CN103304449A - Method for preparing fatty alcohol polyoxyalkylene ether sulfonate - Google Patents
Method for preparing fatty alcohol polyoxyalkylene ether sulfonate Download PDFInfo
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- CN103304449A CN103304449A CN2013102355225A CN201310235522A CN103304449A CN 103304449 A CN103304449 A CN 103304449A CN 2013102355225 A CN2013102355225 A CN 2013102355225A CN 201310235522 A CN201310235522 A CN 201310235522A CN 103304449 A CN103304449 A CN 103304449A
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- fatty alcohol
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- extraction solvent
- alcohol polyoxyethylene
- polyoxyalkylene ether
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Abstract
The invention discloses a method for preparing a novel surfactant, namely fatty alcohol polyoxyalkylene ether sulfonate applicable to tertiary oil recovery. The method comprises the step of directly sulfonating by mixing a sulfonating agent in a water phase system by taking fatty alcohol polyoxyalkylene ether sulfate as a raw material to obtain fatty alcohol polyoxyalkylene ether sulfonate. According to the method, through controlling the proportion of mixed sulfonating agent and reasonably regulating the mineralization of an aqueous solution and the acid-base property of the reaction system, the production of the side product fatty alcohol polyoxyalkylene ether in hydrolyzing raw materials can be effectively reduced, and the productivity of the target product can be improved. In addition, the fatty alcohol polyoxyalkylene ether sulfonate is extracted and purified from the reaction mixture by utilizing a proper extraction solvent, so that the purity of the product can be improved. The method is low in cost, small in pollution, high in yield, simple to operate, and convenient to realize industrialization.
Description
Technical field
The present invention relates to a kind of method that is suitable for used for tertiary oil recovery novel surfactant-aliphatic alcohol polyoxyethylene sulfonate for preparing, belong to organic compound and synthesize and separation technology field.
Background technology
The aliphatic alcohol polyoxyethylene sulfonate tensio-active agent belongs to anion-nonionic type tensio-active agent, have 2 kinds of different hydrophilic groups in the surfactant molecule, make its two-fold advantage that has possessed simultaneously nonionic and aniorfic surfactant, have good salt resistant character, dispersing property and good 5 is joined performance; The more important thing is this tensio-active agent under the extreme displacement of reservoir oil environment such as high temperature, high salinity, high contents of calcium and magnesium ion, oil water interfacial tension still can reach 10
-3～10
-4The mN/m order of magnitude.Therefore, this class tensio-active agent especially has broad application prospects in high salinity reservoirs was in field of petroleum exploitation.It is more that the pertinent literature introduction prepares the method for aliphatic alcohol polyoxyethylene sulfonate class tensio-active agent, is broadly divided into sulphite sulfonation method, the third sultone method, sulfoalkylation method, alkene additive process etc.But the problem such as that these preparation methods exist is high such as raw materials cost, productive rate is low, seriously polluted and product is not easily separated is seriously restricting its suitability for industrialized production.That main raw material is fatty alcohol polyoxyethylene ether sulfate by fatty alcohol polyoxyethylene ether sulfate through the most outstanding characteristics of operational path of sulphite Direct Sulfonation synthetic fatty alcohol polyethenoxy ether sulphonate, water is as solvent, with low cost, short and the non-environmental-pollution of flow process meets industrial requirement.But this preparation method's shortcoming is the raw material facile hydrolysis, low conversion rate, and product mixture is not easily separated behind the simultaneous reactions, and this is the bottleneck in its industrial applications process.For example patent US 005318709A does not investigate the salinity of reaction system and the acid-basicity of the aqueous solution, causes productive rate lower.Chinese patent CN 101255127A discloses a kind of method at aqueous phase synthetic fatty alcohol polyethenoxy ether sulphonate, but does not also have the conditions such as acid-basicity of the salinity of optimizing reaction system and the aqueous solution to the impact of product yield; The shortcomings such as simultaneously, product mixture adopts traditional wet distillation method, not only can produce a large amount of foams in sepn process, increases separating difficulty, and high with energy consumption, and the operational cycle is long.Chinese patent CN102070778A discloses a kind of method of utilizing the direct Synthesis aliphatic alcohol polyoxyethylene sulfonate of fatty alcohol polyoxyethylene ether sulfate in microemulsion system, although improved the transformation efficiency of raw material, but reaction system has formed microemulsion system, subsequent separation process also needs breakdown of emulsion to process, and has increased the product separation difficulty.Therefore, although fatty alcohol polyoxyethylene ether sulfate has caused widely research through the technique of sulphite Direct Sulfonation synthetic fatty alcohol polyethenoxy ether sulphonate, but not yet report at present a kind ofly can effectively solve simultaneously the raw material facile hydrolysis method of the low and product mixture separation difficulty of sulphonation rate.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing aliphatic alcohol polyoxyethylene sulfonate, overcome the defective that prior art exists.
The technical scheme that the present invention takes is such.Mix the sulphonating agent proportioning by control, regulate rational aqueous solution salinity and reaction system acid-basicity, effectively reduced the generation of raw material hydrolysising by-product fatty alcohol-polyoxyethylene ether, improved the productive rate of target product.Simultaneously, utilize suitable extraction solvent purification by liquid extraction aliphatic alcohol polyoxyethylene sulfonate from reaction mixture, improved the purity of product.Extraction solvent is reusable after reclaiming.
Concrete, a kind of method for preparing aliphatic alcohol polyoxyethylene sulfonate of the present invention, with fatty alcohol polyoxyethylene ether sulfate with mix sulphonating agent, water in mass ratio, fatty alcohol polyoxyethylene ether sulfate: mix sulphonating agent: water=1:(0.5～1.5): mix (3.5～9.8), under heating condition, react 2～6 h, take out after the cooling, obtain product mixture, at a certain temperature, product mixture adds a certain amount of extraction solvent extraction, after the phase-splitting, extraction solvent is removed in the organic phase underpressure distillation, obtain the finished product aliphatic alcohol polyoxyethylene sulfonate of content about 90%, reclaim simultaneously extraction solvent, recycling.
Among the present invention, the mixing sulphonating agent is Na
2SO
3And NaHSO
3Mixture, its fit quality is than being Na
2SO
3: NaHSO
3=(5～9): 1, guarantee aqueous phase system pH=7～8.
Among the present invention, heating condition is 160～200 ℃.
Among the present invention, extraction solvent is the mixture of extraction agent and thinner, and extraction agent is selected from C
4-C
8Alcohols, comprise its positive isomery, and a kind of in the pimelinketone, thinner is kerosene, the volume ratio of extraction agent and thinner is (1:0)～(1:2).
Among the present invention, the extraction solvent consumption is: the volume ratio of product mixture and extraction solvent is preferably 5:(1～5).
Among the present invention, extraction temperature is 50～80 ℃.
The present invention obtains following beneficial effect:
1, the present invention mixes the proportioning of sulphonating agent by control, regulates the salinity of rational water and the acid-basicity of the aqueous solution, is conducive to suppress the raw material hydrolytic side reactions, thereby improves reaction yield.
2, reaction mixture obtains the finished product aliphatic alcohol polyoxyethylene sulfonate of content about 90% after the extraction solvent purification by liquid extraction separates.
3, extraction solvent can be reused after the underpressure distillation Separation and Recovery, has avoided the waste of organic solvent, has economy.
Description of drawings
Fig. 1 is the infrared analysis spectrum of the aliphatic alcohol polyoxyethylene sulfonate for preparing of the present invention.
Among the figure, wave number is 2920～2851 cm
-1The place is the feature of chain alkyl, and wave number is 1130 cm
-1The place is the characteristic peak of C-O-C key, and wave number is 1173cm
-1, 1065 cm
-1, 619 cm
-1The place is sulfonic characteristic peak.
Embodiment
Following examples are used for explanation the present invention.
Embodiment 1
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 73 g, 400 g water, Na
2SO
348.8 g, NaHSO
37g places reactor, and reaction is 4 hours under 190～195 ℃ of conditions, takes out after being cooled to 80 ℃, obtains product mixture.Add 270ml extraction solvent (50% n-hexyl alcohol+50% kerosene) extracted products mixture, tell pure phase, underpressure distillation goes out extraction solvent, obtains finished product 48 g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 93%.
Embodiment 2
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 73 g, 400 g water, Na
2SO
348.8 g, NaHSO
37 g place reactor, and reaction is 4 hours under 190～195 ℃ of conditions, take out after being cooled to 70 ℃, obtain product mixture.Add 270ml n-hexyl alcohol extracted products mixture, tell pure phase, underpressure distillation goes out extraction agent, obtains finished product 46 g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 90%.
Embodiment 3
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 73 g, 600 g water, Na
2SO
348.8 g, NaHSO
37 g place reactor, and reaction is 4 hours under 170～180 ℃ of conditions, take out after being cooled to 80 ℃, obtain product mixture.Add 270ml pimelinketone extracted products mixture, tell organic phase, underpressure distillation goes out extraction agent, obtains finished product 43 g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 89%.
Embodiment 4
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 73 g, 400 g water, Na
2SO
360 g, NaHSO
312 g place reactor, and reaction is 6 hours under 190～195 ℃ of conditions, take out after being cooled to 50 ℃, obtain product mixture.Add 270ml extraction solvent (50% n-Octanol+50% kerosene) extracted products mixture, tell pure phase, underpressure distillation goes out extraction solvent, obtains finished product 49 g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 91%.
Embodiment 5
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 100 g, 400 g water, Na
2SO
360 g, NaHSO
312 g place reactor, and reaction is 4 hours under 190～195 ℃ of conditions, take out after being cooled to 80 ℃, obtain product mixture.Add 270ml extraction solvent (60% propyl carbinol+40% kerosene) extracted products mixture, tell pure phase, underpressure distillation goes out extraction solvent, obtains finished product 64g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 92%.
Embodiment 6
In the 1L potheater, add fatty alcohol polyoxyethylene ether sulfate (70%) 73 g, 400 g water, Na
2SO
348.8 g, NaHSO
37g places reactor, and reaction is 4 hours under 190～195 ℃ of conditions, takes out after being cooled to 80 ℃, obtains product mixture.Add 350ml isooctyl alcohol extracted products mixture, tell pure phase, underpressure distillation goes out extraction agent, obtains finished product 50 g.By two phase titrations, the content of aliphatic alcohol polyoxyethylene sulfonate is 87%.
Claims (6)
1. method for preparing aliphatic alcohol polyoxyethylene sulfonate, it is characterized in that: with fatty alcohol polyoxyethylene ether sulfate with mix sulphonating agent, water in mass ratio, fatty alcohol polyoxyethylene ether sulfate: mix sulphonating agent: water=1:(0.5～1.5): mix (3.5～9.8), under heating condition, react 2～6 h, take out after the cooling, obtain product mixture, at a certain temperature, product mixture adds a certain amount of extraction solvent extraction, after the phase-splitting, extraction solvent is removed in the organic phase underpressure distillation, obtained the finished product aliphatic alcohol polyoxyethylene sulfonate, reclaim simultaneously extraction solvent, recycling.
2. method according to claim 1, it is characterized in that mixing sulphonating agent is Na
2SO
3And NaHSO
3Mixture, its fit quality is than being Na
2SO
3: NaHSO
3=(5～9): 1, aqueous phase system pH=7～8.
3. method according to claim 1 is characterized in that heating condition is 160 ℃～200 ℃.
4. method according to claim 1, it is characterized in that: described extraction solvent is the mixture of extraction agent and thinner, and extraction agent is selected from C
4-C
8Alcohols, pimelinketone in a kind of, thinner is kerosene, the volume ratio of extraction agent and thinner is (1:0)～(1:2).
5. according to claim 1 or 4 described methods, it is characterized in that, the extraction solvent consumption is: the volume ratio of product mixture and extraction solvent is 5:(1～5).
6. according to claim 1 or 4 described methods, it is characterized in that, extraction temperature is 50～80 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4816188A (en) * | 1984-10-20 | 1989-03-28 | Lion Corporation | Process for the preparation of saturated/unsaturated mixed fatty acid ester sulfonates |
| US5318709A (en) * | 1989-06-05 | 1994-06-07 | Henkel Kommanditgesellschaft Auf Aktien | Process for the production of surfactant mixtures based on ether sulfonates and their use |
| CN101255127A (en) * | 2008-04-01 | 2008-09-03 | 江南大学 | Synthesis of aliphatic alcohol polyoxyethylene sulfonate and complex formulation used for tertiary oil recovery displacement agent |
| CN101279934A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Aliphatic acid polyethenoxy ether sulphonate and preparation thereof |
-
2013
- 2013-06-14 CN CN2013102355225A patent/CN103304449A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4816188A (en) * | 1984-10-20 | 1989-03-28 | Lion Corporation | Process for the preparation of saturated/unsaturated mixed fatty acid ester sulfonates |
| US5318709A (en) * | 1989-06-05 | 1994-06-07 | Henkel Kommanditgesellschaft Auf Aktien | Process for the production of surfactant mixtures based on ether sulfonates and their use |
| CN101279934A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Aliphatic acid polyethenoxy ether sulphonate and preparation thereof |
| CN101255127A (en) * | 2008-04-01 | 2008-09-03 | 江南大学 | Synthesis of aliphatic alcohol polyoxyethylene sulfonate and complex formulation used for tertiary oil recovery displacement agent |
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Application publication date: 20130918 |