CN101781340A - Purification method of sucrose fatty acid ester - Google Patents
Purification method of sucrose fatty acid ester Download PDFInfo
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Abstract
The invention relates to a purification method of a mixture containing sucrose fatty acid ester; the mixture containing sucrose fatty acid ester is prepared from a sucrose fatty acid ester crude product which is prepared from the preparation of sucrose fatty acid ester with solvent or without solvent; the sucrose fatty acid ester crude product is pre-treated and prepared, and then is purified to prepare the sucrose fatty acid ester; the purification step is to carry out secondary molecular distillation to the sucrose fatty acid ester crude product; the temperature of primary distillation is 100 to 140DEG C, the distillation pressure is 600 to 800Pa, the temperature of secondary distillation is 100 to 150DEG C and the pressure is 0.01 to 1Pa; light phase and heavy phase of secondary distillation are separated, and the heavy phase prepared is the purified sucrose fatty acid ester product. The purification process of the method of the invention has the advantages of short product heating time, good product color, high vacuum degree, little solvent residue in the product, reasonable production process, wastewater containing sugar and salt produced in the production process, and convenient environmental-friendly treatment.
Description
(1) technical field
The present invention relates to a kind of method of purification of sucrose fatty ester, particularly relate to method with molecular distillation purification sucrose fatty ester.
(2) background technology
It is that a kind of HLB (hydrophilic-lipophilic balance) codomain is wide, effective, safe, the emulsifying agent of applied range that sucrose fatty ester is called for short sucrose ester (sucrose fatty acid ester), usually use as additive in the process for processing of Chemicals, cosmetics of everyday use, food and medicine, equal approved sucrose ester such as The World Health Organization (WHO), United Nations's grain tissue (FAO), the European Community, Japan, China and the U.S. is as foodstuff additive.
Molecular distillation is a kind of special liquid--a liquid isolation technique, and it is different from the tradition distillation and relies on the boiling-point difference separation principle, but realizes separating by the difference of different substances molecular motion mean free path.Molecular distillation technique, have the incomparable advantage of other isolation technique: 1, (zero load≤1Pa), heated time short (in second), separation efficiency are high, are suitable for the separation of high boiling point, thermo-sensitivity, readily oxidizable substance especially for service temperature low (far below boiling point), vacuum tightness height; 2, can remove lower-molecular substance (deodorization), weight molecule material (decolouring) and remove impurity in the mixture effectively; 3, its sepn process is a physical separating process, can protect separated material not contaminated well, particularly can keep the original quality of natural extract; 4, separation degree height is higher than tradition distillation and common thin-film evaporator.
The method sucrose ester ester-interchange method of the suitability for industrialized production of present sucrose ester, the ester-interchange method synthesis of sucrose ester is divided into solvent method and solventless method, but contain sucrose monoester in the product that these two kinds of methods are produced, saccharose diester, sucrose polyfatty acid esters and unreacted sucrose, fatty acid soaps, lipid acid, fatty acid methyl ester and/or mono-glycerides and/or fatty acid propylene glycol ester, impurity such as catalyzer, the method of described respectively a kind of sucrose ester of purifying in Chinese patent ZL200510006011.1 and European patent EP 0448996, its method be with the sucrose ester dissolving crude product in the organic solvent that can dissolve it, in 100 parts sucrose ester crude product, add 20 to 200 weight part alkaline earth metal compounds then and react; The excessive adding of alkaline earth metal compound makes the possibility of sucrose ester purification reaction end posthydrolysis very big, and the sucrose ester instability is unfavorable for obtaining highly purified sucrose ester; Alkaline earth metal compound generally is insoluble to organic solvent, directly with organic solvent in impurity fatty acid soaps or stearic acid reaction, react and be difficult to carry out, impurity is difficult for removing, and reacts not thorough, can not effectively remove impurity.
The present invention removes lipid acid and unreacted fatty acid methyl ester and/or mono-glycerides and/or fatty acid propylene glycol ester distillation with molecular distillation technique, obtains the sucrose ester product through the molecular distillation purifying.
(3) summary of the invention
Technical problem to be solved by this invention provides a kind of method of purification of utilizing molecular distillation technique to carry out sucrose fatty ester, has advantage effective, that technology is simple, by product is conveniently recycled.
In order to realize above purpose, technical scheme of the present invention is:
A kind of method of purification that contains the sucrose-fatty ester mixture, the described sucrose-fatty ester mixture that contains prepares the sucrose fatty ester crude product that sucrose fatty ester obtains from solvent method or solventless method, described sucrose fatty ester crude product in the presence of organic solvent through acidifying, the washing pre-treatment step gets the sucrose fatty ester crude product, again the sucrose fatty ester crude product is purified and make sucrose fatty ester, described method of purification comprises the steps: the sucrose fatty ester crude product is carried out the secondary molecular distillation, one-level distillatory temperature is 100～140 ℃, distillation pressure is 600～800Pa, the temperature of secondary distillation is 100～150 ℃, pressure 0.01～1Pa, secondary distillation is light to be separated with heavy phase mutually, and the gained heavy phase is the sucrose fatty ester product of purifying.Need in the molecular distillation operating process to regulate the distillation flow according to the molecular distillation equipment production capacity, this is to well known to a person skilled in the art working method, according to the difference of equipment, to do suitably to adjust, the flow control the during distillation of embodiment of the invention one-level is at 0.05～2kg/h.
No matter be the no-solvent process or the sucrose fatty ester of solvent method preparation, the thick product of the sucrose fatty ester of acquisition, all available method of purification purification sucrose fatty ester of the present invention.The solventless method that the present invention refers to is under condition of no solvent, directly uses sucrose, and fatty acid ester, fatty acid soaps reach and react under catalyst action, distillation then, and cooling obtains the sucrose fatty ester crude product.Described fatty acid ester can be methyl esters, propylene glycol ester or triglyceride level (winterized stearin), but commonly used be fatty acid methyl ester.The solvent method of indication of the present invention is that fatty acid ester, organic solvent, sucrose are carried out the homogeneous phase transesterify under the salt of wormwood catalyst action, underpressure distillation then, after reclaiming solvent, obtain the sucrose fatty ester crude product, the fatty acid ester that solvent method is used selects fatty acid methyl ester usually.
Before the present invention was recommended in the method for purification processing, preferably elder generation got the sucrose fatty ester crude product with the pre-treatment step of the acidifying in the presence of organic solvent of sucrose fatty ester crude product, washing, and the sucrose fatty ester crude product is purified makes sucrose fatty ester again; Here acidifying purpose is that the fatty acid soaps acidifying in the sucrose-fatty ester mixture is become the purpose of lipid acid, washing is to remove residual sucrose, salt and water colo(u)r; Described method of purification comprises the steps: the sucrose fatty ester crude product is carried out the secondary molecular distillation, one-level distillatory temperature is 100～140 ℃, distillation pressure is 600～800Pa, the temperature of secondary distillation is 100～150 ℃, pressure 0.01～1Pa, secondary distillation is light to be separated with heavy phase mutually, and the gained heavy phase is the sucrose ester product of purifying.
Pre-treatment step of the present invention is: the sucrose fatty ester crude product is added in the mixing solutions of organic solvent and water, heating for dissolving is behind acid adjusting PH 3～4, standing demix, get organic layer, after washing, carry out underpressure distillation and remove organic solvent, get the sucrose fatty ester crude product.
Described organic solvent is propyl carbinol, ethyl acetate, butanone.
The present invention is used for acidifying acid preferably sulfuric acid, citric acid, acetic acid or hydrochloric acid.
Recommend described volume of organic solvent consumption to count 0.5～10ml/g with the quality of sucrose ester crude product.The volume ratio of organic solvent and water is 1: 0.01～1 in the mixing solutions of organic solvent and water.
One-level distillation temperature of the present invention is preferably 110～120 ℃, and distillation pressure is 600～800Pa, and described secondary distillation temperature is 110～140 ℃, and distillation pressure is 0.1～0.5Pa.Concrete, the present invention recommends the following method of purification that contains the sucrose-fatty ester mixture, the sucrose fatty ester crude product of solvent method or solventless method acquisition is added in the mixing solutions of organic solvent and water, heating for dissolving, behind acid adjusting PH 3～4, standing demix is got organic layer, after washing, carry out underpressure distillation and remove organic solvent, get the sucrose fatty ester crude product; The sucrose fatty ester crude product is carried out the secondary molecular distillation, one-level distillatory temperature is 110～120 ℃, distillation pressure is 600～800Pa, the temperature of secondary distillation is 100～150 ℃, pressure 0.1～0.5Pa, secondary distillation is light to be separated with heavy phase mutually, and the gained heavy phase is the sucrose ester product of purifying, described organic solvent is propyl carbinol, ethyl acetate or butanone, and described acid is sulfuric acid, citric acid, acetic acid or hydrochloric acid.
Advantage of the present invention and positively effect: 1, product distills product heated time weak point in the purification process among the present invention, and product color is good; 2, the vacuum tightness height of product distillation purification process among the present invention, dissolvent residual is few in the product; 3, the lipid acid of distillation gained and fatty acid methyl ester and/or mono-glycerides and/or the direct recovery set of fatty acid propylene glycol ester are used for the synthetic of sucrose ester crude product; 4, production technique is reasonable, the waste water that contains sugar and salt that produces in the production process, and environmental protection treatment is convenient.Therefore the present invention both had been fit to the purification of solventless method synthetic sucrose ester crude product, also was fit to the purification of solvent method synthetic sucrose ester crude product, and the sucrose ester product of acquisition meets European Union, the U.S. and JIS, has vast market prospect.
(4) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this.
Embodiment one:
1, solventless method synthetic sucrose fatty ester crude product
With 171 gram sucrose, 150 gram methyl stearates, 54 gram potassium stearates and 22.5 gram salt of wormwood, be 140～145 ℃ in temperature, pressure is heated and stirred reaction 8 hours under the condition of 2000Pa, cool off sucrose fatty ester crude product 372.5 grams
2, the pre-treatment of sucrose fatty ester crude product
Get above-mentioned sucrose fatty ester crude product 300 grams, add in 200 milliliters of ethyl acetate and 200 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 3 with mass concentration 10% citric acid, leave standstill, divide sub-cloud water; Add 100 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 176 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content (%)
Sucrose ester 67.3
Unreacted sucrose 0.4
Potassium stearate 0.6
Stearic acid 25.3
Methyl stearate 6.4
Wherein in the sucrose ester monoester content be 45.4%, dibasic acid esters 21.8%, polyester 32.8%.
3, purifying: get the above-mentioned sucrose ester crude product of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 100 ℃, pressure 800Pa, flow 0.1kg/h; The temperature of secondary distillation is 110 ℃, pressure 0.01Pa.Secondary distillation gained heavy phase is sucrose ester product 70.3 grams of purifying, after testing: acid number 2.1mgKOH/g, free sugar 0.6%, ash content 0.28%, total ester content 95.4%, monoester content 48.6%.
Embodiment two:
1, solventless method synthetic sucrose fatty ester crude product
With 200 gram sucrose, 150 gram methyl stearates, 50 gram potassium stearates and 25 gram salt of wormwood, be 140～145 ℃ in temperature, pressure is heated and stirred reaction 8 hours under the condition of 2000Pa, cool off sucrose-fatty product 398 grams.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 300 grams, add in 400 milliliters of butanone and 200 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 4 with mass concentration 5% hydrochloric acid, leave standstill, divide sub-cloud water; Add 200 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 170 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content, %
Sucrose ester 71.3
Unreacted sucrose 0.6
Potassium stearate 0.9
Stearic acid 22.5
Methyl stearate 4.7
In the above-mentioned sucrose ester monoester content be 51.0%, dibasic acid esters 28.6%, polyester 20.4%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 110 ℃, pressure 600Pa, flow 1.0kg/h; The temperature of secondary distillation is 120 ℃, pressure 0.05Pa.Secondary distillation gained heavy phase is sucrose ester product 74.9 grams of purifying, after testing: acid number 3.2mgKOH/g, free sugar 0.9%, ash content 0.45%, total ester content 94.6%, monoester content 53.5%.
Embodiment three:
1, methyl-sulphoxide is a solvent synthetic sucrose fatty ester crude product
Get sucrose 250 grams and be dissolved in 750 milliliters of methyl-sulphoxides, and in wherein adding methyl stearate 75 grams.Add salt of wormwood 4 grams in this mixture, in 85 ℃ of reactions 4.5 hours, decompression simultaneously distillated the methyl alcohol that generates in the reaction down.Reaction finishes to add immediately stearic acid 17 grams, and under decompression and 80 ℃ it is concentrated the back oven dry, sucrose fatty ester crude product 345 restrains.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 300 grams, add in 3000 milliliters of propyl carbinols and 200 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 3 with 20% sulfuric acid, leave standstill, divide sub-cloud water; Add 200 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 150 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content, %
Sucrose ester 85.6
Unreacted sucrose 0.5
Potassium stearate 0.1
Stearic acid 11.4
Methyl stearate 2.4
In the above-mentioned sucrose ester monoester content be 73.0%, dibasic acid esters 20.3%, polyester 6.7%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 115 ℃, pressure 700Pa, flow 2.0kg/h; The temperature of secondary distillation is 120 ℃, pressure 0.8Pa.Secondary distillation gained heavy phase is sucrose ester product 92.6 grams of purifying, after testing: acid number 3.0mgKOH/g, free sugar 0.6%, ash content 0.04%, total ester content 97.7%, monoester content 73.5%.
Embodiment four:
1, propylene glycol ester method synthetic sucrose fatty ester crude product
Behind Powdered sucrose 204 grams, propylene glycol cetylate 94 grams and potassium palmitate thorough mixing, put into reaction flask, and soak in 175 ℃ of oil baths, be melt into the mobile paste, pressure slowly reduces to 1333～666Pa reaction 20 minutes, cools off to such an extent that sucrose fatty ester crude product 346 restrains.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 300 grams, add in 600 milliliters of butanone and 100 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 4 with 10% citric acid, leave standstill, divide sub-cloud water; Add 100 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 185 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content, %
Sucrose ester 73.2
Unreacted sucrose 0.8
Potassium palmitate 0.6
Palmitinic acid 17.5
Palmitinic acid propylene glycol ester 7.9
In the above-mentioned sucrose ester monoester content be 43.7%, dibasic acid esters 32.7%, polyester 23.6%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 120 ℃, pressure 800Pa, flow 0.2kg/h; The temperature of secondary distillation is 125 ℃, pressure 0.1Pa.Secondary distillation gained heavy phase is sucrose ester product 75.4 grams of purifying, after testing: acid number 1.6mgKOH/g, free sugar 1.1%, ash content 0.24%, total ester content 96.7%, monoester content 45.3%.
Embodiment five:
1, with water is solvent synthetic sucrose fatty ester crude product
In 1500 ml flasks, add 200 gram sucrose, 100 gram sodium stearate and water 100 grams, stir the mixing solutions that makes it to form homogeneous.Under 100～120 ℃, most of water is distillated then, add salt of wormwood 4 grams.Temperature is elevated to 150 ℃, slowly steams remaining moisture under 6665Pa, and adds 100 gram methyl stearates simultaneously, and insulation reaction 3 hours is cooled off to such an extent that sucrose fatty ester crude product 392 restrains.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 300 grams, add in 1200 milliliters of propyl carbinols and 200 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 3 with 10% citric acid, leave standstill, divide sub-cloud water; Add 200 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 172 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content, %
Sucrose ester 58.2
Unreacted sucrose 0.8
Sodium stearate 0.8
Stearic acid 24.8
Methyl stearate 15.4
In the above-mentioned sucrose ester monoester content be 46.7%, dibasic acid esters 37.2%, polyester 16.1%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 120 ℃, pressure 800Pa, flow 0.5kg/h; The temperature of secondary distillation is 130 ℃, pressure 0.5Pa.Secondary distillation gained heavy phase is sucrose ester product 60.2 grams of purifying, after testing: acid number 1.4mgKOH/g, free sugar 1.3%, ash content 0.4%, total ester content 95.6%, monoester content 58.3%.
Embodiment six:
1, solventless method synthetic sucrose fatty ester crude product
With 171 gram sucrose, 171 gram methyl stearates, 50 gram potassium stearates and 25 gram salt of wormwood, be 138～145 ℃ in temperature, pressure is heated and stirred reaction 9 hours under the condition of 2000Pa, cool off sucrose-fatty product 386 grams.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 300 grams, add in 1500 milliliters of ethyl acetate and 250 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 3 with 5% hydrochloric acid, leave standstill, divide sub-cloud water; Add 250 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 167 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content, %
Sucrose ester 66.4
Unreacted sucrose 0.7
Potassium stearate 0.8
Stearic acid 23.8
Methyl stearate 8.3
In the above-mentioned sucrose ester monoester content be 46.4%, dibasic acid esters 32.7%, polyester 20.9%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 120 ℃, pressure 600Pa, flow 0.5kg/h; The temperature of secondary distillation is 140 ℃, pressure 0.1Pa.Secondary distillation gained heavy phase is sucrose ester product 67.4 gram, acid number 0.6mgKOH/g, free sugar 1.1%, ash content 0.4%, total ester content 97.6%, the monoester contents 47.9% after testing of purifying.
Embodiment seven:
1, with water is solvent synthetic sucrose fatty ester crude product
In 1500 ml flasks, add 200 gram sucrose, 100 gram sodium stearate and water 240 grams, stir the mixing solutions that makes it to form homogeneous.Add winterized stearin 110 gram and salt of wormwood 4 grams then, temperature is elevated to 150 ℃, decompression dehydration under 1333Pa, form melts after, under 667Pa and 160 ± 2 ℃ of insulation reaction 2 hours, cool off to such an extent that sucrose fatty ester crude product 410 restrains.
2, the pre-treatment of sucrose fatty ester crude product: get above-mentioned sucrose fatty ester crude product 400 grams, add in 1200 milliliters of propyl carbinols and 200 ml waters, stir down at 50 ℃ and make it dissolving; After regulating PH and be 3 with 10% citric acid, leave standstill, divide sub-cloud water; Add 200 ml waters washing 2 times again, remove residual sucrose, salt and water colo(u)r; With the upper strata organic solvent layer, 95 ℃ of underpressure distillation, to remove organic solvent and get sucrose fatty ester crude product 172 grams, it is as follows that described sucrose fatty ester crude product is measured content:
Component title content %
Sucrose ester 56.3
Unreacted sucrose 0.6
Sodium stearate 0.5
Stearic acid 28.5
Stearin 14.1
In the above-mentioned sucrose ester monoester content be 56.7%, dibasic acid esters 32.2%, polyester 11.1%.
3, purifying: get the above-mentioned sucrose ester sample of 100 grams, distill with molecular distillation apparatus, wherein one-level distillatory temperature is 120 ℃, pressure 800Pa, flow 0.8kg/h; The temperature of secondary distillation is 130 ℃, pressure 0.5Pa.Secondary distillation gained heavy phase is sucrose ester product 57.6 grams of purifying, after testing: acid number 3.4mgKOH/g, free sugar 1.0%, ash content 0.32%, total ester content 95.6%, monoester content 57.3%.
Claims (10)
1. method of purification that contains the sucrose-fatty ester mixture, the described sucrose-fatty ester mixture that contains prepares the sucrose fatty ester crude product that sucrose fatty ester obtains from solvent method or solventless method, described sucrose fatty ester crude product in the presence of organic solvent through acidifying, the washing pre-treatment step gets the sucrose fatty ester crude product, again the sucrose fatty ester crude product is purified and make sucrose fatty ester, it is characterized in that described method of purification comprises the steps: the sucrose fatty ester crude product is carried out the secondary molecular distillation, one-level distillatory temperature is 100～140 ℃, distillation pressure is 600～800Pa, the temperature of secondary distillation is 100～150 ℃, pressure 0.01～1Pa, secondary distillation is light to be separated with heavy phase mutually, and the gained heavy phase is the sucrose fatty ester product of purifying.
2. the method for purification that contains the sucrose-fatty ester mixture as claimed in claim 1, it is characterized in that described solventless method is under condition of no solvent, directly reach and under catalyst action, react with sucrose, fatty acid ester, fatty acid soaps, distillation then, cooling obtains the sucrose fatty ester crude product.
3. the method for purification that contains the sucrose-fatty ester mixture as claimed in claim 1, it is characterized in that described solvent method is that fatty acid ester, organic solvent, sucrose are carried out the homogeneous phase transesterification reaction under the salt of wormwood catalyst action, underpressure distillation then, after reclaiming solvent, obtain the sucrose fatty ester crude product.
4. method of purification as claimed in claim 1, it is characterized in that described pre-treatment step is: the sucrose fatty ester crude product is added in the mixing solutions of organic solvent and water, heating for dissolving, behind acid adjusting PH 3～4, standing demix, get organic layer, after washing, carry out underpressure distillation and remove organic solvent, get the sucrose fatty ester crude product.
5. method of purification as claimed in claim 4 is characterized in that described organic solvent is propyl carbinol, ethyl acetate, butanone.
6. method of purification as claimed in claim 4 is characterized in that described volume of organic solvent consumption counts 0.5～10ml/g with the quality of sucrose ester crude product, and the volume ratio of organic solvent and water is 1: 0.01～1 in the mixing solutions of organic solvent and water.
7. method of purification as claimed in claim 4 is characterized in that described acid is sulfuric acid, citric acid, acetic acid or hydrochloric acid.
8. method of purification as claimed in claim 1 is characterized in that described one-level distillation temperature is 110～120 ℃.
9. method of purification as claimed in claim 1 is characterized in that described secondary distillation temperature is 110～140 ℃.
10. method of purification as claimed in claim 1 is characterized in that described secondary pressure is 0.1～0.5Pa.
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| CN104004033A (en) * | 2013-06-21 | 2014-08-27 | 浙江迪耳化工有限公司 | Purification and separation method for sucrose fatty acid ester |
| CN106854226A (en) * | 2016-12-08 | 2017-06-16 | 广西科技师范学院 | The process for purification of sucrose fatty ester |
| CN107325134A (en) * | 2017-06-21 | 2017-11-07 | 广州市禾基生物科技有限公司 | A kind of sucrose-fatty esters compound and preparation method thereof and purification process |
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| CN104004033A (en) * | 2013-06-21 | 2014-08-27 | 浙江迪耳化工有限公司 | Purification and separation method for sucrose fatty acid ester |
| CN104004033B (en) * | 2013-06-21 | 2016-08-10 | 浙江迪耳化工有限公司 | A kind of method for purifying and separating of sucrose fatty acid ester |
| CN106854226A (en) * | 2016-12-08 | 2017-06-16 | 广西科技师范学院 | The process for purification of sucrose fatty ester |
| CN106854226B (en) * | 2016-12-08 | 2023-07-25 | 广西科技师范学院 | Refining method of sucrose fatty acid ester |
| CN107325134A (en) * | 2017-06-21 | 2017-11-07 | 广州市禾基生物科技有限公司 | A kind of sucrose-fatty esters compound and preparation method thereof and purification process |
| CN109232676B (en) * | 2018-11-16 | 2021-08-03 | 山东福田药业有限公司 | Separation method of L-ribose |
| CN109232676A (en) * | 2018-11-16 | 2019-01-18 | 山东福田药业有限公司 | A kind of separation method of L- ribose |
| CN109942643A (en) * | 2019-03-14 | 2019-06-28 | 柳州职业技术学院 | A kind of method for purifying and separating of sucrose fatty ester |
| CN109942643B (en) * | 2019-03-14 | 2022-06-28 | 柳州职业技术学院 | Purification and separation method of sucrose fatty acid ester |
| CN110229197A (en) * | 2019-07-06 | 2019-09-13 | 潍坊大耀新材料有限公司 | A kind of preparation method of the one's own physical property sucrose ester of small molecule without solvent |
| CN112915565A (en) * | 2021-03-04 | 2021-06-08 | 安徽金禾实业股份有限公司 | Rotary continuous production equipment and production method for sucrose-6-ester |
| CN113151373A (en) * | 2021-03-09 | 2021-07-23 | 武汉臻治生物科技有限公司 | Preparation method and application of sucrose monoester with antibacterial and antitumor activities |
| CN113773352A (en) * | 2021-09-08 | 2021-12-10 | 暨南大学 | Method for preparing series sucrose esters in green solvent |
| CN114929720A (en) * | 2022-04-15 | 2022-08-19 | 广州嘉德乐生化科技有限公司 | Solvent-free synthesis method of sucrose ester with high monoester content |
| WO2023197278A1 (en) * | 2022-04-15 | 2023-10-19 | 广州嘉德乐生化科技有限公司 | Solvent-free synthesis method for sucrose ester having high monoester content |
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