CN110903331A - Method for separating fatty alcohol from alkyl glycoside crude product - Google Patents
Method for separating fatty alcohol from alkyl glycoside crude product Download PDFInfo
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- 150000002191 fatty alcohols Chemical class 0.000 title claims abstract description 100
- -1 alkyl glycoside Chemical class 0.000 title claims abstract description 54
- 229930182470 glycoside Natural products 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000012043 crude product Substances 0.000 title claims abstract description 6
- 238000000605 extraction Methods 0.000 claims abstract description 72
- 238000000926 separation method Methods 0.000 claims abstract description 38
- 238000009835 boiling Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 7
- 229920000544 Gore-Tex Polymers 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims 2
- 210000003437 trachea Anatomy 0.000 claims 2
- 238000010276 construction Methods 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 22
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 239000012265 solid product Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 304
- 229910002092 carbon dioxide Inorganic materials 0.000 description 152
- 239000007789 gas Substances 0.000 description 38
- 230000000694 effects Effects 0.000 description 7
- 229930182478 glucoside Natural products 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000002608 ionic liquid Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 239000011552 falling film Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- KVNRLNFWIYMESJ-UHFFFAOYSA-N butyronitrile Chemical compound CCCC#N KVNRLNFWIYMESJ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/04—Acyclic radicals, not substituted by cyclic structures attached to an oxygen atom of the saccharide radical
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for separating fatty alcohol from alkyl glycoside crude product, belonging to the technical field of light chemical industry daily necessities separation, the method for separating fatty alcohol from alkyl glycoside crude product adopts supercritical CO2 extraction separation technology to extract and separate unreacted fatty alcohol, so as to obtain high-purity alkyl glycoside solid product, does not need to use organic solvent, does not need post-treatment, has low cost, is easy for large-scale production, and can lead CO2 to the cavity channel through the arrangement of semi-permeable suspension barrel and air cavity channel, so that the CO2 fluid containing fatty alcohol is in micro-boiling condition, further the overflow of gaseous CO2 is accelerated, further the separation efficiency is accelerated, on the other hand, compared with the CO2 separated in one direction in the prior art, the separated gaseous CO2 is discharged from the upper part and the air cavity channel outwards in multiple directions after the CO2 is stopped, the moving path of the gaseous CO2 during overflowing can be effectively reduced, and therefore the separation efficiency of the gaseous CO2 and the fatty alcohol is remarkably improved.
Description
Technical Field
The invention relates to the technical field of separation of light chemical articles for daily use, in particular to a method for separating fatty alcohol from a crude product of alkyl glycoside.
Background
Alkyl glucoside (Alkyl polyglucoside for short) is a novel nonionic surfactant synthesized by removing a molecule of water from glucose and fatty alcohol serving as raw materials under the catalysis of acid and the like, and the composition of the nonionic surfactant is a mixture of mono-glycoside, di-glycoside, tri-glycoside and poly-glycoside, and is also called Alkyl Polyglycoside. APG has a series of excellent properties such as thickening, solubilizing, emulsifying, etc., and high surface activity, safety and compatibility, and thus it has wide applications in many fields such as daily chemicals, medicines, building materials, etc., including detergents, cosmetics, disinfectant lotions, industrial aids, and pesticide emulsions.
In the preparation of alkyl glucoside, the reactant fatty alcohol is usually in a great excess, and the excess must be removed from the reaction product, otherwise, the surface activity of the alkyl glucoside is reduced, the product quality is affected, and the reactant fatty alcohol is wasted. In order to remove the fatty alcohol from the product, a high-temperature high-vacuum method is generally adopted, and the fatty alcohol is distilled out of the product mixture by falling film distillation according to the difference of the boiling points of the alkyl glucoside and the fatty alcohol, so as to achieve the purpose of removing the fatty alcohol. However, the temperature of the falling film distillation is generally as high as 150 ℃, so that the energy consumption is high, and the product is easy to coke at high temperature to generate color, thereby affecting the appearance and quality of the product; in addition, even under high temperature and high vacuum, the viscosity of the alkyl glucose glycoside is high, so that the pipeline is easily blocked, and the normal production is influenced; in order to remove the color of the product, hydrogen peroxide is often used to perform oxidation and decoloration treatment on the product, which not only increases the subsequent treatment procedures, but also increases the production cost.
Aiming at the problem of removing fatty alcohol in alkyl glucoside, the invention patent with application number of 2016111777183 discloses a method for separating and purifying alkyl glucoside by using ionic liquid, which comprises the steps of extracting fatty alcohol in an alkyl glucoside mixture by using imidazole ionic liquid and/or pyridine ionic liquid as an extracting agent, then back-extracting fatty alcohol in the ionic liquid by using ether and/or ethyl acetate as the extracting agent, and finally separating the fatty alcohol from the ether extracting agent by a distillation method. Although the method can obtain solid alkyl glycoside, the separation process has complex steps and high cost, and is difficult to industrially apply. The invention patent with application number 201710752316X discloses a method for obtaining powdered alkyl glycoside, which uses a mixture of more than two of methyl formate, methyl acetate, ethyl acetate, methyl propionate, ethyl propionate, acetone, butanone, cyclopentanone, cyclohexanone, methanol, ethanol, propanol, butanol, ethylene glycol, polyethylene glycol, acetonitrile, propionitrile and butyronitrile as an extracting agent, and extracts for 3-6 times at 30-60 ℃ to obtain powdered alkyl glycoside. Application No. 2019104300559 discloses an alkyl glycoside bleaching device, which mainly aims at the problem of color generation of alkyl glycoside caused by a method for removing fatty alcohol by high-temperature distillation.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for separating fatty alcohol from crude alkyl glycoside products, which adopts a supercritical CO2 extraction separation technology to extract and separate unreacted fatty alcohol from a mixture of unreacted fatty alcohol and alkyl glycoside to obtain a high-purity solid alkyl glycoside product, does not need to use an organic solvent, is an environment-friendly green separation method, does not need post-treatment, has low cost and is easy for large-scale production, and through the arrangement of a semi-transparent suspended barrel and a gas cavity channel, CO2 can be introduced into the gas cavity channel to ensure that CO2 fluid containing fatty alcohol is in a micro-boiling state, further the overflow of gaseous CO2 is accelerated, the separation efficiency is accelerated, on the other hand, compared with the CO2 which is discharged and separated in one direction in the prior art, gaseous CO2 is separated after CO2 is stopped being introduced from an auxiliary gas pipe, the invention can not only discharge from the upper part and the air cavity channel in a multidirectional way, but also effectively reduce the movement path when the gaseous CO2 overflows, thereby obviously improving the separation efficiency of the gaseous CO2 and the fatty alcohol.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for separating fatty alcohol from crude alkyl glycoside comprises the following steps:
s1, placing a certain amount of crude alkyl glycoside into an extraction kettle, starting a supercritical CO2 extraction separation system, setting the extraction temperature and the extraction pressure, and pumping CO2 into the extraction kettle from a CO2 gas source;
s2, when the temperature and the pressure in the extraction kettle reach set values, continuously pumping CO2 through a CO2 high-pressure pump according to a certain flow rate to extract fatty alcohol;
s3, separating fatty alcohol from CO2 by reducing pressure of CO2 containing the fatty alcohol in a separator, and recycling CO2 of the separated fatty alcohol;
s4, when the extraction time reaches the preset value, recovering CO2 in the extraction kettle, then taking out the solid pure product of the alkyl glycoside from the extraction kettle, and reusing the fatty alcohol separated from the separator.
Further, the extraction temperature in the step S1 is set to be 20-80 ℃, preferably 25-60 ℃; the extraction pressure is set to 10MPa to 50MPa, preferably 15MPa to 45 MPa.
Further, the constant flow rate CO2 in S2 is set to 3kg/hr to 10kg/hr, preferably 5 to 8 kg/hr.
Further, the pressure reduction in S3 means that the pressure of the separator is set to 3MPa to 7MPa, preferably 4.5 to 5.5 MPa.
Further, the extraction time in S4 is set to 20 minutes to 180 minutes, preferably 30 to 90 minutes.
Further, a CO2 gas source, a CO2 high-pressure pump, an extraction kettle and a separator jointly form a supercritical CO2 extraction separation system, the CO2 gas source, the CO2 high-pressure pump, the extraction kettle and the separator are connected with one another through pipelines, an output pipeline of the separator is communicated with an input pipeline of the CO2 high-pressure pump, the lower end of the separator is connected with a boiling assisting gas pipe communicated with a CO2 gas source, the lower end of the separator is also connected with an auxiliary gas exhaust pipe communicated with an output pipeline of the separator, and the pipeline between the CO2 gas source and the CO2 high-pressure pump, the pipeline between the extraction kettle and the separator, the boiling assisting gas pipe and the auxiliary gas exhaust pipe are connected with valves.
Further, a semi-permeable suspension barrel is fixedly connected inside the separator, an air cavity channel is enclosed between the inner walls below the separator by the semi-permeable suspension barrel, when the separation of CO2 is started, CO2 can be introduced from the boiling-assistant air pipe to the bottom of the air cavity channel, CO2 can penetrate through the lower permeable part and enter the CO2 fluid containing fatty alcohol, at the moment, CO2 gas can form impact bubbles inside the CO2 fluid containing fatty alcohol, the bubbles are continuously exploded in the CO2 fluid containing fatty alcohol, so that the effect of stirring the CO2 fluid containing fatty alcohol is realized, the CO2 fluid containing fatty alcohol is subjected to micro-boiling, the overflow of gaseous CO2 is accelerated, the separation efficiency is accelerated, after the separation is half, the introduction of CO2 from the boiling-assistant air pipe can be stopped, at the moment, the upper part of the lower permeable part leaks out, so that the air cavity channel can be communicated with the inside of the separator, at the moment, gaseous CO2 can not only burst from the upper part, the gas-phase CO2 can enter the gas cavity channel, so that when the gas-phase CO2 at the bottom overflows, the gas-phase CO2 which does not need to penetrate through the whole oily fatty alcohol in a fluid state overflows from the upper part, the gas-phase CO2 can overflow from the side wall and the bottom of the semi-permeable suspension barrel nearby and enter the gas cavity channel, and then is discharged from the auxiliary exhaust pipe or enters the separator through the lower through part again to be discharged upwards, compared with the prior art which discharges separated CO2 in one direction, the gas-phase CO2 separation device can effectively reduce the movement path of the gas-phase CO2, and can discharge gas CO2 in multiple directions, thereby obviously improving the separation efficiency of the gas-phase CO2 and the fatty alcohol.
Furthermore, the semi-permeable suspended barrel comprises an upper connecting part fixedly connected with the inner wall of the separator and a lower permeable part fixedly connected with the lower end of the upper connecting part.
Furthermore, the upper connecting part is of a solid structure, the lower through part is of a porous structure, so that gaseous CO2 can pass through the lower through part and move between the semi-transparent suspended barrel and the air cavity channel, the dividing point of the upper connecting part and the lower through part is positioned between the bisection point of the semi-transparent suspended barrel and the upper trisection point, the dividing point is too high, so that when CO2 is introduced from the boiling-assistant air pipe to accelerate the separation of CO2, the air cavity channel is communicated with the inside of the separator, the generation of the micro-boiling phenomenon in CO2 fluid containing fatty alcohol is not facilitated, the dividing point is too low, the contact surface of CO2 introduced from the boiling-assistant air pipe and CO2 fluid containing fatty alcohol is contacted, the generation of the micro-boiling phenomenon in CO2 fluid containing fatty alcohol is slow, and the effect of accelerating the separation efficiency is not obvious.
Further, the semi-permeable suspended barrel is adhered with an inner semi-permeable diaphragm, the inner semi-permeable diaphragm is made of a GORE-TEX material, CO2 gas molecules can penetrate through the inner semi-permeable diaphragm, water molecules of the inner semi-permeable diaphragm cannot penetrate through the inner semi-permeable diaphragm, water belongs to small molecules, fatty alcohol belongs to organic macromolecules, the fatty alcohol cannot penetrate through the inner semi-permeable diaphragm, the fatty alcohol is difficult to enter an air cavity channel, the separation rate of CO2 and the fatty alcohol is effectively improved, and the thickness of the GORE-TEX is 1-2 mm.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
according to the scheme, a supercritical CO2 extraction separation technology is adopted, unreacted fatty alcohol is extracted and separated, a high-purity alkyl glycoside solid product is obtained, an organic solvent is not needed, post-treatment is not needed, the cost is low, large-scale production is easy, and through the arrangement of a semi-permeable suspension barrel and an air cavity channel, on one hand, CO2 can be introduced into the cavity channel, so that the CO2 fluid containing the fatty alcohol is in a micro-boiling state, the overflow of gaseous CO2 is accelerated, and the separation efficiency is accelerated, on the other hand, compared with the prior art that separated CO2 is discharged in one direction, after CO2 is stopped to be introduced, separated gaseous CO2 is separated, the invention can discharge from the upper part and the air cavity channel outwards in a multi-direction, and can effectively reduce the movement path when the gaseous CO2 overflows, so that the separation efficiency of the gaseous CO2 and the fatty alcohol is remarkably improved.
Drawings
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic view of the lower half of the separator of the present invention;
FIG. 3 is a schematic view of the structure of the present invention when CO2 is introduced into the lower part of the separator;
FIG. 4 is a schematic diagram of the separated gaseous CO2 as it overflows in multiple directions in accordance with the present invention;
fig. 5 is a schematic diagram of a prior art separated gaseous CO2 as it overflows upward.
The reference numbers in the figures illustrate:
11 upper connecting parts, 12 lower through parts, 21 boiling-assistant air pipes, 22 exhaust-assistant pipes and 3 inner semi-through diaphragms.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a method for separating fatty alcohol from crude alkyl glycoside comprises the steps of putting 1000 g of crude alkyl glycoside into an extraction kettle, closing a kettle cover, heating the extraction kettle, opening a valve when the temperature of the extraction kettle reaches 25 ℃, pumping carbon dioxide into the extraction kettle from a CO2 gas source through a CO2 high-pressure pump to enable CO2 to fully contact the crude alkyl glycoside, opening the valve when the pressure reaches 25MPa to enable CO2 to take extracted fatty alcohol out of the extraction kettle and enter a separator, setting the pressure in the separator to be 5MPa, setting the flow rate of CO2 to be 5kg/hr, and recycling CO2 after separating fatty alcohol in the separator. And after the extraction is carried out for 60 minutes, the CO2 high-pressure pump is closed, after the pressure in the extraction kettle reaches the normal pressure, the extraction kettle is opened, and the alkyl glycoside product after the fatty alcohol is separated is taken out, wherein the content of the fatty alcohol is 1.4 percent. The CO2 collected from the separator can be reused.
The supercritical CO2 extraction and separation system is composed of a CO2 gas source, a CO2 high-pressure pump, an extraction kettle and a separator, the CO2 gas source, the CO2 high-pressure pump, the extraction kettle and the separator are connected with one another through pipelines, an output pipeline of the separator is communicated with an input pipeline of a CO2 high-pressure pump, the lower end of the separator is connected with an auxiliary boiling gas pipe 21 communicated with a CO2 gas source, the lower end of the separator is also connected with an auxiliary exhaust pipe 22 communicated with an output pipeline of the separator, and the pipelines between the CO2 gas source and the CO2 high-pressure pump, the pipeline between the extraction kettle and the separator, the auxiliary boiling gas pipe 21 and the auxiliary exhaust pipe 22 are connected with valves.
Referring to fig. 2, a semi-permeable suspension barrel is fixedly connected inside the separator, a gas cavity channel is enclosed between the inner walls below the separator by the semi-permeable suspension barrel, referring to fig. 3, when the CO2 separation is started, CO2 can be introduced from the boiling-assistant gas pipe 21 to the bottom of the gas cavity channel, CO2 can penetrate through the lower permeable part 12 and enter the CO2 fluid containing fatty alcohol, at this time, the CO2 gas forms impact bubbles inside the CO2 fluid containing fatty alcohol, the bubbles are continuously exploded in the CO2 fluid containing fatty alcohol, so that the effect of stirring the CO2 fluid containing fatty alcohol is achieved, the CO2 fluid containing fatty alcohol is slightly boiled, the overflow of the gaseous CO2 is accelerated, the separation efficiency is accelerated, after the separation is half, referring to fig. 4, the introduction of CO2 from the boiling-assistant gas pipe 21 can be stopped, at this time, the upper part of the lower permeable part 12 leaks out, so that the gas cavity channel can be communicated with the inside the separator, at this time, the gaseous CO2 can not only flow out from the top, but also enter the air cavity channel, so that when the gaseous CO2 at the bottom overflows, the gaseous CO2 which does not need to penetrate through the whole oily fatty alcohol in a fluid state overflows from the top, and can overflow from the side wall and the bottom of the semi-permeable suspension barrel nearby and enter the air cavity channel, so as to be discharged from the auxiliary exhaust pipe 22 or further pass through the lower through part 12 to enter the separator to be discharged upwards, compared with the prior art which discharges the separated CO2 in one direction, the invention can effectively reduce the movement path of the gaseous CO2, and can discharge the gas CO2 in multiple directions, thereby obviously improving the separation efficiency of the gaseous CO2 and the fatty alcohol.
Referring to fig. 2, the semi-permeable suspension barrel includes an upper connection part 11 fixedly connected to an inner wall of the separator and a lower through part 12 fixedly connected to a lower end of the upper connection part 11, the upper connection part 11 is a solid structure, the lower through part 12 is a porous structure, so that gaseous CO2 can pass through the lower through part 12 and move between the semi-permeable suspension barrel and the air cavity channel, and a boundary point between the upper connection part 11 and the lower through part 12 is located between a bisection point and an upper trisection point of the semi-permeable suspension barrel, the boundary point is too high, so that the air cavity channel is communicated with the inside of the separator when CO2 is introduced from the boiling-assisting gas pipe 21 to accelerate the separation of CO2, which is not favorable for the generation of the micro-boiling phenomenon in the CO2 fluid containing fatty alcohol, the boundary point is too low, a contact surface of the CO2 introduced from the boiling-assisting gas pipe 21 and the CO2 fluid containing fatty alcohol is too small, so that the micro-boiling phenomenon in the CO2 fluid containing fatty alcohol is generated slowly, the effect of accelerating the separation efficiency is not obvious, the inner semi-permeable diaphragm 3 is adhered to the semi-permeable suspension barrel, the inner semi-permeable diaphragm 3 is made of GORE-TEX materials, CO2 gas molecules can penetrate through the inner semi-permeable diaphragm 3, water molecules of the CO2 gas molecules cannot penetrate through the inner semi-permeable diaphragm 3, water belongs to small molecules, fatty alcohol belongs to organic macromolecules, the fatty alcohol cannot penetrate through the inner semi-permeable diaphragm 3, the fatty alcohol is difficult to enter an air cavity channel, the separation rate of CO2 and the fatty alcohol is effectively improved, and the thickness of the GORE-TEX is 1-2 mm.
Example 2:
referring to fig. 1, 1000 g of crude alkyl glycoside is put into an extraction kettle, after a kettle cover is closed, the extraction kettle is heated, when the temperature of the extraction kettle reaches 55 ℃, a valve is opened, carbon dioxide is pumped into the extraction kettle from a CO2 gas source through a CO2 high-pressure pump, CO2 is in full contact with the crude alkyl glycoside, when the pressure reaches 35MPa, the valve is opened, CO2 carries extracted fatty alcohol out of the extraction, the fatty alcohol enters a separator, the pressure in the separator is set to be 5.5MPa, the flow rate of CO2 is 6kg/hr, and after the fatty alcohol is separated in the separator, CO2 is recycled. And after 30 minutes of extraction, closing the CO2 high-pressure pump, opening the extraction kettle after the pressure in the extraction kettle reaches the normal pressure, and taking out the alkyl glycoside product after fatty alcohol separation, wherein the fatty alcohol content is 1.1%. The CO2 collected from the separator can be reused.
Example 3:
referring to fig. 1, 1000 g of crude alkyl glycoside is put into an extraction kettle, after a kettle cover is closed, the extraction kettle is heated, when the temperature of the extraction kettle reaches 60 ℃, a valve is opened, carbon dioxide is pumped into the extraction kettle from a CO2 gas source through a CO2 high-pressure pump, CO2 is in full contact with the crude alkyl glycoside, when the pressure reaches 45MPa, the valve is opened, CO2 is led out of the extraction with the extracted fatty alcohol and enters a separator, the pressure in the separator is set to be 5MPa, the flow rate of CO2 is 10kg/hr, and after the fatty alcohol is separated in the separator, CO2 is recycled. And after 20 minutes of extraction, closing the CO2 high-pressure pump, opening the extraction kettle after the pressure in the extraction kettle reaches the normal pressure, and taking out the alkyl glycoside product after fatty alcohol separation, wherein the fatty alcohol content is 0.9%. The CO2 collected from the separator can be reused.
Example 4:
referring to fig. 1, 1000 g of crude alkyl glycoside is put into an extraction kettle, after a kettle cover is closed, the extraction kettle is heated, when the temperature of the extraction kettle reaches 30 ℃, a valve is opened, carbon dioxide is pumped into the extraction kettle from a CO2 gas source through a CO2 high-pressure pump, CO2 is in full contact with the crude alkyl glycoside, when the pressure reaches 15MPa, the valve is opened, CO2 carries extracted fatty alcohol out of the extraction, the fatty alcohol enters a separator, the pressure in the separator is set to be 5MPa, the flow rate of CO2 is 8kg/hr, and after the fatty alcohol is separated in the separator, CO2 is recycled. And after the extraction is carried out for 60 minutes, the CO2 high-pressure pump is closed, after the pressure in the extraction kettle reaches the normal pressure, the extraction kettle is opened, and the alkyl glycoside product after the fatty alcohol is separated is taken out, wherein the content of the fatty alcohol is 1.2 percent. The CO2 collected from the separator can be reused.
The parts not mentioned in examples 2, 3 and 4 all remained the same as in example 1.
By adopting a supercritical CO2 extraction separation technology, unreacted fatty alcohol is extracted and separated to obtain a high-purity alkyl glycoside solid product, an organic solvent is not required, post-treatment is not required, the cost is low, large-scale production is easy, and through the arrangement of a semi-permeable suspension barrel and an air cavity channel, on one hand, CO2 can be introduced into the cavity channel to enable the CO2 fluid containing the fatty alcohol to be in a micro-boiling state, so that the overflow of gaseous CO2 is accelerated, and the separation efficiency is accelerated, on the other hand, compared with the CO2 which is discharged and separated in one direction in the prior art, the gaseous CO2 which is separated after the CO2 is stopped being introduced from the boiling-assisted air pipe 21 is discharged, the invention can discharge from the upper part and the air cavity channel outwards in a multi-direction, and can effectively reduce the movement path when the gaseous CO2 overflows, so that the separation efficiency of the gaseous CO2 and the fatty alcohol is.
The above; but are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (10)
1. A method for separating fatty alcohol from alkyl glycoside crude products is characterized in that: the method comprises the following steps:
s1, placing a certain amount of crude alkyl glycoside into an extraction kettle, starting a supercritical CO2 extraction separation system, setting the extraction temperature and the extraction pressure, and pumping CO2 into the extraction kettle from a CO2 gas source;
s2, when the temperature and the pressure in the extraction kettle reach set values, continuously pumping CO2 through a CO2 high-pressure pump according to a certain flow rate to extract fatty alcohol;
s3, separating fatty alcohol from CO2 by reducing pressure of CO2 containing the fatty alcohol in a separator, and recycling CO2 of the separated fatty alcohol;
s4, when the extraction time reaches the preset value, recovering CO2 in the extraction kettle, then taking out the solid pure product of the alkyl glycoside from the extraction kettle, and reusing the fatty alcohol separated from the separator.
2. The method of claim 1, wherein the fatty alcohol is separated from the crude alkyl glycoside: the extraction temperature in the step S1 is set to be 20-80 ℃, preferably 25-60 ℃; the extraction pressure is set to 10MPa to 50 MPa.
3. The method of claim 1, wherein the fatty alcohol is separated from the crude alkyl glycoside: the constant flow rate CO2 in S2 is set to 3kg/hr to 10 kg/hr.
4. The method of claim 1, wherein the fatty alcohol is separated from the crude alkyl glycoside: the pressure reduction in S3 means that the pressure of the separator is set to 3MPa to 7 MPa.
5. The method of claim 1, wherein the fatty alcohol is separated from the crude alkyl glycoside: the extraction time in S4 was set to 20 minutes to 180 minutes.
6. The method of claim 1, wherein the fatty alcohol is separated from the crude alkyl glycoside: CO2 air supply, CO2 high-pressure pump, extraction cauldron and separator constitute supercritical CO2 extraction separation system jointly, CO2 air supply, CO2 high-pressure pump, extraction cauldron and separator all pass through the pipe connection between two liang, the output pipeline of separator communicates with each other with the input pipeline of CO2 high-pressure pump, the separator lower extreme is connected one and is helped boiling trachea (21) that the CO2 air supply communicates with each other, the separator lower extreme still is connected with the communicating helping blast pipe (22) of separator output pipeline, all be connected with the valve on pipeline, the pipeline between extraction cauldron and the separator, helping boiling trachea (21) and the helping blast pipe (22) between CO2 air supply and the CO2 high-pressure pump.
7. The method of claim 6, wherein the fatty alcohol is separated from the crude alkyl glycoside: the separator is characterized in that a semi-permeable suspension barrel is fixedly connected inside the separator, and an air cavity channel is formed by the semi-permeable suspension barrel and the inner wall below the separator in a surrounding mode.
8. The method of claim 7, wherein the fatty alcohol in the crude alkyl glycoside is selected from the group consisting of: the semi-permeable suspended barrel comprises an upper connecting part (11) fixedly connected with the inner wall of the separator and a lower permeable part (12) fixedly connected with the lower end of the upper connecting part (11).
9. The method of claim 8, wherein the fatty alcohol is separated from the crude alkyl glycoside: go up even portion (11) and be solid construction, under penetrating portion (12) be porous structure, and go up even portion (11) and under penetrating portion (12) demarcation point be located between the dichotomous point of semi-permeable suspended barrel and the trisection point of top.
10. The method of claim 9, wherein the fatty alcohol in the crude alkyl glycoside is separated from the fatty alcohol in the crude alkyl glycoside by: the semi-permeable suspended barrel is adhered with an inner semi-permeable diaphragm (3), the inner semi-permeable diaphragm (3) is made of a GORE-TEX material, and the thickness of the GORE-TEX is 1-2 mm.
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| CN113476894A (en) * | 2021-09-07 | 2021-10-08 | 江苏高科制药设备有限公司 | Supercritical extraction equipment for pharmacy |
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| CN113105778A (en) * | 2021-04-14 | 2021-07-13 | 徐鹏 | Efficient preparation process of thickening agent |
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