CN102850554A - Vegetable fiber surfactant and compound surfactant - Google Patents
Vegetable fiber surfactant and compound surfactant Download PDFInfo
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- CN102850554A CN102850554A CN2012103160022A CN201210316002A CN102850554A CN 102850554 A CN102850554 A CN 102850554A CN 2012103160022 A CN2012103160022 A CN 2012103160022A CN 201210316002 A CN201210316002 A CN 201210316002A CN 102850554 A CN102850554 A CN 102850554A
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- tensio
- active agent
- vegetable fibre
- surfactant
- compound surfactant
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Abstract
The invention discloses a vegetable fiber surfactant and a compound surfactant. The vegetable fiber surfactant is obtained after sulphating of vegetable fiber; the compound surfactant is obtained by compounding the vegetable fiber surfactant with a micro-molecular surfactant, and the micro-molecular surfactant is sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, Tween or Span. According to the invention, a polymer surfactant is prepared through a chemical reaction of a natural polymer (vegetable fiber), and such a method is simple and convenient and has the main advantage that the used natural polymer (vegetable fiber) is a ready-made, cheap, easily available and environment friendly material. Furthermore, the compound surfactant provided by the invention has a synergistic effect and a surface tension of less than 30.0 mN/m and has a thickening effect and rotary viscosity of 2.0 to 10.0 mPa.s, so the compound surfactant has application potential in improvement of oil recovery efficiency and in the daily-use chemical industry.
Description
Technical field
The invention belongs to the vegetable fibre Application Areas, be specifically related to a kind of vegetable fibre tensio-active agent, and the compound surfactant that is prepared by this vegetable fibre tensio-active agent.
Background technology
21 century, environmental issue is extensively paid close attention to by people.Vegetable fibre is the abundantest natural reproducible macromolecular material of occurring in nature, and its year growth total amount is up to the more than one hundred billion ton, considerably beyond existing petroleum total reserve on the earth.In today that petroleum resources day by day lack, fully use the vegetable fibre resource, bring into play function and the characteristic of this unique resource, widen its Application Areas, be one of study hotspot of current industry.This wherein, the preparation of vegetable fibre tensio-active agent and composite is exploitation and the effective way of using the vegetable fibre resource.
Tensio-active agent is the important organic compound of a class, and its structure contains hydrophilic group and hydrophobic group, and its Application Areas spreads all over the various fields such as chemical industry, light industry, oil, food-processing, medicine, agricultural, textile printing and dyeing and mechanical workout.
At present, small molecules tensio-active agent price, and general non-biodegradation affect soil and water system after using.In recent years, polymeric surface active agent has caused widely attention.Polymeric surface active agent refers to relative molecular weight more than thousands of, has the macromolecular compound of surface active function.Compare with the small molecules tensio-active agent, it is generally outstanding that polymeric surface active agent reduces capillary ability, but thickening property, dispersiveness, flocculence etc. obviously are better than the small molecules tensio-active agent.
Summary of the invention
The small molecules tensio-active agent is expensive in order to overcome, the defective of hard degradation, and primary and foremost purpose of the present invention is to provide a kind of preparation method of vegetable fibre tensio-active agent.
Another object of the present invention is to provide the vegetable fibre tensio-active agent by the aforesaid method preparation, this vegetable fibre tensio-active agent is water miscible polymeric surface active agent, raw material sources are abundant, and be natural, can overcome effectively that the small molecules tensio-active agent is expensive, the defective of hard degradation.
The defectives such as simple employing small molecules tensio-active agent is expensive in order to overcome, hard degradation, surface tension is large, thickening effectiveness is bad, a further object of the present invention is to provide the compound surfactant that is prepared by above-mentioned vegetable fibre tensio-active agent.
The 4th purpose of the present invention is to provide the purposes by above-mentioned compound surfactant.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of vegetable fibre tensio-active agent may further comprise the steps:
Get vegetable fibre, soak 10-36h with organic solvent; Then drip sulphoating agent, stirring reaction 0.5 ~ 5.0h under the room temperature, then the pH value with reaction system is adjusted to neutrality, with filter residue and drying, obtains the vegetable fibre tensio-active agent after the filtration.
Described vegetable fibre is 1g:(1.2-1.8 with the ratio of the consumption of sulphoating agent) ml.
Described vegetable fibre is a kind of in bagasse, corn stalk, bamboo powder, pine powder, fiber crops, cotton or the sorghum stalk; Described vegetable fibre, dry before using, then be crushed to 60 ~ 150 orders.
Described organic solvent is a kind of in sherwood oil, toluene, dimethylbenzene or the hexane.
Described sulphoating agent is a kind of in the vitriol oil, oleum, sulphur trioxide or the chlorsulfonic acid;
The mass concentration of the described vitriol oil is 98%; Described oleum is with SO
3Massfraction calculate, be that (20 acid are in sulfuric acid, and sulfur trioxide content is 20% in 20 acid; ), 25 acid (25 acid are in sulfuric acid, and sulfur trioxide content is 25%); Or 30 acid (30 acid are in sulfuric acid, and sulfur trioxide content is 30%; ).
Described sulphoating agent will be used solvent cut before use; During dilution, the volume ratio of sulphoating agent and solvent is 1:(0.8-1.3);
Described solvent is more than one in sherwood oil, toluene, dimethylbenzene or the hexane.
It is to regulate with alkaline solution that described pH value with reaction system is adjusted to neutrality; Described alkaline solution is NaOH, KOH, NaHCO
3, K
2CO
3Or Na
2CO
3Solution.
Described dropping is to finish in 10 ~ 60min; Described drying is at 105 ℃ of lower dry 1.0 ~ 3.0h.
By the vegetable fibre tensio-active agent that aforesaid method prepares, when its mass concentration was 0.05 ~ 5.00%, surface tension was 40.0 ~ 65.0mN/m.
A kind of compound surfactant is by obtaining behind above-mentioned vegetable fibre tensio-active agent and the small molecules surfactant compound; Preferably, contain 0.05 ~ 5.00% vegetable fibre tensio-active agent and 0.05 ~ 5.00% small molecules tensio-active agent in the described compound surfactant, surplus is water; Described concentration is mass concentration.
Described small molecules tensio-active agent is sodium lauryl sulphate (SDS), Sodium dodecylbenzene sulfonate (LDS), tween or class of department; Above-mentioned tween surfactants is a kind of in polysorbas20, polysorbate40 or the polysorbate60 etc.
Above-mentioned compound surfactant, when containing the small molecules tensio-active agent of 0.05 ~ 5.00% vegetable fibre tensio-active agent and 0.05 ~ 5.00%, surface tension is 25.0 ~ 30.0mN/m, has the surface tension of reduction effect; Rotary viscosity is 2.0 ~ 10.0mPas, and thickening effectiveness is arranged; Described concentration is mass concentration.
Above-mentioned compound surfactant can be applicable to the fields such as oil recovery and daily-use chemical industry.
Principle of the present invention is:
Vegetable fibre is water insoluble, without surfactivity.Simple small molecules tensio-active agent cost is high, non-degradable, and raw material is petroleum chemicals, polluted source and soil etc.The present invention processes the vegetable fibre sulphating, can obtain the water-soluble polymer tensio-active agent; With itself and small molecules surfactant compound, can obtain the lower capillary compound surfactant of having of synergistic effect.This compound surfactant not only has the performances such as thickening, dispersion, protective colloid, also have biodegradable, use the advantages such as safety and reserves are abundant.
The present invention has following advantage and effect with respect to prior art:
1, the present invention utilizes the chemical reaction of natural polymer (vegetable fibre) to produce polymeric surface active agent, be a kind of comparatively easy method, major advantage is that the natural polymer (vegetable fibre) that adopts is environment-friendly material ready-made, cheap and easy to get.
2, compound surfactant of the present invention has synergistic effect, and surface tension can be below 30.0mN/m; And having thickening effectiveness, rotary viscosity makes it aspect raising oil recovery and the daily-use chemical industry application potential arranged at 2.0 ~ 10.0mPas.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited to this.
In following examples, the surface tension of tensio-active agent and the testing method of rotary viscosity are as follows:
Surface tension: surfactant dissolves in water, is made into the sample of different mass concentration, on the BZY-1 surface tension instrument, measures surface tension at 25 ℃.
Rotary viscosity: surfactant dissolves in water, is made into the sample of different mass concentration, on the NDJ-1A rotary viscometer, measures rotary viscosity at 25 ℃.
Embodiment 1
A kind of vegetable fibre tensio-active agent is prepared by following steps:
The bagasse of 130.0g is crushed to 80 orders behind 105 ℃ of dry 2h, add the 200ml sherwood oil, placement is spent the night, and then drips the sulphoating agent (the 200ml hexane mixes with 98% vitriol oil of 200ml) of 400ml dilution, drips and finishes in 30min, under the room temperature behind the stirring reaction 2.0h, the pH value of conditioned reaction system is filtered to neutral, and filter residue is in 105 ℃ of dry 1.5h, obtain vegetable fibre tensio-active agent 513.0g, i.e. the bagasse sulfuric ester.
Gained bagasse sulfuric ester is made into the aqueous solution, and surface tension was 54.8mN/m when mass concentration was 1.00%; Surface tension was 53.3mN/m when mass concentration was 0.50%, and rotary viscosity is 2.0mPas.
Compound surfactant is prepared by following steps:
Above-mentioned bagasse sulfuric ester is mixed with sodium lauryl sulphate (SDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of bagasse sulfuric ester is the mass concentration of 0.12%, SDS when being 0.12%, and surface tension is 29.7mN/m, and rotary viscosity is 8.0mPas.
Above-mentioned bagasse sulfuric ester is mixed with Sodium dodecylbenzene sulfonate (LDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of bagasse sulfuric ester is 0.12%, and when the mass concentration of Sodium dodecylbenzene sulfonate (LDS) was 0.12%, surface tension 27.5mN/m, rotary viscosity were 5.0mPas.
Embodiment 2
A kind of vegetable fibre tensio-active agent is prepared by following steps:
26.0 gram pine powders at 105 ℃ of dry 2h, then are crushed to 100 orders, add 40.0ml toluene, placement is spent the night; With 30.0ml oleum (SO
3Mass content be 20%) with being added drop-wise to after the 40ml dilution with toluene in the pine powder mixture, dropping is finished in 60min, under the room temperature behind the stirring reaction 1.0h, the pH value of conditioned reaction system is to neutral, filter, 105 ℃ of dry 2.0h obtain vegetable fibre tensio-active agent 80.0g, i.e. the pine sulfuric ester.
When the aqueous solution mass concentration of gained pine sulfuric ester was 1.00%, surface tension was 47.8mN/m; When mass concentration was 0.50%, surface tension was 46.9mN/m, and rotary viscosity is 2.5mPas.
Compound surfactant is prepared by following steps:
Above-mentioned pine powder sulfuric ester is mixed with sodium lauryl sulphate (SDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of pine powder sulfuric ester is the mass concentration of 0.12%, SDS when being 0.12%, and surface tension is 28.8mN/m, and rotary viscosity is 4.5mPas.
Above-mentioned pine powder sulfuric ester is mixed with polysorbate60, water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of pine powder sulfuric ester is 0.12%, and when the mass concentration of polysorbate60 was 0.12%, surface tension 28.2mN/m, rotary viscosity were 8.0mPas.
Embodiment 3
A kind of vegetable fibre tensio-active agent is prepared by following steps:
The cotton of 260.0 grams in 105 ℃ of dry 2h, then is crushed to 150 orders, adds the 400ml hexane, soaked overnight; The sulphoating agent of 800ml dilution (be that 98% the vitriol oil be mixed to get by 200 sherwood oils, 200ml hexane and 400ml mass concentration) is added drop-wise in the said mixture, dropping is finished in 10min, under the room temperature behind the stirring reaction 3.5h, the pH value of conditioned reaction system is to neutral, filter, 105 ℃ of dry 1.5h obtain vegetable fibre tensio-active agent 836.7g, i.e. cotton sulfuric ester.
When the aqueous solution mass concentration of the cotton sulfuric ester of gained is 3.23%, be 55.0mN/m during surface tension; Surface tension was 57.0mN/m when mass concentration was 1.62%, and rotary viscosity is 2.5mPas.
A kind of compound surfactant is prepared by following steps:
Above-mentioned cotton sulfuric ester is mixed with sodium lauryl sulphate (SDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of cotton sulfuric ester is the mass concentration of 0.12%, SDS when being 0.12%, and surface tension is 27.4mN/m, and rotary viscosity is 6.0mPas.
Embodiment 4
A kind of vegetable fibre tensio-active agent is prepared by following steps:
The bamboo powder of 780.0g in 105 ℃ of dry 2h, then is crushed to 80 orders, adds 1000ml dimethylbenzene, soaked overnight is with 1200ml SO
3Finish in 20min with being added drop-wise in the mixture after the dilution of 1000ml sherwood oil, dripping, then stirring reaction 4.0h under the room temperature, the pH value of conditioned reaction system is to neutral, filter, 105 ℃ of dry 2.5h obtain vegetable fibre tensio-active agent 2949.0g, i.e. bamboo sulfuric ester.
When the aqueous solution mass concentration of gained bamboo sulfuric ester was 3.23%, surface tension was 59.2mN/m; Surface tension was 61.2mN/m when mass concentration was 1.62%, and rotary viscosity is 2.0mPas.
Compound surfactant is prepared by following steps:
Above-mentioned bamboo sulfuric ester is mixed with sodium lauryl sulphate (SDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of bamboo sulfuric ester is the mass concentration of 0.12%, SDS when being 0.12%, and surface tension is 29.8mN/m, and rotary viscosity is 6.0mPas.
Above-mentioned bamboo sulfuric ester is mixed with Sodium dodecylbenzene sulfonate (LDS), water, obtain compound surfactant after stirring.In compound surfactant, the mass concentration of bamboo sulfuric ester is 0.12%, and when the mass concentration of Sodium dodecylbenzene sulfonate (LDS) was 0.12%, surface tension 28.4mN/m, rotary viscosity were 4.0mPas.
Comparative Examples
A kind of vegetable fibre tensio-active agent is prepared by following steps:
13.0g bagasse is added in the 20.0ml hexane, soaked overnight, filtration drying obtains not sulphating bagasse 13.0 grams.Being distributed in the water of resulting not sulphating bagasse, surface tension is 72.5mN/m when the mass content of bagasse is 1.00%, and surface tension was 72.5mN/m when mass content was 0.50%, and rotary viscosity is 0.5mPas.
And sodium lauryl sulphate (SDS) mass concentration is when being 1.00%, and its surface tension is 33.4mN/m, and rotary viscosity is 2.5mPas;
When Sodium dodecylbenzene sulfonate (LDS) mass concentration was 1.00%, its surface tension was 30.2mN/m, and rotary viscosity is 2.0mPas.
Compound system is prepared by following steps:
Not sulphating bagasse and sodium lauryl sulphate (SDS) and the composite compound surfactant that obtains of water with gained.In compound surfactant, the mass concentration of sulphating bagasse is not the mass concentration of 0.25%, SDS when being 0.25%, and surface tension is 33.4mN/m, and rotary viscosity is 1.0mPas;
Not sulphating bagasse and Sodium dodecylbenzene sulfonate (LDS) and the composite compound surfactant that obtains of water with gained.In compound surfactant, the mass concentration of sulphating bagasse is not 0.25%, and when the mass concentration of Sodium dodecylbenzene sulfonate (LDS) was 0.25%, surface tension 30.6mN/m, rotary viscosity were 1.5mPas.
Contrast by embodiment and Comparative Examples can be found out: when vegetable fibre does not form sulfuric ester (Comparative Examples), do not have surfactivity, if with such vegetable fibre (namely not forming the vegetable fibre of sulfuric ester) and small molecules surfactant compound, coordinating effect is not obvious, does not reach the effect that reduces surface tension and thickening.The present invention can obtain surface tension compound surfactant low, that thickening effectiveness is good with vegetable fibre and the small molecules surfactant compound of sulphating.
Above-described embodiment is the better 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 the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a vegetable fibre tensio-active agent is characterized in that may further comprise the steps:
Get vegetable fibre, soak 10-36h with organic solvent; Then drip sulphoating agent, stirring reaction 0.5 ~ 5.0h under the room temperature, then the pH value with reaction system is adjusted to neutrality, with filter residue and drying, obtains the vegetable fibre tensio-active agent after the filtration;
Described vegetable fibre is 1g:(1.2-1.8 with the ratio of the consumption of sulphoating agent) ml.
2. the preparation method of vegetable fibre tensio-active agent according to claim 1 is characterized in that:
Described vegetable fibre is a kind of in bagasse, corn stalk, bamboo powder, pine powder, fiber crops, cotton or the sorghum stalk;
Described vegetable fibre, dry before using, then be crushed to 60 ~ 150 orders.
3. the preparation method of vegetable fibre tensio-active agent according to claim 1 is characterized in that:
Described organic solvent is a kind of in sherwood oil, toluene, dimethylbenzene or the hexane;
Described sulphoating agent is a kind of in the vitriol oil, oleum, sulphur trioxide or the chlorsulfonic acid.
4. the preparation method of vegetable fibre tensio-active agent according to claim 1 is characterized in that:
Described sulphoating agent will be used solvent cut before use; During dilution, the volume ratio of sulphoating agent and solvent is 1:(0.8-1.3);
Described solvent is more than one in sherwood oil, toluene, dimethylbenzene or the hexane;
Described dropping is to finish in 10 ~ 60min.
5. a vegetable fibre tensio-active agent is characterized in that: prepared by the described method of claim 1-4;
Described vegetable fibre tensio-active agent, when mass concentration was 0.05 ~ 5.00%, surface tension was 40.0 ~ 65.0mN/m.
6. a compound surfactant is characterized in that: by obtaining behind vegetable fibre tensio-active agent claimed in claim 5 and the small molecules surfactant compound;
Described small molecules tensio-active agent is sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, tween or class of department.
7. compound surfactant according to claim 6 is characterized in that: contain 0.05 ~ 5.00% vegetable fibre tensio-active agent and 0.05 ~ 5.00% small molecules tensio-active agent in the described compound surfactant; Described concentration is mass concentration.
8. compound surfactant according to claim 6 is characterized in that: contain 0.05 ~ 5.00% vegetable fibre tensio-active agent and 0.05 ~ 5.00% small molecules tensio-active agent in the described compound surfactant, surplus is water; Described concentration is mass concentration.
9. compound surfactant according to claim 6, it is characterized in that: described compound surfactant, when containing the small molecules tensio-active agent of 0.05 ~ 5.00% vegetable fibre tensio-active agent and 0.05 ~ 5.00%, surface tension is 25.0 ~ 30.0mN/m, and rotary viscosity is 2.0 ~ 10.0mPas; Described concentration is mass concentration.
10. each described compound surfactant application in oil recovery and filed of daily-use chemical industry of claim 6-9.
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|---|---|---|---|
| CN2012103160022A CN102850554A (en) | 2012-08-30 | 2012-08-30 | Vegetable fiber surfactant and compound surfactant |
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|---|---|---|---|
| CN2012103160022A CN102850554A (en) | 2012-08-30 | 2012-08-30 | Vegetable fiber surfactant and compound surfactant |
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Citations (5)
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|---|---|---|---|---|
| US5013825A (en) * | 1990-02-22 | 1991-05-07 | Westvaco Corporation | Sulfation of lignin |
| RU2268271C1 (en) * | 2004-07-15 | 2006-01-20 | Государственное образовательное учреждение высшего профессионального образования Алтайский государственный университет | Method of preparing water-soluble sulfuric acid esters of lingo-carbohydrate materials |
| CN101120102A (en) * | 2005-02-15 | 2008-02-06 | 奥克西特诺工业与贸易公司 | Acid hydrolysis process of cellulosic and lignocellulosic materials, digestion vessel and hydrolysis reactor |
| CN101148481A (en) * | 2007-11-01 | 2008-03-26 | 华侨大学 | Oligomeric glucose sulfuric ester and preparation thereof |
| CN102580610A (en) * | 2012-01-09 | 2012-07-18 | 中科院广州化学有限公司 | Lignosulfonate alkylation modified surfactant and preparation method and application thereof |
-
2012
- 2012-08-30 CN CN2012103160022A patent/CN102850554A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5013825A (en) * | 1990-02-22 | 1991-05-07 | Westvaco Corporation | Sulfation of lignin |
| RU2268271C1 (en) * | 2004-07-15 | 2006-01-20 | Государственное образовательное учреждение высшего профессионального образования Алтайский государственный университет | Method of preparing water-soluble sulfuric acid esters of lingo-carbohydrate materials |
| CN101120102A (en) * | 2005-02-15 | 2008-02-06 | 奥克西特诺工业与贸易公司 | Acid hydrolysis process of cellulosic and lignocellulosic materials, digestion vessel and hydrolysis reactor |
| CN101148481A (en) * | 2007-11-01 | 2008-03-26 | 华侨大学 | Oligomeric glucose sulfuric ester and preparation thereof |
| CN102580610A (en) * | 2012-01-09 | 2012-07-18 | 中科院广州化学有限公司 | Lignosulfonate alkylation modified surfactant and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李杰训: "《三元复合驱地面工程技术试验进展》", 31 May 2009, 中国石油大学出版社 * |
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Application publication date: 20130102 |