CN113582887A - Purification method and purification system of crude petroleum sodium sulfonate - Google Patents
Purification method and purification system of crude petroleum sodium sulfonate Download PDFInfo
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- CN113582887A CN113582887A CN202110942146.8A CN202110942146A CN113582887A CN 113582887 A CN113582887 A CN 113582887A CN 202110942146 A CN202110942146 A CN 202110942146A CN 113582887 A CN113582887 A CN 113582887A
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Abstract
The invention relates to a purification method and a purification system of crude petroleum sodium sulfonate, which comprises the following steps: s1: obtaining crude sodium petroleum sulfonate, and adding an ethanol aqueous solution into the crude sodium petroleum sulfonate; s2: heating to 55-65 ℃, and then standing for a certain time; s3: the upper layer of extract oil is separated out, then the middle impurity layer is separated out, and the lower layer of extract is refined to obtain the purified petroleum sodium sulfonate. An ethanol aqueous solution is added into crude petroleum sodium sulfonate, then the mixture is heated and then is kept stand, and then a layered solution is formed, namely the ethanol aqueous solution absorbs impurities in the petroleum sodium sulfonate, which are easily dissolved in ethanol and water, oil substances with lighter density are arranged at the upper layer, and an impurity intermediate state is formed at the middle part, which is positioned at the middle position of the layered solution.
Description
Technical Field
The invention relates to a purification and refining technology of chemical substances, in particular to a purification method and a purification system of crude petroleum sodium sulfonate.
Background
Sodium petroleum sulfonate is a very common inorganic substance and its molecular formula can be represented as RSO3Na (R ═ C14 to C22 alkyl). In particular applications, it can be applied in the textile field, in the field of printing and dyeing auxiliaries and in the field of liquid detergents.
In the preparation process of the sodium petroleum sulfonate, the sodium petroleum sulfonate can be obtained through petroleum fractions and subsequent chemical reactions, however, the prepared sodium petroleum sulfonate has some impurities which need to be removed when the use grade of the sodium petroleum sulfonate is higher.
Through analysis of the crude petroleum sodium sulfonate, the components of the crude petroleum sodium sulfonate mainly comprise base oil, petroleum sodium sulfonate, impurities and water, wherein the base oil is a petroleum hydrocarbon oily mixed substance, the ratio of the base oil is 40-65%, the ratio of the petroleum sodium sulfonate is 25-50%, the ratio of the impurities is about 5%, and the ratio of the water is 1-5%. Base oils, also known as basestocks, are derived from petroleum materials added at the time of feed production.
In the prior art, generally, salting-out and other manners can be adopted for purification, and other types of impurity removal methods special for petroleum sodium sulfonate also appear, however, the problems that the process steps are complicated and mass production is not facilitated generally exist in the methods for removing the petroleum sodium sulfonate in the prior art, so that the impurity removal efficiency is reduced.
Disclosure of Invention
The invention mainly aims to provide a method and a related system device which have simple steps and are suitable for removing impurities in petroleum sodium sulfonate in a large scale.
In order to accomplish the above object, the present invention provides a method for purifying crude sodium petroleum sulfonate, comprising the steps of:
s1: obtaining crude sodium petroleum sulfonate, and adding an ethanol aqueous solution into the crude sodium petroleum sulfonate;
s2: heating to 55-65 deg.C, and standing for a certain time to obtain upper layer extractive oil, middle impurity layer and lower layer extractive solution;
s3: the upper layer of extract oil is separated out, then the middle impurity layer is separated out, and the lower layer of extract is refined to obtain the purified petroleum sodium sulfonate.
The beneficial effect of above-mentioned scheme does: the method comprises the steps of adding an ethanol aqueous solution into crude petroleum sodium sulfonate, heating, refining, and forming a layered solution, wherein the ethanol aqueous solution absorbs impurities in the petroleum sodium sulfonate, which are easily dissolved in ethanol and water, an oil substance with relatively low density is arranged at the upper layer, an impurity intermediate state is formed at the middle part and is positioned at the middle position of the layered solution, and then the intermediate solution layer can be separated, so that the aim of quickly and efficiently removing the impurities in the petroleum sodium sulfonate is fulfilled, and the method is suitable for large-scale production. Through experimental analysis, the impurity content in the treated petroleum sodium sulfonate is lower than 1%.
In a preferred scheme, the middle impurity layer and the lower extraction liquid are respectively rectified to obtain recovered ethanol, the recovered ethanol is used for refining and purifying the petroleum sodium sulfonate again, and impurities are discarded.
In a preferred embodiment, the temperature of the elevated temperature is 60 ℃ and the standing step is kept at a constant temperature for 24 hours. It was experimentally confirmed that the refining time must be 12 hours or more, or the effect of separation is not good, and preferably 24 hours or more, so that a three-layer solution state with a distinct boundary and easy separation can be obtained. In addition, the temperature of the temperature rise is the optimal temperature at 60 ℃, and the solubility of the impurities dissolved in the ethanol at the temperature is maximized, namely the purity of the finally obtained petroleum sodium sulfonate is the highest.
In a preferred embodiment, the concentration ratio of ethanol in the ethanol aqueous solution is 50% by weight.
The invention provides a purification system of petroleum sodium sulfonate, which comprises:
a separation column;
the first feeding tower is used for containing crude petroleum sodium sulfonate and is connected with the separation tower through a first pipeline and a first valve;
the second feeding tower is used for containing the ethanol water solution and is connected with the separation tower through a second pipeline and a second valve;
the first recovery tower is used for bearing upper layer extraction oil and is connected with the separation tower through a third pipeline and a third valve;
the second recovery tower is used for containing the lower-layer extract, is connected with the separation tower through a fourth pipeline and a fourth valve and is arranged at the lower position of the separation tower;
the third recovery tower is used for bearing the intermediate impurity layer and is connected with the separation tower through a fifth pipeline and a fifth valve;
the rectifying tower is connected with the third recovery tower through a sixth pipeline and a sixth valve, the rectifying tower is provided with an outflow pipeline, and the outflow pipeline is connected with the second feeding tower.
Preferably, the separation column is provided with a side wall part at a middle position, the side wall part is penetrated by the fifth pipeline, the fifth pipeline transversely penetrates through the side wall part, and a port of the fifth pipeline is positioned in the intermediate impurity layer.
Preferably, the part of the fifth pipeline, which is located on the intermediate impurity layer, is provided with a telescopic section, a first rotating arm section and a second rotating arm section which are sequentially connected, the first rotating arm section circumferentially rotates relative to the telescopic section, and the second rotating arm section can circumferentially rotate around the first rotating arm section.
The purification method of the purification system of the petroleum sodium sulfonate comprises the following steps:
adding crude sodium petroleum sulfonate to the separation column through a first feed column along a first conduit and a first valve;
then adding an ethanol aqueous solution into the separation tower through a second pipeline and a second valve of the second feeding tower;
heating the separation tower to 55-65 ℃, and standing for a certain time to obtain upper-layer extract oil, a middle impurity layer and a lower-layer extract;
firstly, leading the upper layer of extracted oil into a first recovery tower through a third pipeline and a third valve; then, the intermediate impurity layer is led into a third recovery tower through a fifth pipeline and a fifth valve, and finally the lower layer extract is led into a second recovery tower through a fourth pipeline and a fourth valve;
and guiding the middle impurity layer in the third recovery tower into the rectifying tower through a sixth pipeline and a sixth valve for refining and fractionation to obtain a recovered ethanol water solution and impurities, and returning the recovered ethanol water solution to the second feeding tower for recycling.
In a preferable scheme, the temperature is raised to 60 ℃, the standing step is kept at a constant temperature for 24 hours; the weight concentration ratio of ethanol in the ethanol water solution is 50%.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a schematic diagram of a purification system for sodium petroleum sulfonate according to the present invention.
Detailed Description
The technical solution in the embodiments of the present invention is clearly and completely described below with reference to the drawings in the embodiments of the present invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
The first embodiment:
the invention provides a method for purifying crude petroleum sodium sulfonate, which comprises the following steps:
s1: obtaining crude sodium petroleum sulfonate, and adding an ethanol aqueous solution into the crude sodium petroleum sulfonate;
s2: heating to 55-65 deg.C, and standing for a certain time to obtain upper layer extractive oil, middle impurity layer and lower layer extractive solution;
s3: the upper layer of extract oil is separated out, then the middle impurity layer is separated out, and the lower layer of extract is refined to obtain the purified petroleum sodium sulfonate.
The method comprises the steps of adding an ethanol aqueous solution into crude sodium petroleum sulfonate, heating, standing, and forming a layered solution, wherein the ethanol aqueous solution absorbs impurities in the sodium petroleum sulfonate, which are easily dissolved in ethanol and water, an oil substance with relatively low density is arranged at the upper position, an impurity intermediate state is formed at the middle position, the impurity intermediate state is positioned at the middle position of the layered solution, and then the intermediate solution layer can be separated, so that the purpose of quickly and efficiently removing the impurities in the sodium petroleum sulfonate is realized, and the method is suitable for large-scale production. Through experimental analysis, the impurity content in the treated petroleum sodium sulfonate is lower than 1%.
Second embodiment:
preferably, the middle impurity layer and the lower extraction liquid are respectively rectified to obtain recovered ethanol, the recovered ethanol is used for refining and purifying the petroleum sodium sulfonate again, and the impurities are discarded. The temperature of the temperature rise was 60 ℃, and the standing step was kept constant for 24 hours. The weight concentration ratio of ethanol in the ethanol water solution is 50%. It was experimentally confirmed that the refining time must be 12 hours or more, or the effect of separation is not good, and preferably 24 hours or more, so that a three-layer solution state with a distinct boundary and easy separation can be obtained. In addition, the temperature of the temperature rise is the optimal temperature at 60 ℃, and the solubility of the impurities dissolved in the ethanol at the temperature is maximized, namely the purity of the finally obtained petroleum sodium sulfonate is the highest.
In one particular test example, the crude sodium petroleum sulfonate was composed of 55% base oil, 5% impurities, 35% sodium petroleum sulfonate, and the balance water. Ethanol water solution with the weight proportion of 50 percent is adopted for carrying out layered extraction, the temperature rise is controlled at 60 ℃, and the standing time is 24 hours. Fractionating the obtained lower layer extract to remove ethanol and water to obtain 65% of petroleum sodium sulfonate, impurities below 1%, and heavy base oil as the rest.
In addition, when the extractant of the ethanol aqueous solution is replaced by an ester solvent such as ethyl acetate, butyl acetate, dichloromethane and the like, the purpose of controlling the impurities of the refined petroleum sodium sulfonate to be below 1 percent cannot be achieved, namely, the impurities of other solvents are all above 1 percent after extraction.
The third embodiment:
as shown in fig. 1, the system for purifying sodium petroleum sulfonate provided by the present invention comprises a separation tower 1, a first feeding tower 2, a second feeding tower 3, a first recovery tower 4, a second recovery tower 5, a third recovery tower 6 and a rectification tower 7;
the first feeding tower 2 is used for containing crude sodium petroleum sulfonate, and the first feeding tower 2 is connected with the separation tower 1 through a first pipeline and a first valve;
the second feeding tower 3 is used for containing an ethanol water solution, and the second feeding tower 3 is connected with the separation tower 1 through a second pipeline and a second valve;
the first recovery tower 4 is used for bearing upper layer extraction oil, and the first recovery tower 4 is connected with the separation tower through a third pipeline and a third valve; the end of the third pipe is inserted into the upper layer of the extraction oil by adopting a pumping mode, and then the upper layer of the extraction oil is sucked into the first recovery tower 4;
the second recovery tower 5 is used for containing the lower layer of extract, the second recovery tower 5 is connected with the separation tower 1 through a fourth pipeline and a fourth valve, and the second recovery tower 5 is arranged at the lower position of the separation tower 1; the lower layer of the pumped liquid can be discharged into the second recovery tower 5 by the action of gravity.
The third recovery tower 6 is used for bearing the intermediate impurity layer, and the third recovery tower 6 is connected with the separation tower through a fifth pipeline and a fifth valve; the end of the fifth pipe may be inserted into the intermediate impurity layer and then suck the intermediate impurity layer into the third recovery tower 6.
Rectifying column 7 through sixth pipeline and sixth valve with third recovery tower 6 is connected, rectifying column 6 has the outflow pipeline, the outflow pipeline with the second feeding tower is connected.
The purification method of the purification system of the petroleum sodium sulfonate comprises the following steps:
adding crude sodium petroleum sulfonate into the separation tower through a first feeding tower 2 along a first pipeline and a first valve;
then adding an ethanol water solution into the separation tower through a second pipeline and a second valve of the second feeding tower 2;
heating the separation tower 1 to 55-65 ℃, and standing for a certain time to obtain upper-layer extract oil, a middle impurity layer and a lower-layer extract;
firstly, leading the upper layer of extracted oil into a first recovery tower 2 through a third pipeline and a third valve; then, the intermediate impurity layer is introduced into a third recovery tower 6 through a fifth pipeline and a fifth valve, and finally the lower layer extract is introduced into a second recovery tower 5 through a fourth pipeline and a fourth valve; in the method, firstly, the upper layer of extraction oil is transferred into the first recovery tower 2, and then the middle impurity layer is introduced into the third recovery tower 6, so that the contact between the extraction liquid and the middle impurity layer can be avoided to the maximum extent, if the middle impurity layer is extracted firstly, part of the upper layer of extraction oil is inevitably contacted with the residual middle impurity layer on the side wall of the separation tower, and the separation efficiency is reduced.
And guiding the intermediate impurity layer in the third recovery tower 6 into a rectifying tower 7 through a sixth pipeline and a sixth valve for refining and fractionation to obtain a recovered ethanol water solution and impurities, and returning the recovered ethanol water solution to the second feeding tower 2 for recycling.
The fourth embodiment:
and a side wall part is formed at the middle position of the separation tower, the fifth pipeline penetrates through the side wall part, the fifth pipeline transversely penetrates through the side wall part, and a port of the fifth pipeline is positioned in the intermediate impurity layer. Through the arrangement of the structure, the suction process can be more conveniently completed by inserting the fifth pipeline to the position of the intermediate impurity layer.
The part of the fifth pipeline, which is located on the middle impurity layer, is provided with a telescopic section, a first rotating arm section and a second rotating arm section which are sequentially connected, wherein the first rotating arm section is opposite to the telescopic section and rotates in the circumferential direction, and the second rotating arm section can rotate around the first rotating arm section and rotate in the circumferential direction. The distance between the end part of the pipeline and the side wall can be adjusted through the telescopic action of the telescopic section, the operation of absorbing the middle impurity layer is preferably carried out at the position close to the side wall at the end part of the pipeline, thus, the middle impurity layer can be completely sucked, and the position of the end part of the pipeline can be moved at intervals in the process, namely, the inlet at the end position of the pipeline moves along the position of the middle impurity layer close to the side wall so as to completely suck residual impurities on the side wall at different positions, and the angle and the position of the inlet at the end part of the pipeline can be well adjusted through the free rotation action of the first rotating arm and the second rotating arm, thereby making it very easy to adjust the port position of the fifth pipe to different heights and positions to achieve a suction action for the intermediate impurity layer, in particular for the intermediate impurity layer near the sidewall position.
The temperature of the temperature rise is 60 ℃, the standing step is kept constant, and the time is 24 hours; the weight concentration ratio of ethanol in the ethanol water solution is 50%.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. A method for purifying crude sodium petroleum sulfonate, which is characterized by comprising the following steps:
s1: obtaining crude sodium petroleum sulfonate, and adding an ethanol aqueous solution into the crude sodium petroleum sulfonate;
s2: heating to 55-65 deg.C, and standing for a certain time to obtain upper layer extractive oil, middle impurity layer and lower layer extractive solution;
s3: the upper layer of extract oil is separated out, then the middle impurity layer is separated out, and the lower layer of extract is refined to obtain the purified petroleum sodium sulfonate.
2. The method for purifying crude sodium petroleum sulfonate according to claim 1, wherein the middle impurity layer and the lower extraction liquid are respectively rectified to obtain recovered ethanol, the recovered ethanol is used for refining and purifying sodium petroleum sulfonate again, and impurities are discarded.
3. The method for purifying sodium crude petroleum sulfonate according to claim 1, wherein the temperature of the temperature rise is 60 ℃, and the standing step is maintained at a constant temperature for 24 hours.
4. The method of purifying crude sodium petroleum sulfonate according to claim 1, wherein the concentration ratio of ethanol in the aqueous ethanol solution is 50% by weight.
5. A system for purifying sodium petroleum sulfonate, which is characterized by comprising:
a separation column;
the first feeding tower is used for containing crude petroleum sodium sulfonate and is connected with the separation tower through a first pipeline and a first valve;
the second feeding tower is used for containing the ethanol water solution and is connected with the separation tower through a second pipeline and a second valve;
the first recovery tower is used for bearing upper layer extraction oil and is connected with the separation tower through a third pipeline and a third valve;
the second recovery tower is used for containing the lower-layer extract, is connected with the separation tower through a fourth pipeline and a fourth valve and is arranged at the lower position of the separation tower;
the third recovery tower is used for bearing the intermediate impurity layer and is connected with the separation tower through a fifth pipeline and a fifth valve;
the rectifying tower is connected with the third recovery tower through a sixth pipeline and a sixth valve, the rectifying tower is provided with an outflow pipeline, and the outflow pipeline is connected with the second feeding tower.
6. The purification system of sodium petroleum sulfonate according to claim 5,
and a side wall part is formed at the middle position of the separation tower, the fifth pipeline penetrates through the side wall part, the fifth pipeline transversely penetrates through the side wall part, and a port of the fifth pipeline is positioned in the intermediate impurity layer.
7. The purification system of sodium petroleum sulfonate according to claim 5,
the part of the fifth pipeline, which is located on the middle impurity layer, is provided with a telescopic section, a first rotating arm section and a second rotating arm section which are sequentially connected, wherein the first rotating arm section is opposite to the telescopic section and rotates in the circumferential direction, and the second rotating arm section can rotate around the first rotating arm section and rotate in the circumferential direction.
8. The purification method of sodium petroleum sulfonate according to claim 5, comprising the steps of:
adding crude sodium petroleum sulfonate to the separation column through a first feed column along a first conduit and a first valve;
then adding an ethanol aqueous solution into the separation tower through a second pipeline and a second valve of the second feeding tower;
heating the separation tower to 55-65 ℃, and standing for a certain time to obtain upper-layer extract oil, a middle impurity layer and a lower-layer extract;
firstly, leading the upper layer of extracted oil into a first recovery tower through a third pipeline and a third valve; then, the intermediate impurity layer is led into a third recovery tower through a fifth pipeline and a fifth valve, and finally the lower layer extract is led into a second recovery tower through a fourth pipeline and a fourth valve;
and guiding the middle impurity layer in the third recovery tower into the rectifying tower through a sixth pipeline and a sixth valve for refining and fractionation to obtain a recovered ethanol water solution and impurities, and returning the recovered ethanol water solution to the second feeding tower for recycling.
9. The purification method of sodium petroleum sulfonate according to claim 8, wherein the temperature of the temperature rise is 60 ℃, the standing step is kept at a constant temperature for 24 hours; the weight concentration ratio of ethanol in the ethanol water solution is 50%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218800A (en) * | 1997-12-03 | 1999-06-09 | 中国科学院新疆化学研究所 | Process for producing petroleum sodium sulfonate product |
| CN104072374A (en) * | 2013-03-29 | 2014-10-01 | 池银萍 | Preparation method of dimethyl terephthalate (DMT) |
| CN111377802A (en) * | 2018-12-27 | 2020-07-07 | 湖南中创化工股份有限公司 | Preparation method and system of sec-butyl alcohol |
| CN112142562A (en) * | 2019-06-28 | 2020-12-29 | 国家能源投资集团有限责任公司 | Method and device for reducing separation energy consumption of ethanol crude product prepared by acetic acid hydrogenation |
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- 2021-08-17 CN CN202110942146.8A patent/CN113582887A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218800A (en) * | 1997-12-03 | 1999-06-09 | 中国科学院新疆化学研究所 | Process for producing petroleum sodium sulfonate product |
| CN104072374A (en) * | 2013-03-29 | 2014-10-01 | 池银萍 | Preparation method of dimethyl terephthalate (DMT) |
| CN111377802A (en) * | 2018-12-27 | 2020-07-07 | 湖南中创化工股份有限公司 | Preparation method and system of sec-butyl alcohol |
| CN112142562A (en) * | 2019-06-28 | 2020-12-29 | 国家能源投资集团有限责任公司 | Method and device for reducing separation energy consumption of ethanol crude product prepared by acetic acid hydrogenation |
Non-Patent Citations (1)
| Title |
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| 李莎莎等: "石油磺酸钠的合成及性能研究" * |
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