CN1307188C - Method for extracting sucrose fatty acid ester - Google Patents
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- CN1307188C CN1307188C CNB2005100060111A CN200510006011A CN1307188C CN 1307188 C CN1307188 C CN 1307188C CN B2005100060111 A CNB2005100060111 A CN B2005100060111A CN 200510006011 A CN200510006011 A CN 200510006011A CN 1307188 C CN1307188 C CN 1307188C
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- sucrose ester
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- 229930006000 Sucrose Natural products 0.000 title claims abstract description 90
- 239000005720 sucrose Substances 0.000 title claims abstract description 89
- -1 sucrose fatty acid ester Chemical class 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 41
- 235000014113 dietary fatty acids Nutrition 0.000 title abstract 3
- 229930195729 fatty acid Natural products 0.000 title abstract 3
- 239000000194 fatty acid Substances 0.000 title abstract 3
- 239000012043 crude product Substances 0.000 claims abstract description 38
- 239000002253 acid Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 16
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- 239000000344 soap Substances 0.000 claims description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000292 calcium oxide Substances 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005119 centrifugation Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000007086 side reaction Methods 0.000 abstract 1
- 229960004793 sucrose Drugs 0.000 description 74
- 239000012074 organic phase Substances 0.000 description 21
- 150000002148 esters Chemical class 0.000 description 20
- 235000000346 sugar Nutrition 0.000 description 19
- 239000000203 mixture Substances 0.000 description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000012535 impurity Substances 0.000 description 14
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 11
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 10
- 150000002632 lipids Chemical class 0.000 description 10
- 229920000728 polyester Polymers 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 description 7
- 235000011152 sodium sulphate Nutrition 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 1
- 235000013681 dietary sucrose Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Saccharide Compounds (AREA)
Abstract
The present invention discloses a purification method of sucrose fatty acid ester, which comprises the following steps: firstly, a crude product of sucrose ester is dissolved in a water separable organic solvent to obtain a solution of the crude product of the sucrose ester; secondly, the solution is stirred under the condition of the temperature of 30 to 80DEG C, and dilute acid is dropped so that the pH value reaches 6.0(+/-)0.5; thirdly, water is removed to obtain a solution of the acidified crude product, the solution of the acidified crude product is stirred at the temperature within the range of 40 to 110DEG C to react with an added alkaline earth metal compound, and the reaction time is generally from 10 minutes to 180 minutes; finally, generated solid fatty acid salt is removed with a centrifugation method, a precipitation method or a filtration method, and the purified sucrose ester product can be obtained after the clear solution is heated and distilled at reduced pressure. The present invention has the advantages of reasonable technological process, favorable purifying effect, short reaction time, few side reactions, wide adaptable ranges and low production cost.
Description
Technical field
The present invention relates to a kind of method of purification of ester, especially a kind of method of purification of sucrose fatty ester.
Background technology
The industrial method of synthesis of sucrose ester is an ester-interchange method at present, 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 residual sugar, soap body, lipid acid, fatty acid methyl ester, impurity such as catalyzer, in European Patent Application in 1991, told about a kind of method of purifying sucrose ester, this method be with the sucrose ester dissolving crude product in the organic solvent that can dissolve it, in the sucrose ester crude product of 100 weight parts, add 20 to 200 weight part alkaline earth metal compounds then and react; This method alkaline earth metal compound add-on is big, 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; Direct and the impurity soap body reaction of alkaline earth metal compound, reaction is difficult to carry out, and impurity is difficult for removing, and reacts not thorough, can not effectively remove impurity, therefore can only handle foreign matter content at the sucrose ester crude product below 5%.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technological process is reasonable, refining effect good, the reaction times is fast, negative reaction is few, the method for purification of wide accommodation, sucrose fatty ester that production cost is low.
The present invention addresses the above problem the technical scheme that is adopted: the method for purification of this sucrose fatty ester, wherein:
A, with the sucrose ester dissolving crude product can with the organic solvent of water sepn in, obtain the sucrose ester crude product solution;
B, under 30 ℃ of-80 ℃ of conditions, stir and dripping dilute acid, make pH value reach 6.0 ± 0.5, remove moisture then, obtain souring soln;
C, souring soln stirred in 40 ℃-110 ℃ temperature range and add alkaline earth metal compound react, the add-on of alkaline earth metal compound is to add 1-19 weight part alkaline earth metal compound in per 100 weight part sucrose ester crude products, reaction times is 10 minutes-180 minutes, obtains reaction mixture;
D, above-mentioned reaction mixture is removed the solids soap of generation with centrifugal, precipitation or filter method, the solution that will remove solids soap promptly can obtain the sucrose ester product of purifying through the heating underpressure distillation.
The present invention is after obtaining the sucrose ester crude product solution, and adding concentration is the sodium chloride aqueous solution of 2%-10%, then the water layer branch is gone.
Organic solvent of the present invention comprises butanone and/or propyl carbinol and/or ethyl acetate and/or chloroform.
Diluted acid of the present invention is hydrochloric acid, acetic acid, citric acid, dilute sulphuric acid.
Alkaline earth metal compound of the present invention comprises calcium hydroxide and/or calcium oxide and/or calcium chloride and/or magnesium hydroxide and/or magnesium oxide and/or barium oxide and/or hydrated barta.
The water content of the present invention's its solution after removing moisture, obtaining souring soln is 0.1-3.0%.
The present invention compared with prior art has the following advantages and effect: 1, optimized processing step, production technique is reasonable; 2, the reaction times fast, production cost is low; 3, negative reaction is few, and the sucrose ester product content height, the impurity that obtain are few; 4, the present invention is specially adapted to the purification of solventless method synthetic sucrose ester crude product, also is applicable to the purification of solvent method synthetic sucrose ester crude product; 5, complete processing is simple, no raw material problem in short supply.6, the technology of the present invention not only can purifying soap body content less than 5% sucrose ester first product, also can handle the sucrose ester crude product of soap body content up to 5-30%, therefore, the present invention is not only applicable to the purification of the sucrose ester crude product of solvent method production, and be specially adapted to the purifying of solventless method synthetic sucrose ester crude product, usually handle once with the technology of the present invention, can obtain to meet the high-quality sucrose ester product of China, the U.S. and JIS, have broad application prospects.The technology of the present invention lab scale is researched and developed successfully and auspicious continuous heavy rain chemical industry company limited obtains the suitability for industrialized production achievement in Hangzhou.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, and following examples are explanation of the invention and the present invention is not limited to following examples.
Example one:
By solvent-free ester-interchange method synthetic industrial sucrose product A, the component of its crude product is as follows:
Component content (%)
Sucrose ester 48.0
Unreacted free sugar 30.1
Soap body 13.5
Lipid acid 3.8
Fatty acid methyl ester 2.7
Impurity such as catalyzer 1.9
In the sucrose ester monoester content be 50.2%, dibasic acid esters 30.1%, polyester 19.7%.
The above-mentioned sucrose ester crude product A of 100 grams adds 380ml butanone (c, p) and 8%Nacl aqueous solution 220ml, and mixture stirred branch vibration layer 25 minutes at 35 ℃.Under 55 ℃, transfer PH to 5.9 ± 0.3, stirred 12 minutes, divide and remove the bottom water layer with dilute sulphuric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, organic phase is under 45 ℃ of stirrings, add calcium oxide 1 gram reaction 40 minutes, after the filtration with organic phase clear liquid evaporated under reduced pressure, can obtain sucrose ester sample 46.8 grams of purifying, its total ester content is 93.6%, acid number 1.5, free sugar 0.97%, ash 0.83%, and the monoester content of sample is 49.2%.
Example two:
By solvent-free ester-interchange method synthetic industrial sucrose product B, the component of its crude product is as follows:
Component content (%)
Sucrose ester 53.5
Unreacted free sugar 23.0
Soap body 16.1
Lipid acid 3.8
Fatty acid methyl ester 1.9
Impurity such as catalyzer 1.7
In the sucrose ester monoester content be 60.2%, dibasic acid esters 23.7%, polyester 16.1%.
The above-mentioned sucrose ester crude product B of 100 grams adds 400ml ethyl acetate (c, p) and 5%Nacl aqueous solution 250ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 55 ℃, transfer PH to 5.9 ± 0.3, reacted 12 minutes, divide and remove the bottom water layer with dilute hydrochloric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, organic phase is under 40 ℃ of stirrings, the mixture (1: 2 W/W) that adds calcium oxide and calcium hydroxide 11 restrains totally, stirring reaction 50 minutes, after the filtration with organic phase clear liquid evaporated under reduced pressure, can obtain sucrose ester sample 52.1 gram of purifying, its total ester content is 93.7%, acid number 1.03, free sugar 0.89%, ash 1.02%, and the monoester content of sample is 59.6%.
Example three:
By solvent-free ester-interchange method synthetic industrial sucrose products C, the component of its crude product is as follows:
Component content (%)
Sucrose ester 60.2
Unreacted free sugar 18.8
Soap body 11.2
Lipid acid 3.9
Fatty acid methyl ester 4.0
Impurity such as catalyzer 1.9
In the sucrose ester monoester content be 40.7%, dibasic acid esters 31.6%, polyester 23.7%.
The above-mentioned sucrose ester crude product C of 100 grams adds 400ml propyl carbinol (c, p) and 4%Nacl aqueous solution 220ml, and mixture stirred branch vibration layer 25 minutes at 65 ℃.Under 55 ℃, transfer PH to 6.2 ± 0.3, reacted 15 minutes, divide and remove the bottom water layer with acetic acid.Organic phase is under 100 ℃, add 20% calcium chloride solution to PH to 6.5 ± 0.3, stirring reaction 25 minutes, obtain the organic phase clear liquid with centrifuging, this organic phase of evaporated under reduced pressure, can obtain sucrose ester sample 58.7 gram of purifying, its total ester content is 94.1%, acid number 2.12, free sugar 0.84%, ash 0.86%, and the monoester content of sample is 40.3%.
Example four:
By solvent-free ester-interchange method synthetic industrial sucrose product D, the component of its crude product is as follows:
Component content (%)
Sucrose ester 55.2
Unreacted free sugar 19.8
Soap body 15.6
Lipid acid 3.5
Fatty acid methyl ester 4.1
Impurity such as catalyzer 1.8
In the sucrose ester monoester content be 55.1%, dibasic acid esters 25.8%, polyester 19.1%.
The above-mentioned sucrose ester crude product D of 100 grams adds 380ml butanone (c, p) and 5%Nacl aqueous solution 220ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 30 ℃, transfer PH to 5.8 ± 0.3, reacted 10--15 minute, divide and remove the bottom water layer with dilute hydrochloric acid.Boil off excessive moisture in the organic phase with distillation method, again under 50 ℃ of stirrings, added magnesium hydroxide and magnesian mixture (1: 1, W: W) 10 gram reactions are 40 minutes, with organic phase clear liquid evaporated under reduced pressure, can obtain the sucrose ester sample 53.5g of purifying after the filtration, its total ester content is 94.1%, acid number 1.08, free sugar 0.87%, ash 0.77%, the monoester content of sample are 54.8%.
In this example, magnesium hydroxide and magnesian mixture also the mixture replacing of available hydrogen barium oxide and barytic mixture or calcium hydroxide and calcium oxide react.
Example five:
By solvent-free ester-interchange method synthetic industrial sucrose product E, the component of its crude product is as follows:
Component content (%)
Sucrose ester 53.2
Unreacted free sugar 21.9
Soap body 15.0
Lipid acid 3.8
Fatty acid methyl ester 4.2
Impurity such as catalyzer 1.9
In the sucrose ester monoester content be 54.2%, dibasic acid esters 26.1%, polyester 19.7%.
The above-mentioned sucrose ester crude product E of 100 grams adds 380ml ethyl acetate and 10%Nacl aqueous solution 220ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Transfer PH to 6.0 ± 0.2 with rare sulfosalt down at 40 ℃, reacted 10--15 minute, divide and remove the bottom water layer.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, again under 55 ℃ of stirrings, add calcium oxide 2.0 gram reactions 30 minutes, after the filtration with the limpid evaporated under reduced pressure of organic phase, can obtain the sucrose ester sample 51.8g of purifying, its total ester content is 94.8%, and acid number 1.1, free sugar 0.76%, ash 0.65%, the monoester content of sample are 53.9%.
Example six:
By solvent-free ester-interchange method synthetic industrial sucrose product F, the component of its crude product is as follows:
Component content (%)
Sucrose ester 51.3
Unreacted free sugar 22.8
Soap body 13.2
Lipid acid 3.7
Fatty acid methyl ester 4.0
Impurity such as catalyzer 1.8
In the sucrose ester monoester content be 52.3%, dibasic acid esters 28.7%, polyester 19.2%.
The above-mentioned sucrose ester crude product F of 100 grams adds 400ml chloroform and 3%Nacl aqueous solution 250ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 50 ℃, transfer PH to 6.3 ± 0.3, reacted 15 minutes, divide and remove the bottom water layer with citric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, again under 75 ℃ of stirrings, add calcium chloride 19 gram reactions 40 minutes, after the filtration with organic phase clear liquid evaporated under reduced pressure, can obtain the sucrose ester sample 50.8g of purifying, its total ester content is 93.1%, and acid number 1.2, free sugar 0.82%, ash 0.57%, the monoester content of sample are 51.8%.
Example seven:
By solvent-free ester-interchange method synthetic industrial sucrose product G, the component of its crude product is as follows:
Component content (%)
Sucrose ester 56.8
Unreacted free sugar 17.7
Soap body 16.5
Lipid acid 3.4
Fatty acid methyl ester 3.7
Impurity such as catalyzer 1.9
In the sucrose ester monoester content be 60.2%, dibasic acid esters 21.5%, polyester 18.3%.
The above-mentioned sucrose ester crude product G of 100 grams adds 380ml chloroform and 6%Nacl aqueous solution 220ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 50 ℃, transfer PH to 6.0 ± 0.3, reacted 15 minutes, divide and remove the bottom water layer with dilute hydrochloric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, again under 45 ℃ of stirrings, add magnesium oxide 16 gram reactions 50 minutes, after the filtration with the limpid evaporated under reduced pressure of organic phase, can obtain the sucrose ester sample 54.6g of purifying, its total ester content is 94.1%, and acid number 0.98, free sugar 0.77%, ash 0.71%, the monoester content of sample are 58.4%.
Example eight:
By solvent-free ester-interchange method synthetic industrial sucrose product H, the component of its crude product is as follows:
Component content (%)
Sucrose ester 52.8
Unreacted free sugar 22.9
Soap body 14.3
Lipid acid 4.3
Fatty acid methyl ester 3.9
Impurity such as catalyzer 1.8
In the sucrose ester monoester content be 51.7%, dibasic acid esters 29.8%, polyester 18.5%.
The above-mentioned sucrose ester crude product G of 100 grams adds 400ml propyl carbinol and 6%Nacl aqueous solution 250ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 70 ℃, transfer PH to 6.1 ± 0.3, reacted 10--15 minute, divide and remove the bottom water layer with citric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, again under 108 ℃ of stirrings, the mixture of adding calcium oxide and calcium chloride (1: 1, W: W) 3 gram reactions are 30 minutes, with organic phase clear liquid evaporated under reduced pressure, can obtain the sucrose ester sample 51.2g of purifying after the filtration, its total ester content is 93.7%, acid number 1.2, free sugar 0.88%, ash 0.74%, the monoester content of sample are 50.6%.
Example nine:
By solvent-free ester-interchange method synthetic industrial sucrose product I, the component of its crude product is as follows:
Component content (%)
Sucrose ester 51.8
Unreacted free sugar 24.3
Soap body 13.9
Lipid acid 4.0
Fatty acid methyl ester 4.1
Impurity such as catalyzer 1.9
In the sucrose ester monoester content be 53.3%, dibasic acid esters 28.3%, polyester 18.4%.
The above-mentioned sucrose ester crude product I of 100 grams adds 400m ethyl acetate (c, p) and 6%Nacl aqueous solution 250ml, and mixture stirred branch vibration layer 25 minutes at 60 ℃.Under 80 ℃, transfer PH to 6.0 ± 0.3, reacted 12--15 minute, divide and remove the bottom water layer with dilute hydrochloric acid.Remove excessive moisture in the organic phase with anhydrous sodium sulphate, again under 60 ℃ of stirrings, the mixture of adding magnesium oxide and calcium oxide (1: 1, W: W) 5 gram reactions are 50 minutes, with organic phase clear liquid evaporated under reduced pressure, can obtain the sucrose ester sample 50.3g of purifying after the filtration, its total ester content is 94.2%, acid number 1.1, free sugar 0.75%, ash 0.68%, the monoester content of sample are 52.8%.
Claims (6)
1, a kind of method of purification of sucrose fatty ester is characterized in that:
A, with the sucrose ester dissolving crude product can with the organic solvent of water sepn in, obtain the sucrose ester crude product solution;
B, under 30 ℃ of-80 ℃ of conditions, stir and dripping dilute acid, make pH value reach 6.0 ± 0.5, remove moisture then, obtain souring soln;
C, souring soln stirred in 40 ℃-110 ℃ temperature range and add alkaline earth metal compound react, the add-on of alkaline earth metal compound is to add 1-19 weight part alkaline earth metal compound in per 100 weight part sucrose ester crude products, reaction times is 10 minutes-180 minutes, obtains reaction mixture;
D, above-mentioned reaction mixture is removed the solids soap of generation with centrifugal, precipitation or filter method, the solution that will remove solids soap promptly can obtain the sucrose ester product of purifying through the heating underpressure distillation.
2, the method for purification of sucrose fatty ester according to claim 1 is characterized in that: after obtaining described sucrose ester crude product solution, adding concentration is the sodium chloride aqueous solution of 2%-10%, then the water layer branch is gone.
3, the method for purification of sucrose fatty ester according to claim 1 and 2 is characterized in that: described organic solvent comprises butanone and/or propyl carbinol and/or ethyl acetate and/or chloroform.
4, the method for purification of sucrose fatty ester according to claim 1 and 2 is characterized in that: described diluted acid is hydrochloric acid, acetic acid, citric acid, dilute sulphuric acid.
5, the method for purification of sucrose fatty ester according to claim 1 and 2 is characterized in that: described alkaline earth metal compound comprises calcium hydroxide and/or calcium oxide and/or calcium chloride and/or magnesium hydroxide and/or magnesium oxide and/or barium oxide and/or hydrated barta.
6, the method for purification of sucrose fatty ester according to claim 1 and 2 is characterized in that: the water content of its solution is 0.1-3.0% after describedly removing moisture, obtaining souring soln.
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| CNB2005100060111A CN1307188C (en) | 2005-01-07 | 2005-01-07 | Method for extracting sucrose fatty acid ester |
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| CNB2005100060111A CN1307188C (en) | 2005-01-07 | 2005-01-07 | Method for extracting sucrose fatty acid ester |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103087118B (en) * | 2013-02-28 | 2016-03-16 | 广西高通食品科技有限公司 | A kind of method of purification of sucrose fatty ester |
| CN107790066A (en) * | 2016-09-05 | 2018-03-13 | 丰益(上海)生物技术研发中心有限公司 | The method for reducing content of plasticizing agent in raw material |
| CN107325134B (en) * | 2017-06-21 | 2018-09-28 | 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 |
| 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 |
| CN112999970A (en) * | 2021-03-09 | 2021-06-22 | 武汉臻治生物科技有限公司 | Compound emulsifier based on sucrose and grease transesterification and preparation method and application thereof |
| CN113651862A (en) * | 2021-08-16 | 2021-11-16 | 广西大学 | Purification and separation method of sucrose fatty acid ester |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0459172A1 (en) * | 1990-05-16 | 1991-12-04 | Dai-Ichi Kogyo Seiyaku Co., Ltd. | Process for decolorizing sucrose fatty acid esters |
-
2005
- 2005-01-07 CN CNB2005100060111A patent/CN1307188C/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0459172A1 (en) * | 1990-05-16 | 1991-12-04 | Dai-Ichi Kogyo Seiyaku Co., Ltd. | Process for decolorizing sucrose fatty acid esters |
Non-Patent Citations (1)
| Title |
|---|
| 蔗糖酯粗品的纯化工艺研究 刘志伟，武汉工业学院学报，第11期 1999 * |
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Assignee: Xiamen Yinlu Foods Group Co., Ltd. Assignor: Yuan Changgui Contract fulfillment period: 2009.4.28 to 2015.4.27 Contract record no.: 2009990000687 Denomination of invention: Purification method of sucrose fatty acid ester Granted publication date: 20070328 License type: Exclusive license Record date: 20090624 |
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