosphite, is warming up to 115 ℃ of insulations 1 hour, continue to heat up, after reaching 200 ℃, be incubated 2.5 hours, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtain diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 135Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 110Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 5 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
Embodiment 7
By 263Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, pass into nitrogen, start stirring, be warming up to 75 ℃ of insulations 1 hour, add 0.8Kg zinc acetate, 2Kg zinc oxide, 1Kg sodium pyrosulfate, 1Kg sodium phosphite, be warming up to 115 ℃ of insulations 3 hours, continue heat up, be incubated 5 hours after reaching 195 ℃, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtains diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 118Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 112Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 3 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
By 267Kg isooctyl alcohol, 98Kg MALEIC ANHYDRIDE drops in reaction kettle of the esterification, passes into nitrogen, start stirring, be warming up to 90 ℃ of insulations 2 hours, add 0.5Kg Dibutyltin oxide, 1Kg tosic acid, 5.5Kg phosphorous acid, be warming up to 115 ℃ of insulations 3 hours, continue heat up, be incubated 2 hours after reaching 200 ℃, material is cooled to 60 ℃, with 1 μ filter-cloth filtering, obtains diisooctyl butenedioate.
By 340Kg diisooctyl butenedioate, 136Kg water drops in sulfonation reaction still 1, starts stirring, and with sodium hydroxide, being neutralized to acid number is 0～0.3mgKOH/g, adds 114.5Kg sodium bisulfite, opens large water of condensation, is warming up to 110～115 ℃ and carries out back flow reaction.Liquidometer by backflow header tank 3 is observed through the condensed fluid total amount of condenser 2, controls the backflow controlled value 4 of bottom, only the water of backflow header tank 3 lower floors is refluxed, and the oil reservoir on upper strata contains a large amount of isooctyl alcohol, will not reflux.Back flow reaction is 4.5 hours altogether, obtains the Aerosol OT solution of homogeneous phase transparent.
Application comparative example
Aerosol OT conventionally need to be dissolved in and in solvent, obtain quickly penetrating agent product.Use the Aerosol OT that this production technique obtains to mix rear as shown in table 1 with commercially available certain company's fast penetrant T product index and penetrating quality contrast with solvent Virahol.
The physical and chemical index of table 1 product of the present invention and commercially available prod and penetrating quality contrast
| Laboratory sample | Product of the present invention | Commercially available certain company's fast penetrant T |
| Outward appearance | Achromaticity and clarification liquid | Achromaticity and clarification liquid |
| Smell | Without isooctyl alcohol smell | Without isooctyl alcohol smell |
| Color and luster (pt-co) | 3 | 3 |
| Solid content (%) | 70.05 | 71.94 |
| Actives (%) | 64.24 | 65.97 |
| Moisture (%) | 23.81 | 22.47 |
| Solvent | Virahol | Virahol |
| Surface tension (mNm -1) | 23.3748 | 24.1331 |
| Acid number (mgKOH/g) | 0.02 | 0.42 |
| Iodine number (mgl 2/g) | 0.11 | 0.05 |
| PH value (1% aqueous solution, 25 ℃) | 6.0 | 6.2 |
| Saponification value (mgKOH/g) | 175.34 | 174.74 |
| Isooctyl alcohol content (%) | 0.33 | 0.84 |
| Viscosity (mPaS) | 205 | 188 |
| Seepage force (S, 1% aqueous solution, 25 ℃) | ≤5 | ≤5 |
| Seepage force is with respect to standard substance (%) | 100±5 | 100±5 |
From table 1 correlation data, in the situation that using same solvent, solid content and actives to approach, the surface tension of product Aerosol OT of the present invention is lower, and still less, purity is higher for isooctyl alcohol content.
Product Aerosol OT of the present invention and commercially available certain company's fast penetrant T are carried out to gas chromatographic analysis, as shown in Figure 2, the gas chromatogram of commercially available certain company's fast penetrant T as shown in Figure 3 for the gas chromatogram of product Aerosol OT of the present invention.From Fig. 2 and Fig. 3, can find out, the collection of illustrative plates of two kinds of products is basically identical, and retention time is solvent at the peak of 1.1～1.4min, and retention time is object of reference propyl carbinol at the peak of about 2.12min, and retention time is isooctyl alcohol at the peak of about 5.6min.By calculating conversion, learn, the isooctyl alcohol content of product Aerosol OT of the present invention is obviously less than this commercially available prod.
Product Aerosol OT of the present invention and commercially available certain company's fast penetrant T are carried out to Infrared spectroscopy, and infrared spectrogram as shown in Figure 4, can find out from infrared spectrogram, and the main absorption peak of the collection of illustrative plates of two kinds of products is basically identical.At about 3450cm
-1place is O-H stretching vibration peak, and this is because product wetting ability is very strong, and during detection, moisture can not be completely except clean; 2960cm
-1locating strong peak is C-H stretching vibration peak, 1735cm
-1locating strong peak is the C=O stretching vibration peak of ester, 1460cm
-1place is-CH
3with the rocking vibration peak of-CH, 1380cm
-1place is-CH
3scissoring vibration peak, these several places show to have generated different monooctyl ester; 1220cm
-1near wide cut resonance peak place is that the stretching vibration coabsorption of sulfonic group vibration and a C-O-C mono-causes, 1050cm
-1place is S=O stretching vibration peak, 530cm
-1place is the charateristic avsorption band of sulfo group, and these several places show that two keys of intermediate have carried out sulfonation reaction.Collection of illustrative plates shows, two kinds of products are all Aerosol OTs.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. a preparation method for Aerosol OT, is characterized in that comprising the steps:
(1) Esterification Stage: in nitrogen atmosphere, different monooctyl ester and MALEIC ANHYDRIDE are dropped in reactor at 60 ℃～90 ℃ to alcoholysis reaction 1～2 hour, add again catalyzer and colour protecting agent, be warming up to 115 ℃ of insulation esterifications 1～3 hour, then be warming up to 185 ℃～205 ℃ insulation reaction 2～5 hours, obtain intermediate diisooctyl butenedioate;
(2) the sulfonation stage: the described diisooctyl butenedioate of step (1) is proceeded to sulfonation reaction still after filtering, adding sodium hydroxide that diisooctyl butenedioate is neutralized to acid number is 0～0.3mgKOH/g, add sodium bisulfite and water, be warming up to 110～115 ℃ and carry out back flow reaction 2～5 hours, obtain Aerosol OT.
2. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the mol ratio of the different monooctyl ester described in step (1) and MALEIC ANHYDRIDE is (2～2.1): 1.
3. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the described catalyzer of step (1) is more than one in zinc acetate, zinc oxide, sodium pyrosulfate, boric acid, oxalic acid, phosphoric acid, citric acid, load phosphotungstic acid, Witco 1298 Soft Acid, tosic acid or Dibutyltin oxide.
4. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the described catalyzer of step (1) is more than one in boric acid, phosphoric acid, load phosphotungstic acid, tosic acid or Dibutyltin oxide.
5. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the described colour protecting agent of step (1) is phosphorous acid, sodium phosphite, Hypophosporous Acid, 50 or sodium hypophosphite.
6. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the consumption of the described catalyzer of step (1) is 0.05%～1.5% of isooctyl alcohol and MALEIC ANHYDRIDE gross weight.
7. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the consumption of the described colour protecting agent of step (1) is 0.05%～1.5% of isooctyl alcohol and MALEIC ANHYDRIDE gross weight.
8. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: in step (2), the mol ratio of diisooctyl butenedioate and sodium bisulfite is 1:(1.0～1.1).
9. the preparation method of a kind of Aerosol OT according to claim 1, is characterized in that: the water adding in step (2) accounts for sodium bisulfite and water always adds 20%～30% of weight.
10. the preparation method of a kind of Aerosol OT according to claim 1, it is characterized in that: in the back flow reaction described in step (2), azeotrope, through condenser condenses, separates profit two-phase at backflow header tank, the lower layer of water that only refluxes, the isooctyl alcohol of the oil reservoir that do not reflux.
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| JP2018162446A (en) * | 2017-03-24 | 2018-10-18 | 三洋化成工業株式会社 | Method for producing surfactant composition |
| CN110467547A (en) * | 2019-09-11 | 2019-11-19 | 广州方中化工有限公司 | A kind of anhydrous succinic acid di-isooctyl sulfonate sodium and preparation method thereof |
| CN111747871A (en) * | 2020-07-31 | 2020-10-09 | 潍坊市埃里特化学有限公司 | Production process of surfactant dioctyl sodium sulfosuccinate |
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| CN116082198A (en) * | 2023-02-07 | 2023-05-09 | 河北新启元能源技术开发股份有限公司 | Synthesis method of diisooctyl succinate sodium sulfonate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313205A (en) * | 2014-11-05 | 2015-01-28 | 陕西科技大学 | Succinate sulfonated C16-C18 alcohol surfactant and preparation method thereof |
| JP2018162446A (en) * | 2017-03-24 | 2018-10-18 | 三洋化成工業株式会社 | Method for producing surfactant composition |
| CN108129359A (en) * | 2017-11-24 | 2018-06-08 | 湖北富邦科技股份有限公司 | A kind of preparation method of phosphoric acid extraction antifoaming agent |
| CN110467547A (en) * | 2019-09-11 | 2019-11-19 | 广州方中化工有限公司 | A kind of anhydrous succinic acid di-isooctyl sulfonate sodium and preparation method thereof |
| CN111747871A (en) * | 2020-07-31 | 2020-10-09 | 潍坊市埃里特化学有限公司 | Production process of surfactant dioctyl sodium sulfosuccinate |
| CN114259968A (en) * | 2022-01-10 | 2022-04-01 | 安徽森科生物科技有限公司 | Reation kettle is used in production of succinic acid diisooctyl ester sodium sulfonate |
| CN116082198A (en) * | 2023-02-07 | 2023-05-09 | 河北新启元能源技术开发股份有限公司 | Synthesis method of diisooctyl succinate sodium sulfonate |
| CN116082198B (en) * | 2023-02-07 | 2024-04-26 | 河北新启元能源技术开发股份有限公司 | Synthesis method of diisooctyl succinate sodium sulfonate |
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