CN107163091A - A kind of fractional extraction method of sucrose fatty ester - Google Patents
A kind of fractional extraction method of sucrose fatty ester Download PDFInfo
- Publication number
- CN107163091A CN107163091A CN201710441551.5A CN201710441551A CN107163091A CN 107163091 A CN107163091 A CN 107163091A CN 201710441551 A CN201710441551 A CN 201710441551A CN 107163091 A CN107163091 A CN 107163091A
- Authority
- CN
- China
- Prior art keywords
- sucrose
- fatty ester
- ester
- fatty
- sucrose fatty
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a kind of fractional extraction method of sucrose fatty ester, comprise the following steps：1) sucrose-fatty ester admixture is dispersed in C1~C3In alcohol, 0~30 DEG C of stirring is extracted, and filtering obtains filtrate and solid, and filtrate is distilled, dried, sucrose fatty ester product I is obtained；2) by step 1) solid that is filtrated to get is dispersed in C4~C8In alcohol, 10~50 DEG C of stirrings are extracted, and filtering obtains filtrate and solid, and filtrate is distilled, dried, sucrose fatty ester product I I is obtained.The fractional extraction method of the present invention can complete the purifying and separation of sucrose fatty ester simultaneously, technical process is simple, product purity is high, the rate of recovery is high, easily-recovered organic solvent is recycled, grading extraction process will not produce salt-containing organic wastewater, finally give high-purity, the sucrose fatty ester product of high monoester content, and the obtained recyclable synthesis covered for sucrose fatty ester of solid residue.
Description
Technical field
The present invention relates to a kind of fractional extraction method of sucrose fatty ester.
Background technology
Sucrose fatty ester is the one or more hydroxyls and C of sucrose8~C22Aliphatic acid be esterified to be formed a class green
Nonionic surface active agent, has the advantages that hydrophilic lipophilic balance is wide, emulsifiability is excellent, nontoxic, biodegradable, quilt
It is widely used in the industries such as food, medicine, cosmetics.At present, the industrial production of sucrose fatty ester, which is mainly, uses ester-interchange method,
It can be subdivided into solvent method and solventless method, the sucrose fatty ester that both approaches are obtained and not only contain sucrose-fatty list
Ester, sucrose-fatty diester and sucrose fatty polyester, also containing unreacted sucrose, fatty acid methyl ester (or ethyl ester or glycerine
Ester), aliphatic acid potassium (or sodium), the impurity such as catalyst, wherein, the content of sucrose-fatty monoesters generally 20%~55% it
Between.Therefore, to expect high-purity, the sucrose fatty ester of high monoester content, it is necessary to sucrose fatty ester carry out purification and
Separation.
United States Patent (USP) US 3748324 is using the two-phase solvent dissolution extraction such as butanone/water or ethyl acetate/water sucrose fat
Acid esters, and adjust pH value to 3.5~5.0 or add divalent metal salt and remove soap impurity, so as to realize sucrose-fatty
The purification of ester.
Chinese patent CN 104004033A use butanone dissolving sucrose fatty acid ester at 70 DEG C, filter out undissolved sucrose
Afterwards, CaCl is added in 55 DEG C of stirrings are descended toward filtrate2The aqueous solution, reaction is separated by filtration to obtain filtrate and solid, filtrate warp after 1 hour
Wash, distill, being dried to obtain the sucrose fatty ester of low monoester content, solid is through extraction at 70 DEG C of butanone, washing, distillation, dry
It is dry, obtain the sucrose fatty ester of high monoester content.
Chinese patent CN 103087118A use butanone, butanol or the ethyl acetate dissolving sucrose fatty acid ester at 55 DEG C,
It is directly added into dissolved with CaCl2The NaCl aqueous solution, filter out sediment fatty acid calcium etc., organic layer is washed with brine, after layering, cold
But crystallization, obtains purity>98% sucrose fatty ester, monoester content is 20% or so.
In addition, for the separation of the sucrose fatty ester without impurity such as sucrose, soaps, Chinese patent CN
The method that 105037450A uses crystallisation by cooling, by adjusting ratio and consumption, the chilling temperature and time of etoh solvent/water,
The sucrose fatty ester of isolated different monoester contents.
However, the method generally existing problems with of above-mentioned purification ＆ isolation sucrose fatty ester：1) sucrose fatty ester
Total ester, especially monoester content are relatively low, do not reach the requirement of high-end product market；2) complex technical process, sucrose fatty ester
The rate of recovery is not high, refines cost high；3) solvent usage amount is big, and the NaCl salt solution introduced in technique can cause saliferous, organic waste
The process problem of water, improves cost, adds environmental protection pressure；4) due to needing to add CaCl2、MgSO4Deng divalent metal salt
Precipitated fatty acid soap, adds solid waste.
The content of the invention
It is an object of the invention to provide a kind of fractional extraction method of sucrose fatty ester.
The technical solution used in the present invention is：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) sucrose-fatty ester admixture is dispersed in C1~C3In alcohol, 0~30 DEG C stirring extract, filtering, obtain filtrate and
Solid, is distilled to filtrate, is dried, obtain sucrose fatty ester product I；
2) by step 1) solid that is filtrated to get is dispersed in C4~C8In alcohol, 10~50 DEG C of stirrings are extracted, and filtering is filtered
Liquid and solid, are distilled to filtrate, are dried, obtain sucrose fatty ester product I I.
The mass percent of sucrose-fatty monoesters is 50%~95% in described sucrose fatty ester product I, described
Sucrose fatty ester product I I in sucrose-fatty monoesters mass percent be 1%~50%.
Described sucrose fatty ester contains C8~C22Fatty acyl group.
Described sucrose-fatty ester admixture includes sucrose-fatty monoesters, sucrose and/or soap, also comprising sugarcane
Sugar fatty acid diester, the ester of sucrose-fatty three, the ester of sucrose-fatty four, sucrose-fatty five-ester, the ester of sucrose-fatty six, sucrose
At least one of the ester of aliphatic acid seven, sucrose-fatty octaester.
Described soap is at least one of potassium stearate, odium stearate, potassium palmitate, sodium palmitate.
Described C1~C3Alcohol is at least one of methanol, ethanol, propyl alcohol, isopropanol.
Described C4~C8Alcohol is at least one in n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, hexanol, enanthol, octanol
Kind.
Described sucrose-fatty ester admixture, C1~C3Alcohol, C4~C8The mass ratio of alcohol is 1：(1~10)：(1~10).
Step 1) and 2) in stirring extract time be 10~60min, mixer rotating speed be 100~1000rpm.
The beneficial effects of the invention are as follows：
1) fractional extraction method of sucrose fatty ester of the invention can complete simultaneously sucrose fatty ester purifying and
Separation, finally gives high-purity, the sucrose fatty ester product of high monoester content；
2) the fractional extraction method technical process of sucrose fatty ester of the invention is simple, product purity is high, the rate of recovery is high,
Easily-recovered organic solvent is recycled, grading extraction process will not produce salt-containing organic wastewater；
3) solid residue (sucrose, soap) that the fractional extraction method of sucrose fatty ester of the invention is obtained can be returned
Receive synthesis of the set for sucrose fatty ester.
Embodiment
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) sucrose-fatty ester admixture is dispersed in C1~C3In alcohol, 0~30 DEG C stirring extract, filtering, obtain filtrate and
Solid, is distilled to filtrate, is dried, obtain sucrose fatty ester product I；
2) by step 1) solid that is filtrated to get is dispersed in C4~C8In alcohol, 10~50 DEG C of stirrings are extracted, and filtering is filtered
Liquid and solid, are distilled to filtrate, are dried, obtain sucrose fatty ester product I I.
It is preferred that, a kind of fractional extraction method of sucrose fatty ester comprises the following steps：
1) sucrose-fatty ester admixture is dispersed in C1~C3In alcohol, 0~30 DEG C stirring extract, filtering, obtain filtrate and
Solid, carries out repeating to extract 1~5 time, merging filtrate according to aforesaid operations to the solid being filtrated to get, filtrate is distilled,
Dry, obtain sucrose fatty ester product I；
2) by step 1) solid that is filtrated to get is dispersed in C4~C8In alcohol, 10~50 DEG C of stirrings are extracted, and filtering is filtered
Liquid and solid, are distilled to filtrate, are dried, obtain sucrose fatty ester product I I, dried recovered solid residue.
It is preferred that, in described sucrose fatty ester product I the mass percent of sucrose-fatty monoesters be 50%~
The mass percent of sucrose-fatty monoesters is 1%~50% in 95%, described sucrose fatty ester product I I.
It is preferred that, described sucrose fatty ester contains C8~C22Fatty acyl group.
It is preferred that, described sucrose-fatty ester admixture includes sucrose-fatty monoesters, sucrose and/or soap,
Also include sucrose-fatty diester, the ester of sucrose-fatty three, the ester of sucrose-fatty four, sucrose-fatty five-ester, sucrose-fatty
At least one of six esters, the ester of sucrose-fatty seven, sucrose-fatty octaester.
It is preferred that, described soap is at least one in potassium stearate, odium stearate, potassium palmitate, sodium palmitate
Kind.
It is preferred that, described C1~C3Alcohol is at least one of methanol, ethanol, propyl alcohol, isopropanol.
It is preferred that, described C4~C8Alcohol is in n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, hexanol, enanthol, octanol
It is at least one.
It is preferred that, described sucrose-fatty ester admixture, C1~C3Alcohol, C4~C8The mass ratio of alcohol is 1：(1~10)：
(1~10).
It is preferred that, step 1) and 2) in stirring extract time be 10~60min, mixer rotating speed be 100~
1000rpm。
C in the present invention1~C3Alcohol refers to the alcohol containing 1~3 carbon atom, C4~C8Alcohol refers to containing 4~8 carbon originals
The alcohol of son, C8~C22Fatty acyl group refer to that the aliphatic acid containing 8~22 carbon atoms participates in the acyl group that esterification is formed.
The present invention is made further explanation and description with reference to specific embodiment.
Sucrose-fatty ester admixture employed in embodiment 1~5 and comparative example 1~3 is produced by solvent-free process
Sucrose fatty ester commercially produced product, its composition is as shown in the table：
The composition table of the sucrose-fatty ester admixture of the embodiment 1~5 of table 1 and comparative example 1~3
Embodiment 1：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 400g absolute ethyl alcohols, 20 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 400g absolute ethyl alcohols, 20 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, then to solid B2Middle addition 400g absolute ethyl alcohols, 20 DEG C,
15min is extracted in stirring under 500rpm, is separated by filtration and is obtained filtrate A3With solid B3, merging filtrate A1、A2And A3, vacuum distillation recovery
Ethanol, vacuum drying, obtaining 43.5g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 94.9%, single
Ester content is 81.1%, and 13.8%) diester and many ester contents is；
2) to residual solids B3In, 1000g n-butanols are added, 30min is stirred at 30 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 33.2g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 97.0%, and monoester content is 5.7%, and diester and many ester contents are 91.3%) solid residue
22.6g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 4.9%, and free saccharide content is 25.2%, aliphatic acid
Potassium content is 68.6%) the recyclable synthesis covered for sucrose fatty ester.
Embodiment 2：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 200g absolute ethyl alcohols, 20 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 200g absolute ethyl alcohols, 20 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, so repeat stirring and extract 4 times, collect and merging filtrate A1、
A2、A3、A4And A5, vacuum distillation reclaim ethanol, vacuum drying, obtain 42.7g sucrose fatty esters product I (wherein, Sucrose Fatty Acid Ester
The total content of fat acid esters is 95.6%, and monoester content is 83.8%, and 11.7%) diester and many ester contents is；
2) to residual solids B5In, 1000g n-butanols are added, 30min is stirred at 30 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 33.9g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 97.1%, and monoester content is 4.1%, and diester and many ester contents are 93.0%) solid residue
22.7g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 4.0%, and free saccharide content is 25.1%, aliphatic acid
Potassium content is 69.6%) the recyclable synthesis covered for sucrose fatty ester.
Embodiment 3：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 200g absolute methanols, 20 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 200g absolute methanols, 20 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, so repeat stirring and extract 4 times, collect and merging filtrate A1、
A2、A3、A4And A5, vacuum distillation reclaim methanol, vacuum drying, obtain 40.2g sucrose fatty esters product I (wherein, Sucrose Fatty Acid Ester
The total content of fat acid esters is 95.0%, and monoester content is 90.0%, and 5.0%) diester and many ester contents is；
2) to residual solids B5In, 1000g n-butanols are added, 30min is stirred at 30 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 36.6g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 97.3%, and monoester content is 2.7%, and diester and many ester contents are 94.6%) solid residue
22.5g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 3.6%, and free saccharide content is 25.3%, aliphatic acid
Potassium content is 69.8%) the recyclable synthesis covered for sucrose fatty ester.
Embodiment 4：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 1000g isopropanols, 30 DEG C, stir under 1000rpm
30min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 1000g isopropanols, 30 DEG C, under 1000rpm
30min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, collect and merging filtrate A1And A2, vacuum distillation recovery isopropyl
Alcohol, vacuum drying, obtaining 53.1g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 94.5%, monoesters
Content is 62.9%, and 31.6%) diester and many ester contents is；
2) to residual solids B2In, 600g hexanols are added, 30min is stirred at 40 DEG C, is separated by filtration and obtains liquor B and solid
Hexanol is reclaimed in body residue, liquor B vacuum distillation, and vacuum drying obtains 25.3g sucrose fatty ester product I I (wherein, Sucrose Fatty Acid Esters
The total content of fat acid esters is 92.9%, and monoester content is 13.8%, and diester and many ester contents is 79.1%), solid residue are dried
After be weighed as 20.9g (wherein, the total content of sucrose fatty ester be 4.3%, free saccharide content is 26.8%, and aliphatic acid potassium contains
Measure as 67.5%), the recyclable synthesis covered for sucrose fatty ester.
Embodiment 5：
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 1000g absolute ethyl alcohols, 10 DEG C, stir under 300rpm
30min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 1000g absolute ethyl alcohols, 10 DEG C, under 300rpm
30min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, collect and merging filtrate A1And A2, vacuum distillation recovery second
Alcohol, vacuum drying, obtaining 30.6g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 93.5%, monoesters
Content is 80.1%, and 13.4%) diester and many ester contents is；
2) to residual solids B2In, add 1000g octanols, stir 15min at 40 DEG C, be separated by filtration obtain liquor B and
Octanol is reclaimed in solid residue, liquor B vacuum distillation, and vacuum drying obtains 48.1g sucrose fatty ester product I I (wherein, sucrose
The total content of fatty acid ester is 94.8%, and monoester content is 26.6%, and diester and many ester contents is 68.2%), solid residue are done
20.6g is weighed as after dry, and (wherein, the total content of sucrose fatty ester is 1.9%, and free saccharide content is 26.7%, aliphatic acid potassium
Content is 69.9%) the recyclable synthesis covered for sucrose fatty ester.
Embodiment 6：
Sucrose-fatty ester admixture employed in embodiment 6 is the sucrose fatty ester business produced by solvent-free process
Industry product, its composition is as shown in the table：
The composition table of the sucrose-fatty ester admixture of the embodiment 6 of table 2
A kind of fractional extraction method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 2, add 400g absolute ethyl alcohols, 20 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 400g absolute ethyl alcohols, 20 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, then to solid B2Middle addition 400g absolute ethyl alcohols, 20 DEG C,
15min is extracted in stirring under 500rpm, is separated by filtration and is obtained filtrate A3With solid B3, merging filtrate A1、A2And A3, vacuum distillation recovery
Ethanol, vacuum drying, obtaining 18.7g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 82.9%, single
Ester content is 50.8%, and 32.1%) diester and many ester contents is；
2) to residual solids B3In, 1000g n-butanols are added, 60min is stirred at 40 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 55.1g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 92.0%, and monoester content is 1.3%, and diester and many ester contents are 90.7%) solid residue
25.5g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 11.8%, and free saccharide content is 9.4%, aliphatic acid
Potassium content is 76.9%) the recyclable synthesis covered for sucrose fatty ester.
Comparative example 1：
A kind of extracting method of sucrose fatty ester, comprises the following steps：
Take the sucrose-fatty ester admixture shown in 100g tables 1, add 400g butanone, 20 DEG C, stir under 500rpm
15min, is separated by filtration and obtains filtrate and solid residue, and filtrate decompression is distilled to recover butanone, and vacuum drying obtains 51.7g sucrose
(wherein, the total content of sucrose fatty ester is 92.8% to fatty acid ester product, and monoester content is 39.7%, and diester and polyester contain
Measure as 53.1%), solid residue is weighed as 47.4g after drying (wherein, the total content of sucrose fatty ester is 56.1%, is dissociated
Sugared content is 12.0%, and 31.2%) aliphatic acid potassium content is.
Comparative example 2：
A kind of extracting method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 400g absolute ethyl alcohols, 40 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 400g absolute ethyl alcohols, 40 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, then to solid B2Middle addition 400g absolute ethyl alcohols, 40 DEG C,
15min is extracted in stirring under 500rpm, is separated by filtration and is obtained filtrate A3With solid B3, merging filtrate A1、A2And A3, vacuum distillation recovery
Ethanol, vacuum drying, obtaining 71.5g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 89.5%, single
Ester content is 51.0%, and 38.5%) diester and many ester contents is；
2) to residual solids B3In, 1000g n-butanols are added, 30min is stirred at 30 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 11.4g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 91.2%, and monoester content is 7.9%, and diester and many ester contents are 83.3%) solid residue
16.4g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 1.2%, and free saccharide content is 28.7%, aliphatic acid
68.3%) potassium content is.
Comparative example 3：
A kind of extracting method of sucrose fatty ester, comprises the following steps：
1) take the sucrose-fatty ester admixture shown in 100g tables 1, add 1200g absolute ethyl alcohols, 20 DEG C, stir under 500rpm
15min is mixed, is separated by filtration and obtains filtrate A1With solid B1, then to solid B1Middle addition 1200g absolute ethyl alcohols, 20 DEG C, under 500rpm
15min is extracted in stirring, is separated by filtration and is obtained filtrate A2With solid B2, then to solid B2Middle addition 1200g absolute ethyl alcohols, 20 DEG C,
15min is extracted in stirring under 500rpm, is separated by filtration and is obtained filtrate A3With solid B3, merging filtrate A1、A2And A3, vacuum distillation recovery
Ethanol, vacuum drying, obtaining 64.5g sucrose fatty esters product I, (wherein, the total content of sucrose fatty ester is 89.8%, single
Ester content is 57.4%, and 32.4%) diester and many ester contents is；
2) to residual solids B3In, 1000g n-butanols are added, 30min is stirred at 30 DEG C, is separated by filtration and obtains liquor B
And solid residue, liquor B vacuum distillation recovery n-butanol, it is dried in vacuo, obtains 16.7g sucrose fatty ester product Is I (wherein,
The total content of sucrose fatty ester is 94.0%, and monoester content is 2.4%, and diester and many ester contents are 91.6%) solid residue
18.1g is weighed as after drying, and (wherein, the total content of sucrose fatty ester is 5.5%, and free saccharide content is 26.0%, aliphatic acid
66.9%) potassium content is.
Integrated embodiment 1~6 and comparative example 1~3 are understood：Sucrose list in the sucrose fatty ester I that embodiment 1~6 is obtained
The content of ester is significantly larger than comparative example 1~3, illustrates that the fractional extraction method of sucrose fatty ester can be while complete sucrose fat
The purifying and separation of acid esters, can obtain high-purity, the sucrose fatty ester product of high monoester content, and technical process letter
Single, product purity is high, the rate of recovery is high.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of fractional extraction method of sucrose fatty ester, it is characterised in that：Comprise the following steps：
1) sucrose-fatty ester admixture is dispersed in C1~C3In alcohol, 0~30 DEG C of stirring is extracted, filtering, obtains filtrate and solid
Body, is distilled to filtrate, is dried, obtain sucrose fatty ester product I；
2) by step 1) solid that is filtrated to get is dispersed in C4~C8In alcohol, 10~50 DEG C stirring extract, filtering, obtain filtrate and
Solid, is distilled to filtrate, is dried, obtain sucrose fatty ester product I I.
2. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described sucrose fat
The mass percent of sucrose-fatty monoesters is 50%~95% in acid ester product I, in described sucrose fatty ester product I I
The mass percent of sucrose-fatty monoesters is 1%~50%.
3. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described sucrose fat
Acid esters contains C8~C22Fatty acyl group.
4. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described sucrose fat
Acid ester mixtures include sucrose-fatty monoesters, sucrose and/or soap, also comprising sucrose-fatty diester, sucrose fat
Sour three esters, the ester of sucrose-fatty four, sucrose-fatty five-ester, the ester of sucrose-fatty six, the ester of sucrose-fatty seven, sucrose-fatty
At least one of octaester.
5. the fractional extraction method of sucrose fatty ester according to claim 4, it is characterised in that：Described soap
For at least one of potassium stearate, odium stearate, potassium palmitate, sodium palmitate.
6. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described C1~C3Alcohol
For at least one of methanol, ethanol, propyl alcohol, isopropanol.
7. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described C4~C8Alcohol
For at least one of n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, hexanol, enanthol, octanol.
8. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Described sucrose fat
Acid ester mixtures, C1~C3Alcohol, C4~C8The mass ratio of alcohol is 1：(1~10)：(1~10).
9. the fractional extraction method of sucrose fatty ester according to claim 1, it is characterised in that：Step 1) and 2) in stir
The time for mixing extraction is 10~60min, and mixer rotating speed is 100~1000rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710441551.5A CN107163091A (en) | 2017-06-13 | 2017-06-13 | A kind of fractional extraction method of sucrose fatty ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710441551.5A CN107163091A (en) | 2017-06-13 | 2017-06-13 | A kind of fractional extraction method of sucrose fatty ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107163091A true CN107163091A (en) | 2017-09-15 |
Family
ID=59826047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710441551.5A Pending CN107163091A (en) | 2017-06-13 | 2017-06-13 | A kind of fractional extraction method of sucrose fatty ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107163091A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2015020073A1 (en) * | 2013-08-09 | 2015-02-12 | 第一工業製薬株式会社 | Method for producing sucrose fatty acid ester |
| CN104387429A (en) * | 2014-11-11 | 2015-03-04 | 浙江师范大学 | Purification method of sucrose fatty acid ester |
-
2017
- 2017-06-13 CN CN201710441551.5A patent/CN107163091A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2015020073A1 (en) * | 2013-08-09 | 2015-02-12 | 第一工業製薬株式会社 | Method for producing sucrose fatty acid ester |
| CN104387429A (en) * | 2014-11-11 | 2015-03-04 | 浙江师范大学 | Purification method of sucrose fatty acid ester |
Non-Patent Citations (1)
| Title |
|---|
| 朱金丽: "硬脂酸蔗糖酯系表面活性剂的研究", 《中国博士学位论文全文数据库》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1155113A (en) | Process for recovery of polyol fatty acid polyesters | |
| TW203041B (en) | ||
| US10265641B2 (en) | Simultaneous recovery of organic compounds and extractants | |
| CN103087118A (en) | Method for purifying sucrose fatty acid esters | |
| CN104004033B (en) | A kind of method for purifying and separating of sucrose fatty acid ester | |
| CN101774997B (en) | Method for completely and continuously extracting natural vitamin E and phytosterol | |
| CN107163091A (en) | A kind of fractional extraction method of sucrose fatty ester | |
| CN107325134A (en) | A kind of sucrose-fatty esters compound and preparation method thereof and purification process | |
| US2948716A (en) | Purification of sugar esters | |
| SU791248A3 (en) | Method of purifying saccharose esters | |
| CN107383118B (en) | A kind of method for purifying and separating of sucrose fatty ester | |
| CN114015732B (en) | Industrial preparation method of andrographolide and dehydroandrographolide | |
| CN106543196B (en) | A method of extracting sesamin from sesame oil | |
| CN113980070B (en) | Purification method of hydrophilic mannose erythritol lipid | |
| EP0459172B1 (en) | Process for decolorizing sucrose fatty acid esters | |
| CN109942643B (en) | Purification and separation method of sucrose fatty acid ester | |
| CN1056614C (en) | Method for purifying O,S-dimethyl N-acetyphosphoramidothioate | |
| CA2673801A1 (en) | Process for recovering sterols from a crude source containing sterol esters | |
| CN113651862A (en) | Purification and separation method of sucrose fatty acid ester | |
| CN103755685B (en) | Purifying and refining method of esomeprazole sodium | |
| CN106749437A (en) | A kind of recovery method of Glucosamine Sulphate sodium chloride double salt mother liquor | |
| US2302679A (en) | Process of treating wool greases | |
| EP0448996B1 (en) | Process for removing soaps and fatty acids from sucrose fatty acid esters | |
| CN112940062B (en) | Preparation method of 16-dehydroprogesterone | |
| US2729656A (en) | Isolation of sterols |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170915 |
|
| RJ01 | Rejection of invention patent application after publication |