CN106854226B - Refining method of sucrose fatty acid ester - Google Patents
Refining method of sucrose fatty acid ester Download PDFInfo
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- CN106854226B CN106854226B CN201611123120.6A CN201611123120A CN106854226B CN 106854226 B CN106854226 B CN 106854226B CN 201611123120 A CN201611123120 A CN 201611123120A CN 106854226 B CN106854226 B CN 106854226B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
- C07H13/06—Fatty acids
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- 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
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- 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
- Y02P20/10—Process efficiency
Abstract
The invention discloses a refining method of sucrose fatty acid ester, which relates to the technical field of surfactant refining and comprises the following steps: adding water into the sucrose fatty acid ester crude product, heating, regulating pH value, carrying out solid-liquid separation after semisolid precipitation, collecting semisolid substances, washing with hot water to obtain semisolid mixture, adding organic solvent, heating, stirring, standing for layering, cooling the organic layer substance to room temperature to obtain semitransparent congealing mixture, and conveying to sucrose fatty acid ester extraction equipment for differential contact countercurrent extraction. The invention has the advantages of small organic solvent consumption, low refining cost, high purity of sucrose fatty acid ester, simple equipment and simple and convenient operation.
Description
Technical Field
The invention relates to the technical field of surfactant refining, in particular to refining of sucrose fatty acid ester
The method.
Background
Sucrose fatty acid ester is a nonionic surfactant with multifunctional property and excellent performance, and is a mixture composed of sucrose fatty acid monoester, sucrose fatty acid diester and sucrose fatty acid triester. At present, the domestic sucrose fatty acid ester mainly uses fatty acid low-carbon alcohol ester and sucrose as raw materials, adopts an organic solvent method or a solvent-free method to obtain a crude product, and the crude product comprises unreacted raw materials, a catalyst, fatty acid soap and other impurities besides sucrose fatty acid monoester, sucrose fatty acid diester and sucrose fatty acid triester, so that the sucrose fatty acid ester reaches the edible grade, and the impurities in the sucrose fatty acid ester must be controlled within the range required by the national standard.
The impurities contained in the sucrose fatty acid ester crude product mainly comprise unreacted fatty acid lower alcohol ester, sucrose, a catalyst, fatty acid soap and the like. The existing refining methods of sucrose fatty acid ester at present comprise an organic solvent-fatty acid alkali earth metal salt precipitation method, an isobutanol-ethyl acetate two-step extraction method, a water-alcohol-salt method and the like.
The patent number CN200510006011.1 and the patent number CN201310063991. X disclose an organic solvent-fatty acid alkaline earth metal salt precipitation method, wherein alkaline earth metal salt and/or alkaline earth metal oxide aqueous solution is used as a precipitator in an organic solution of sucrose fatty acid ester, so that fatty acid soap substances in a crude sucrose fatty acid ester product generate fatty acid alkaline earth metal salt with smaller solubility in the organic solvent, and the purpose of separating sucrose fatty acid ester from unreacted raw materials, catalysts and soaps is achieved; however, the fatty acid alkali earth metal salt has certain solubility in the organic solvent, the salt water is partially mixed with the organic solvent, so that salt substances are mixed in the organic phase, ash content in the sucrose fatty acid ester finally exceeds the national standard requirement due to the existence of the salt substances, the organic solvent used in the method reaches 3.8-4 times of the crude product amount, and the use amount of the organic solvent is large. Liu Zhiwei in the "study of purification Process of crude sucrose esters" (university of WU-Han Industrial school, 3 rd phase, 1999) a two-step extraction of isobutanol-ethyl acetate was introduced, which had a high solvent consumption, which not only led to a cost increase, but also affected its application in industrial production. Sun Shudong and Zhen Weijun in "research on sucrose ester Synthesis by the compatible method" (university of Xinjiang, nature science edition), vol.19, 4 th edition) a method for refining sucrose fatty acid esters by the "water-alcohol-salt method" was described, which was carried out in a ratio of 80:20:2, the sucrose fatty acid ester is dissolved by a mixed solvent prepared from water, ethanol and sodium chloride, and the product is obtained by cooling and filtering at low temperature and properly washing a filter cake, but the method has the problems that fatty acid soap is not thoroughly separated, materials are difficult to filter and wash, and sodium chloride remains in the product to cause high ash content and is difficult to reach the standard.
Disclosure of Invention
The invention aims to provide a refining method of sucrose fatty acid ester, which can solve
Solves the problems of higher ash content and lower purity of the product.
The method adopting differential contact type countercurrent extraction comprises the following steps: the method comprises the steps of conveying a mixture containing a substance to be separated, a light phase solvent and a heavy phase solvent into sucrose fatty acid ester extraction equipment, providing liquid flowing power by the temperature difference between the upper part and the lower part of the sucrose fatty acid ester extraction equipment by utilizing the characteristic that the substance to be separated has different distribution coefficients in the two phases under the condition of different temperatures, enabling the two phases to be in countercurrent differential contact mass transfer, enabling the concentration of solute in the two phases to continuously change along the flowing direction, and finally purifying the substance to be separated.
In order to solve the problems, the invention adopts the following technical scheme:
the sucrose fatty acid ester refining method uses sucrose fatty acid ester extraction equipment, wherein the sucrose fatty acid ester extraction equipment is tower equipment with a stirrer, and consists of three parts, namely an upper tower section, a middle tower section and a lower tower section, wherein the upper tower section is provided with a cooling water jacket, a first thermometer and an overflow outlet, the lower tower section is provided with a heating water jacket, a second thermometer and a discharge port communicated with a discharge regulating valve, the middle tower section is provided with a feed port communicated with a feed regulating valve, a stirring shaft of the stirrer extends downwards to the middle tower section from top to bottom, and a horizontal stirring blade is arranged on the stirring shaft;
the refining method comprises the following steps:
A. adding water into the sucrose fatty acid ester crude product, heating to 70-90 ℃, adding organic acid to a pH value of 5.5-6.5 under the condition of stirring, performing solid-liquid separation after semisolid is separated out, collecting semisolid substances, washing with hot water at 70-90 ℃, and discharging a water layer to obtain a semisolid mixture;
B. adding an organic solvent into the semi-solid mixture, controlling the temperature to be 60-75 ℃, fully stirring, standing for layering, discharging a water layer, and cooling an organic layer substance to room temperature to obtain a semi-transparent grease-like mixture;
C. conveying the semitransparent grease-like mixture into sucrose fatty acid ester extraction equipment for differential contact countercurrent extraction, when the sucrose fatty acid ester extraction equipment is used, introducing cooling water into a cooling water jacket at the upper section of a tower body, introducing hot water into a heating water jacket at the lower section of the tower body, adding the semitransparent grease-like mixture into a feed inlet and filling the tower body, starting a stirrer when the difference between the temperature displayed by a second thermometer and the temperature displayed by a first thermometer is 10-30 ℃, regulating the feed inlet and a discharge outlet to perform continuous operation, and controlling the discharge flow of the discharge outlet in the step C to be less than or equal to 40% of the feed flow of the feed inlet;
D. and (5) concentrating the materials discharged from the discharge port in vacuum to obtain the refined sucrose fatty acid ester.
Among the above technical schemes, more specific technical schemes may also be: the organic acid in the step A is lactic acid, acetic acid or citric acid.
Further, the organic solvent in the step B is butanone, ethyl acetate, isopropanol or n-butanol.
Further, in the step A, the mass ratio of water, hot water and crude sucrose fatty acid ester is 2:2:1. further, the mass ratio of the organic solvent in the step B to the crude sucrose fatty acid ester in the step A is 0.5-2: 1.
further, the discharge flow of the discharge port (7) in the step C is controlled to be less than or equal to 40% of the feed flow of the feed port (8).
Adding water into the sucrose fatty acid ester crude product, heating to 70-90 ℃ to facilitate dispersion of the sucrose fatty acid ester crude product in hot water, and adding organic acid to adjust the PH value of a sucrose fatty acid ester crude product dispersion liquid to be 5.5-6.5, so that fatty acid soap in the sucrose fatty acid ester crude product is converted into fatty acid, and separating out and floating the fatty acid soap, organic matters such as sucrose fatty acid ester, unreacted fatty acid low-carbon alcohol ester and the like in a semisolid form, and separating the fatty acid soap, the unreacted sucrose, organic acid salt and other water-soluble impurities; the PH value is regulated to be 5.5-6.5, which is favorable for separating out sucrose fatty acid ester from the water phase; if the PH value is too high, the solubility of the sucrose fatty acid ester in water is large, so that the sucrose fatty acid ester is lost; the pH value is too low, sucrose fatty acid ester is coagulated into semisolid with higher hardness in the water phase, and the semisolid coats the catalyst, unreacted sucrose and other impurities, so that the separation of the catalyst, the unreacted sucrose and the other impurities by a washing method is not facilitated.
Adding an organic solvent into the semisolid mixture, heating to 60-75 ℃ for dissolution, so that sucrose fatty acid ester, fatty acid and fatty acid low-carbon alcohol ester in the semisolid mixture are transferred to an organic phase, a good interface is formed between the semisolid mixture and a water phase, water-soluble impurities are further removed, and volatilization of the organic solvent due to overhigh temperature is prevented; the organic phase after the water layer is removed is cooled to room temperature, which is favorable for separating out the semitransparent grease-like mixture and is favorable for the differential contact countercurrent extraction of the sucrose fatty acid ester extraction equipment added in the subsequent step.
The invention adopts sucrose fatty acid ester extraction equipment to carry out differential contact type countercurrent extraction on sucrose fatty acid ester, and the extraction phase and the raffinate phase are in countercurrent differential contact, for example, in a two-phase contact mode in a hollow tower or a packed tower, so that the solute concentration in the two phases is continuously changed along the flowing direction; the semitransparent grease-like mixture in the step B enters the tower body of the sucrose fatty acid ester refining equipment from a feed inlet and is filled with the tower body, when the temperature of the tower bottom material is increased, the temperature difference exists between the tower bottom material and the materials in the middle section and the upper section of the tower body, at the moment, the tower bottom material moves to the middle section of the tower body with lower temperature as reflux rising liquid, and in the rising process, continuous countercurrent differential contact mass transfer is carried out on the tower bottom material and the mixture which naturally falls, so that the concentration of sucrose fatty acid ester, fatty acid and unreacted raw material fatty acid low-carbon alcohol ester in the mixture continuously changes along the flowing direction due to different distribution coefficients: the organic phase of the fatty acid and fatty acid lower alcohol ester entering the reflux ascending liquid continuously ascends, the sucrose fatty acid ester continuously sediments along with the water phase, but the content of the fatty acid and fatty acid lower alcohol ester continuously decreases; when the reflux ascending liquid reaches the upper section of the tower body, the mixture is cooled, sucrose fatty acid ester and water form semitransparent grease-like substances, the semitransparent grease-like substances are separated out from the organic phase, the organic phase containing fatty acid and fatty acid lower alcohol ester continuously ascends to the overflow port at the upper section of the tower body to be discharged out of the tower, and the mixture of the fatty acid and the fatty acid lower alcohol ester is obtained through recycling the organic solvent and drying; the sucrose fatty acid ester and water form semitransparent grease-like substances to be settled towards the bottom of the tower, the sucrose fatty acid ester and water perform continuous countercurrent differential contact mass transfer with reflux ascending liquid with higher temperature in the middle, when the sucrose fatty acid ester reaches the bottom of the tower, the purity of the sucrose fatty acid ester in the water phase is high, and finally the sucrose fatty acid ester is discharged from the tower as a product solution from the bottom of the tower.
The temperature of the material at the bottom of the tower and the temperature of the material at the upper part of the tower body are detected by a temperature monitor, the temperature difference provides mass transfer power for differential contact countercurrent extraction of the material, the mass transfer effect is determined by the temperature difference, and the temperature difference between the material at the bottom of the tower and the material at the upper part of the tower body is controlled to be 10-30 ℃ in view of the production capacity and the product quality of equipment, and the reason is that: the smaller the temperature difference is, the slower the rising speed of the reflux liquid is, the longer the mass transfer time is, and the better the mass transfer effect is, but the productivity of the equipment in unit time is affected; the larger the temperature difference is, the faster the rising speed of the reflux rising liquid is, the faster the mass transfer speed is, and the larger the equipment production capacity is, but the materials are easy to form turbulent flow and channeling, and impurities are easy to mix into the products, so that the purification of the products is not facilitated; the temperature difference between 10 and 30 ℃ has good mass transfer effect and large equipment production capacity.
The flow rate of discharged materials at the bottom of the tower body of the sucrose fatty acid ester extraction equipment is also a factor for determining the production capacity of the equipment, and the invention controls the discharge flow rate of the discharge port to be less than or equal to 40% of the feed flow rate of the feed port, because the larger the discharge flow rate at the bottom of the tower is, the larger the production capacity of the equipment is, but the lower the rising speed of reflux rising liquid is reduced or even reduced, the mixture to be extracted entering from the feed port at the middle part of the tower body is discharged from the bottom of the tower without extraction, so that the quality of the product is disqualified, and the discharge flow rate is large, meanwhile, the relative stability of temperature difference is influenced, so that the instability of a system is caused, therefore, in order to stably operate the extraction process, the discharge port regulating valves at the feed port and the bottom of the tower are regulated under the condition that the temperature of the materials at the bottom of the tower is ensured, and the flow rate of the extract discharged from the bottom of the tower is controlled to be less than or equal to 40% of the mixture to be extracted.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the sucrose fatty acid ester has higher purity: firstly, the water-soluble impurities are easy to separate by a method of acidifying the sucrose fatty acid ester crude dispersion liquid; other metal salt substances are not required to be additionally added to be used as a precipitator, so that the problem of higher ash content of the product caused by entrainment of the metal salt substances in the product is avoided; and finally, carrying out differential contact countercurrent extraction by taking the temperature difference as mass transfer power, so that fat-soluble impurities such as fatty acid low-carbon alcohol ester, fatty acid and the like are easier to separate from sucrose fatty acid ester, and finally, the sucrose fatty acid ester with high purity is obtained.
2. The invention has the advantages of small organic solvent consumption and low refining cost: the invention carries out differential contact countercurrent extraction in a tower device of sucrose fatty acid ester extraction equipment, only uses a primary solvent before extracting the sucrose fatty acid ester, and the mass ratio of the organic solvent to the crude sucrose fatty acid ester is 0.5-2: 1, the use amount of the organic solvent is less than 50% of the prior art, and the refining cost is low.
3. The refining equipment is simple, and the operation is simple and convenient: the differential contact countercurrent extraction is carried out by taking the temperature difference as mass transfer power, and the sucrose fatty acid ester extraction equipment with the built-in stirrer is adopted, so that compared with the traditional tower type extraction equipment such as a packed tower, a sieve plate tower, a turntable tower and the like, the structure is simpler, the continuous operation can be carried out, and compared with the traditional intermittent refined sucrose fatty acid ester equipment, the operation is simpler and more convenient.
Drawings
FIG. 1 is a schematic diagram of the sucrose fatty acid ester extraction apparatus of the present invention.
Detailed Description
The invention is further described in detail below with reference to the attached drawings and examples:
the sucrose fatty acid ester refining uses sucrose fatty acid ester extraction equipment, the sucrose fatty acid ester extraction equipment is tower equipment with a stirrer 4, the sucrose fatty acid ester extraction equipment consists of three parts, namely a tower body upper section 1, a tower body middle section 2 and a tower body lower section 3, wherein the tower body upper section 1 is provided with a cooling water jacket 5, a first thermometer 10 and an overflow port 9, the tower body lower section 3 is provided with a heating water jacket 6, a second thermometer 11 and a discharge port 7 communicated with a discharge regulating valve, the tower body middle section 2 is provided with a feed port 8 communicated with a feed regulating valve, a stirring shaft of the stirrer 4 extends downwards from top to bottom to the tower body middle section 2, and a horizontal stirring blade is arranged on the stirring shaft;
the refining method of the sucrose fatty acid ester comprises the following steps:
A. taking 10 kg of sucrose fatty acid ester crude product, adding 20 kg of water, heating to 70-90 ℃, adding an organic acid aqueous solution under stirring, controlling the pH value to be 5.5-6.5, performing solid-liquid separation after semisolid is separated out, collecting semisolid substances, washing once with hot water at 70-90 ℃, and discharging a water layer to obtain a semisolid mixture;
B. adding 5-20 kg of organic solvent into the semi-solid mixture, controlling the temperature to be 60-75 ℃, fully stirring, standing for layering, discharging a water layer, cooling organic layer substances to room temperature to obtain a semitransparent grease-like mixture, wherein the semitransparent grease-like mixture mainly comprises sucrose fatty acid ester, stearic acid, methyl stearate, water and organic solvent;
C. delivering the mixture obtained in the step B to sucrose fatty acid ester extraction equipment for extraction, introducing cooling water into a cooling water jacket 5 at the upper section of a tower body, introducing hot water into a heating water jacket 6 at the lower section of the tower body, adding the semitransparent grease-like mixture obtained in the step B into a feed inlet 8 and filling the tower body, starting a stirrer 4 when the difference between the temperature displayed by a second temperature measuring device 11 and the temperature displayed by a first temperature measuring device 10 is 10-30 ℃, and rotating at 36 rpm, and continuously operating a regulating valve of the feed inlet 8 and a regulating valve of a discharge outlet 7 at the bottom of the tower under the condition that the temperature of a material at the bottom of the tower and the temperature of the material at the upper section 1 of the tower body are relatively constant, and controlling the discharge flow of the discharge outlet 7 in the step C to be less than or equal to 40% of the feed flow of the feed inlet 8; when the mixture obtained in the step B is added into the extraction equipment from a feed inlet 8, the mixture is settled to a lower section 3 of a tower body, heated to form a reflux ascending liquid at the bottom of the tower, moves to a middle section 2 of the tower body, continuously and counter-currently carries out differential contact mass transfer with the fallen mixture, fatty acid and fatty acid lower alcohol ester in the mixture are transferred to an organic phase in the ascending reflux liquid and continuously ascend to the middle section 2 of the tower body, the mixture is fully mixed with the mixture to be extracted which is just entered into the tower under the action of a stirrer 4, sucrose fatty acid ester and water form a semitransparent grease-like substance under the cooling action of cooling water in the upper section 1 of the tower body, the organic phase containing fatty acid and fatty acid lower alcohol ester is precipitated from the organic phase and is settled in the bottom direction of the tower, the organic phase containing the fatty acid and the fatty acid lower alcohol ester continuously ascends to the overflow port 9 of the upper section 1 of the tower body to be discharged out of the tower, and the mixture of the fatty acid and the fatty acid lower alcohol ester is obtained through recovery and drying of the organic solvent; the sucrose fatty acid ester and water form semitransparent grease-like substances to be settled towards the lower section 3 of the tower body, the continuous countercurrent differential contact mass transfer is carried out on the sucrose fatty acid ester and the reflux ascending liquid with higher temperature in the middle, when the sucrose fatty acid ester reaches the bottom of the tower body, the purity of the sucrose fatty acid ester in the water phase is very high, and finally the sucrose fatty acid ester is taken as a product solution to reach the bottom of the tower and is discharged out of the tower through an outlet material 7;
D. and (3) recycling the organic solvent from the material discharged from the discharge port 7 at normal pressure, and then performing vacuum drying at the temperature of below 95 ℃ to obtain a pure sucrose fatty acid ester product.
Examples 1 to 5
The crude sucrose fatty acid ester in examples 1 to 5 is synthesized by using fatty acid methyl ester and sucrose as an emulsifier and potassium stearate as a catalyst through a solvent-free method, and comprises the following components: 48.2% of sucrose fatty acid ester, 18.2% of free sugar, 5.3% of methyl stearate, 23.5% of fatty acid potassium and 4.8% of other.
Examples 6 to 10
The crude sucrose fatty acid ester in examples 6 to 10 is synthesized by using fatty acid ethyl ester and sucrose as an emulsifier and potassium stearate as a catalyst and by a water solvent method, and comprises the following components: 46.7% of sucrose fatty acid ester, 20.2% of free sugar, 7.1% of ethyl stearate, 23.2% of potassium stearate and 3.8% of other components.
The parameters of each step of examples 1-10 are shown in Table 1:
table 1 parameter table for each step of examples 1 to 10
The test results of each example are shown in Table 2:
table 2 results of the tests of examples 1 to 10
Comparative example one
A translucent gel mixture was prepared under the same conditions as in step A and step B of example 1, without differential contact extraction using sucrose fatty acid ester extraction equipment, and after recovering ethyl acetate, vacuum drying was performed at 95℃or less, the resultant dried product had a sucrose fatty acid ester total ester content of 81.36%, free sugar of 0.24%, an acid value of 24.67mgKOH/g, an ash content of 0.35% and methyl stearate of 5.52%. In this comparative example, the resultant sucrose fatty acid ester has a low total ester content and fatty acid methyl ester are not efficiently removed, as compared with the example, without the differentially contact extracted mixture.
Comparative example two
Refining of sucrose fatty acid ester was carried out according to the method of "study on purification Process of crude sucrose ester" ("university of Wuhan academy of Industrial science", 1999, 3 rd phase).
Adding 500ml of ethyl acetate and 300ml of water into 100g of sucrose fatty acid ester crude product, heating and dissolving at 70 ℃, adjusting the PH=5 by using citric acid, discharging a water layer, adding 14% sodium chloride into an organic phase, stirring for 10min at 70 ℃, cooling to 5 ℃, separating out solids, filtering, adding 100ml of 1:1 isobutanol and water into a filter cake, heating and dissolving at 65 ℃, adjusting the PH=7, discharging the water layer, washing the organic phase for 2 times by using water, recovering the isobutanol, and drying in vacuum to obtain a sucrose fatty acid ester product. Wherein, the total ester content of sucrose fatty acid ester is 83.02%, the acid value is 3.8mgKOH/g, the free sugar is 5.3%, the ash content is 3.3, and the fatty acid methyl ester is 6.27. In this comparative example, compared with the examples, the fatty acid methyl ester was not removed effectively at all times while remaining in the organic phase, and the total amount of the organic solvents ethyl acetate and isobutanol used was 6 times as large as the crude product.
Comparative example three
Sucrose fatty acid esters were purified according to the method of "study on the synthesis of sucrose esters by the method of" university of Xinjiang (Nature science edition) Vol.19, 4 th edition "2002".
Adding 500ml of aqueous solution containing ethanol and sodium chloride (weight ratio of 80:20:2) into 100g of sucrose fatty acid ester crude product, stirring for 10min at 80 ℃, cooling to 5 ℃, obtaining a filter cake, adding 600ml of 3% acetic acid solution, stirring for 10min at 80 ℃, cooling to 5 ℃, filtering, washing the filter cake once by 100ml of 3% acetic acid solution, ethanol and sodium chloride aqueous solution respectively, and vacuum drying the washed filter cake to obtain sucrose fatty acid ester product. Wherein, the sucrose fatty acid ester is 80.1%, the acid value is 5.6mgKOH/g, the free sugar is 7.5%, the ash content is 4.6%, and the fatty acid methyl ester is 4.96%. Because sucrose fatty acid ester encapsulates fatty acid soap, unreacted sucrose and sodium chloride due to coacervation in the refining process and washing is difficult, the impurity content in the product is high, and fatty acid methyl ester cannot be removed effectively.
Claims (4)
1. A refining method of sucrose fatty acid ester is characterized in that:
the sucrose fatty acid ester extraction equipment is used, the sucrose fatty acid ester extraction equipment is tower equipment with a stirrer (4) arranged inside, and consists of three parts, namely an upper tower section (1), a middle tower section (2) and a lower tower section (3), wherein the upper tower section (1) is provided with a cooling water jacket (5) and is provided with a first thermometer (10) and an overflow port (9), the lower tower section (3) is provided with a heating water jacket (6) and is provided with a second thermometer (11) and a discharge port (7) communicated with a discharge regulating valve, the middle tower section (2) is provided with a feed port (8) communicated with the feed regulating valve, a stirring shaft of the stirrer (4) extends downwards from top to the middle tower section (2), and a horizontal stirring blade is arranged on the stirring shaft;
the refining method comprises the following steps:
A. adding water into the sucrose fatty acid ester crude product, heating to 70-90 ℃, adding organic acid to a pH value of 5.5-6.5 under the condition of stirring, performing solid-liquid separation after semisolid is separated out, collecting semisolid substances, washing with hot water at 70-90 ℃, and discharging a water layer to obtain a semisolid mixture;
B. adding an organic solvent into the semi-solid mixture, controlling the temperature to be 60-75 ℃, fully stirring, standing for layering, discharging a water layer, and cooling an organic layer substance to room temperature to obtain a semi-transparent grease-like mixture; wherein the organic solvent is butanone, ethyl acetate, isopropanol or n-butanol;
C. delivering the semitransparent grease-like mixture into sucrose fatty acid ester extraction equipment for differential contact countercurrent extraction, when the sucrose fatty acid ester extraction equipment is used, introducing cooling water into a cooling water jacket (5) at the upper section of a tower body, introducing hot water into a heating water jacket (6) at the lower section of the tower body, adding the semitransparent grease-like mixture into a feed inlet (8) and filling the tower body, when the difference between the temperature displayed by a second thermometer (11) and the temperature displayed by a first thermometer (10) is 10-30 ℃, starting a stirrer (4), regulating the feed inlet (8) and a discharge outlet (7) for continuous operation, and controlling the discharge flow of the discharge outlet (7) in the step C to be less than or equal to 40% of the feed flow of the feed inlet (8);
D. and (3) concentrating the material discharged from the discharge port (7) in vacuum to obtain the refined sucrose fatty acid ester.
2. The method for purifying sucrose fatty acid ester as claimed in claim 1, wherein: the organic acid in the step A is lactic acid, acetic acid or citric acid.
3. The method for purifying sucrose fatty acid ester as claimed in claim 2, wherein: in the step A, the mass ratio of water, hot water and crude sucrose fatty acid ester is 2:2:1.
4. the method for purifying sucrose fatty acid ester as claimed in claim 1, 2 or 3, wherein: the mass ratio of the organic solvent in the step B to the sucrose fatty acid ester crude product in the step A is 0.5-2: 1.
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