CN109734755A - A kind of Sucralose crystallization processes - Google Patents
A kind of Sucralose crystallization processes Download PDFInfo
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- CN109734755A CN109734755A CN201811619279.6A CN201811619279A CN109734755A CN 109734755 A CN109734755 A CN 109734755A CN 201811619279 A CN201811619279 A CN 201811619279A CN 109734755 A CN109734755 A CN 109734755A
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Abstract
The invention discloses a kind of Sucralose crystallization processes, sucrose is obtained into the sucralose-6-ester aqueous solution with high salt containing a large amount of related impurities via esterification and chlorination reaction, after cooling to certain temperature, a small amount of organic solvent is added, the polarity for changing solution, reduces the dissolubility of solute, it can to obtain the crystal of sucralose-6-ester, recycled after mother liquor desalination reduces waste discharge.Such method has purity is high, and step is simple, feature at low cost, easy to industrialized production, and for realizing that green plant area plays an important role.
Description
Technical field
The present invention relates to Sucralose production technical field more particularly to a kind of Sucralose crystallization processes.
Background technique
Sucralose (Sucralose) is the sweetener of new generation developed after Aspartame, 3,4-Dihydro-6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt, sweet taste
For characteristic closest to sucrose, sugariness is about 600 times of sucrose, have sugariness is high, sweet taste is pure, it is low in calories, be not involved in human body generation
It thanks, is highly-safe, fighting the features such as sour hydrolysis ability is strong, being a kind of current quite potential intense sweetener.Trichlorine sugarcane
Sugar is queried now in Aspartame by people because its unique advantage is always the high-end product in sweetener market,
Sucralose should resolutely capture Aspartame market, replace Aspartame, become public shared sweetener.Trichlorine at present
Sucrose is generally that the product obtained after acetyl group is removed in MeOH methanol sodium solution by sucralose-6-ester.Sucrose is passing through
Sucrose-6-ester is obtained after acetylation, the chlorination that sucrose-6-ester is generated in trichloroethanes by DMF and SOCl2 later tries
Agent replaces three hydroxyls to generate sucralose-6-ester, so that intermediate products is stored in trichloroethanes by ammonium hydroxide neutralization and is formed with water
Liquid in, via concentration removal trichloroethanes and remaining DMF, elute trichlorine in water using the adsorption capacity of active carbon
Sucrose-6-ester.A large amount of ammonium salt and associated products are generated in entire production process to bring for subsequent purification with crystallization process
Certain puzzlement.So the yield and purity of sucralose-6-ester directly will affect the quality and receipts of Sucralose product
Rate.So the method for crystallising of sucralose-6-ester will have a direct impact on final result.In the same industry obtain impure amount compared with
The method for generalling use extraction after the turbid solution of more sucralose-6-esters, is extracted using a large amount of organic solvent,
Make sucralose-6-ester dissolution in organic solvent, so that associated products and a large amount of salt are stayed in mother liquor, it will be above-mentioned
Solution concentration progress solvent is replaced into aqueous solution and is crystallized.Trichlorine repeatedly is obtained by organic solvent or water crystallization later
Such method of the product of cane sugar-6-acetic ester consumes a large amount of organic solvents, and residual organic solvent is difficult to handle in mother liquor,
Yield is not high.The present invention introduces a kind of method for crystallising of sucralose-6-ester, the water after above-mentioned active carbon decoloring terminates
In solution, it is only necessary to quantitative organic solvent be added, it is seen that Sucralose -6- when cooling to a certain degree
The crystal of ester, the present invention are that the polarity of solvent is changed by joined ethyl acetate in aqueous solution, make solute in the solution
Dissolubility reduce, then sucralose-6-ester is just slowly precipitated.Obtained sucralose-6-ester crude product only needs once to tie again
Crystalline substance can be obtained by the intermediate that content is 99%.Simple two step is only needed by this method, it is big instead of being used in the same industry
It measures extractant and carries out the mode that extraction repeatedly consumes a large amount of solvents.Mother liquor can recycle organic solvent by easy steps, evaporate
Sewage discharge can be reduced with recycled by dividing, and finally obtained by-product while environment is protected to have certain economic value,
And it is amplified to Yi Shixian in production, and do not need large scale equipment, and it is low in cost, it is suitble to industrialized production.For capturing
Brand names are fired in international market, improve local economy, realize that Sucralose Industry Prosperity prosperity is of great significance.
Summary of the invention
The invention proposes a kind of Sucralose crystallization processes.
To achieve the goals above, present invention employs following technical solutions:
A kind of Sucralose crystallization processes, comprising the following steps:
Step 1: sucrose-6-ester is added rising temperature for dissolving in DMF, obtains the DMF solution of sucrose-6-ester by esterification；
Step 2: trichloroethanes and thionyl chloride is added in chlorination reaction in the DMF solution of sucrose-6-ester, all molten
It is to slowly warm up to certain temperature and held for some time after solution, obtains sucralose-6-ester aqueous solution with high salt；
Step 3: neutralizing concentration, is added after buck adjusts pH value and carries out in sucralose-6-ester aqueous solution with high salt
Concentration obtains concentration sucralose-6-ester aqueous solution；
Step 4: decolorization adsorption is taken off after being diluted with water in concentration sucralose-6-ester aqueous solution with active carbon
Color obtains decoloration sucralose-6-ester aqueous solution；
Step 5: organic solvent is added after removing active carbon in decoloration sucralose-6-ester aqueous solution in primary crystallization,
It is filtered to obtain crystal after precipitating crystal；
Step 6: it recrystallization: will be recrystallized after the dissolution of crystals being precipitated in step 5；
Step 7: disposing mother liquor utilizes: being concentrated, obtains after the mother liquor of primary crystallization to be concentrated to removal organic solvent first
The solution to touch the mark after mixed with the mother liquor of recrystallization after carry out decolorization adsorption and crystallization processes again.
Further, the organic solvent is methyl acetate, ethyl acetate, butyl acetate, dichloroethanes, three chloroethenes
Any one in alkane, hexamethylene；
It further, is the 1/10-3/10 of decoloration sucralose-6-ester aqueous solution using the amount of organic solvent；
Further, the temperature before organic solvent is added controls between 10-30 DEG C.
Further, the temperature after organic solvent is added controls between 10-30 DEG C.
Further, in the esterification sucrose-6-ester DMF solution, be sucrose in DMF solution and tin class urge
Sucrose -6- the ester that the complex compound that agent generates generates under conditions of acetic anhydride obtains sucrose-6-ester after extraction concentration
DMF solution.
Further, the solvent used that extracts is methyl acetate, ethyl acetate, butyl acetate, dichloroethanes, three
Any one in chloroethanes, hexamethylene.
Further, the tin catalyst be carried out in hexamethylene by tin compound with acid anhydrides substance it is molten
The substance that solution obtains.
Further, the sucralose-6-ester aqueous solution with high salt the preparation method is as follows:
Step 1: trichloroethanes is added in the DMF solution of sucrose-6-ester, and is carried out after thionyl chloride is added dropwise in low temperature
It is warming up to 112.5 DEG C and keeps the temperature 2 hours；
Step 2: being added sodium hydroxide after cooling or ammonium hydroxide generates chlorination ammonium salt and the epoxy group by associated products
It is reduced to hydroxyl；
Step 3: related solvents are removed via concentration, and carry out the impurity such as adsorpting pigment using water as carrier with active carbon；
Finally obtain sucralose-6-ester aqueous solution with high salt.
Further, removal organic solvent is concentrated in the mother liquor of the primary crystallization in the step 7 first, detects organic molten
Agent residual quantity is 0.01%, and fraction shows delamination, and upper layer is transferred to head tank and reuses, and continues to be concentrated, detection evaporates
Substance residual is trichloroethanes 0.01% in point, and DMF residual 0.02% reaches the index for applying circulation.
Usefulness: sucrose is obtained the height containing a large amount of related impurities via esterification and chlorination reaction by the present invention
Salt sucralose-6-ester aqueous solution after cooling to certain temperature, is added a small amount of organic solvent, changes the polarity of solution, make
The dissolubility of solute reduces, it can obtains the crystal of sucralose-6-ester, recycled after mother liquor desalination reduces waste row
It puts.Such method has purity is high, and step is simple, feature at low cost, easy to industrialized production, and for realizing green
Plant area plays an important role.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Fig. 2 is the data histograms of the embodiment of the present invention and comparative example.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
In the description of the present invention, it is to be understood that, term " on ", "lower", "front", "rear", "left", "right",
The orientation or positional relationship of the instructions such as "top", "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only
For the convenience of describing the present invention and simplifying the description, rather than the device or element of indication or suggestion meaning must have specifically
Orientation is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
Referring to Fig.1, the chlorination reagent high temperature that sucrose-6-ester is chlorinated that sulfoxide and DMF are generated in trichloroethanes replaces three
After a hydroxyl, while a large amount of related substances are generated, so that PART EPOXY base is reduced to hydroxyl by buck neutralization.Through overrich
Removal trichloroethanes and DMF after contracting, form sucralose-6-ester aqueous solution with high salt after decoloration, wherein also containing
A large amount of impurity, is added the crystal that sucralose-6-ester can be precipitated in a small amount of organic solvent, detection purity be 85% with
On, crystalline rate reaches 95% or more.Related impurities are mainly the low polar impurity in part, and highly polar impurity all remains in substantially
In mother liquor.It obtains carrying out primary water-soluble recrystallization after this product, so that it may purity are promoted to 98%, part Sucralose-
6- ester material remains in mother liquor, and directly set is used decolorization process and used as water supplement, reduces environmental pollution and material is unrestrained
Take, in other words this step yield is 100%.First subcrystalline mother liquor is concentrated later by concentration and recovery organic solvent,
Obtained water, which can equally cover, to be used in decolorization process, and raffinate with high salt is by recycling chlorination ammonium salt for fertilizer after plate-frame filtering
Material production, surplus materials enter carburising step.
The organic solvent is methyl acetate, ethyl acetate, butyl acetate, dichloroethanes, trichloroethanes, hexamethylene
In any one；Amount using organic solvent is the 1/10-3/10 of Sucralose aqueous solution with high salt；Secondly, being added organic molten
Temperature before agent should control between 10-30 DEG C, or control under the conditions of this temperature after organic solvent is added；
Highly polar impurity is the substances such as ammonium chloride, sodium chloride, dichloro sucrose, dichloro cane sugar-6-acetic ester,
Low polar impurity is the substances such as tetrachloro cane sugar-6-acetic ester, tetrachloro sucrose, pentachloro- sucrose, Sucralose diester.
The generation method of the sucralose-6-ester aqueous solution with high salt containing a large amount of related impurities referred in the present invention is
The DMF solution of sucrose-6-ester, low temperature carries out being warming up to 112.5 DEG C of heat preservations 2 hours after thionyl chloride is added dropwise in trichloroethanes,
Sodium hydroxide is added after cooling or ammonium hydroxide generates chlorination ammonium salt and the epoxy group of part associated products is reduced to hydroxyl,
Related solvents are removed via concentration, and carry out the impurity such as adsorpting pigment using water as carrier with active carbon.It is finally obtained above-mentioned
Substance.
The DMF solution of present invention sucrose-6-ester mentioned above is that sucrose generates in DMF solution with tin catalyst
The sucrose-6-ester that is generated under conditions of acetic anhydride of complex compound, the DMF that sucrose-6-ester is obtained after extraction concentration is molten
Liquid.
Present invention extraction mentioned above, the solvent used is methyl acetate, ethyl acetate, butyl acetate, two chloroethenes
Alkane, trichloroethanes, any one in hexamethylene；Tin catalyst is by tin compound and acid anhydrides substance in hexamethylene
The substance dissolved in alkane.
Embodiment 1
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately takes three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, be cooled to 20 DEG C after removing active carbon, 50ml ethyl acetate be added, filtered after slowly precipitating crystal
Crystal is obtained, and detects material purity with HPLC-ELSD, is recrystallized in 200ml water, detects material purity again.
Embodiment 2
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately take three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, be cooled to 20 DEG C after removing active carbon, 40ml ethyl acetate be added, filtered after slowly precipitating crystal
Crystal is obtained, and detects material purity with HPLC-ELSD, is recrystallized in 200ml water, detects material purity again.
Embodiment 3
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately takes three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, be cooled to 20 DEG C after removing active carbon, 40ml butyl acetate be added, filtered after slowly precipitating crystal
Crystal is obtained, and detects material purity with HPLC-ELSD, is recrystallized in 200ml water, detects material purity again.
Embodiment 4
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately takes three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, remove active carbon after do not cool down, be added 40ml ethyl acetate, slow cooling precipitates crystal laggard to 20 DEG C
Row, which filters, obtains crystal, and detects material purity with HPLC-ELSD, is recrystallized in 200ml water, detects substance again
Purity.Embodiment 1
Embodiment 5
Removal organic solvent is concentrated in the mother liquor for collecting primary crystallization first, and detection Determination of Residual Organic Solvents is 0.01%, evaporates
Divide and show delamination, upper layer is transferred to head tank and reuses, and continues to be concentrated, and detecting substance residual in fraction is trichlorine
Ethane 0.01%, DMF residual 0.02%, reaches the index for applying circulation.And the mother liquor for collecting recrystallization mix it is spare at one piece.
An instance analysis 2 is re-started, the water added in decolorization process is using above-mentioned used solution.It is carried out with 5g active carbon
Decoloration does not cool down after removing active carbon, and 40ml ethyl acetate is added, and slow cooling filter after precipitating crystal to 20 DEG C
Material purity is detected to crystal, and with HPLC-ELSD, is recrystallized in 200ml water, detects material purity again.
Comparative example 1
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately take three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, remove active carbon after with three times ethyl acetate extract, extraction after be concentrated into it is more dry after be added 200ml water
Continue to be concentrated out after 50ml comes out to no ethyl acetate, decrease temperature crystalline, and detects material purity with HPLC-ELSD.?
It is recrystallized in 200ml water, detects material purity again.
68.4g sucrose addition 280mlDMF rising temperature for dissolving, 99.6g Dibutyltin oxide addition 20.4ml acetic anhydride,
240ml hexamethylene rising temperature for dissolving, mixes two kinds of solution, and heating vacuum concentration solvent simultaneously adds DMF to fixed liquid level.Cooling drop
After adding the extraction three times of 24g acetic anhydride hexamethylene, syrup is concentrated to get the DMF solution of cane sugar-6-acetic ester, separately take three mouthfuls
600ml trichloroethanes is added in flask, and syrup is slowly added dropwise in 125ml thionyl chloride, is all to slowly warm up to 112 after dissolution
DEG C, keep the temperature 2 hours.20 DEG C are cooled to, is slowly added to be concentrated after sodium hydroxide adjusting PH is 9, and it is living that 400ml water 5g is added
Property charcoal decolourize, remove active carbon after with three times ethyl acetate extract, extraction after be concentrated into it is more dry after be added 200ml water
Continue to be concentrated out after 50ml comes out to no ethyl acetate, decrease temperature crystalline, and detects material purity with HPLC-ELSD.?
It is recrystallized in 200ml water, detects material purity again.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited to
This, anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention
And its inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of Sucralose crystallization processes, it is characterised in that: the following steps are included:
Step 1: sucrose-6-ester is added rising temperature for dissolving in DMF, obtains the DMF solution of sucrose-6-ester by esterification；
Step 2: trichloroethanes and thionyl chloride is added in chlorination reaction in the DMF solution of sucrose-6-ester, all after dissolution
It is to slowly warm up to certain temperature and held for some time, obtains sucralose-6-ester aqueous solution with high salt；
Step 3: neutralizing concentration, is added after buck adjusts pH value and is concentrated in sucralose-6-ester aqueous solution with high salt,
Obtain concentration sucralose-6-ester aqueous solution；
Step 4: decolorization adsorption is decolourized with active carbon, is obtained after being diluted with water in concentration sucralose-6-ester aqueous solution
To decoloration sucralose-6-ester aqueous solution；
Step 5: primary crystallization is added organic solvent after removing active carbon in decoloration sucralose-6-ester aqueous solution, is precipitated
It is filtered to obtain crystal after crystal；
Step 6: it recrystallization: will be recrystallized after the dissolution of crystals being precipitated in step 5；
Step 7: disposing mother liquor utilizes: being concentrated after the mother liquor of primary crystallization to be concentrated to removal organic solvent first, what is obtained reaches
Decolorization adsorption and crystallization processes are carried out after mixing after the solution of index with the mother liquor of recrystallization again.
2. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that the organic solvent is acetic acid
Methyl esters, ethyl acetate, butyl acetate, dichloroethanes, trichloroethanes, any one in hexamethylene.
3. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that the amount using organic solvent is de-
The 1/10-3/10 of color sucralose-6-ester aqueous solution.
4. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that the temperature before organic solvent is added
Control is between 10-30 DEG C.
5. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that the temperature after organic solvent is added
Control is between 10-30 DEG C.
6. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that sucrose-in the esterification
The DMF solution of 6- ester is that sucrose generates under conditions of acetic anhydride in DMF solution with the complex compound of tin catalyst generation
Sucrose-6-ester obtains the DMF solution of sucrose-6-ester after extraction concentration.
7. a kind of Sucralose crystallization processes according to claim 6, which is characterized in that the solvent that uses of extracting is
Methyl acetate, ethyl acetate, butyl acetate, dichloroethanes, trichloroethanes, any one in hexamethylene.
8. a kind of Sucralose crystallization processes according to claim 6, which is characterized in that the tin catalyst is to pass through
The substance that tin compound and acid anhydrides substance are dissolved in hexamethylene.
9. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that the Sucralose -6- with high salt
Aqueous solution of ester the preparation method is as follows:
Step 1: trichloroethanes is added in the DMF solution of sucrose-6-ester, and heats up after thionyl chloride is added dropwise in low temperature
2 hours are kept the temperature to 112.5 DEG C；
Step 2: being added sodium hydroxide after cooling or ammonium hydroxide generates chlorination ammonium salt and is reduced to the epoxy group of associated products
Hydroxyl；
Step 3: related solvents are removed via concentration, and carry out the impurity such as adsorpting pigment using water as carrier with active carbon；Final
To sucralose-6-ester aqueous solution with high salt.
10. a kind of Sucralose crystallization processes according to claim 1, which is characterized in that primary in the step 7
Removal organic solvent is concentrated in the mother liquor of crystallization first, and detection Determination of Residual Organic Solvents is 0.01%, and fraction shows delamination,
Upper layer is transferred to head tank and reuses, and continues to be concentrated, and detecting substance residual in fraction is trichloroethanes 0.01%, DMF residual
0.02%, reach the index for applying circulation.
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| CN111574572A (en) * | 2020-05-22 | 2020-08-25 | 安徽金禾实业股份有限公司 | Continuous preparation and supplement method of organic tin catalyst in sucralose production |
| CN112638924A (en) * | 2020-11-27 | 2021-04-09 | 安徽金禾实业股份有限公司 | Purification method of sucralose-6-ethyl ester |
| CN113150047A (en) * | 2021-04-26 | 2021-07-23 | 南通市常海食品添加剂有限公司 | Method for separating and extracting sucralose-6-acetate |
| CN113214330A (en) * | 2021-05-13 | 2021-08-06 | 安徽金禾化学材料研究所有限公司 | Purification and chlorination process of sucrose-6-ethyl ester |
| WO2024082158A1 (en) * | 2022-10-19 | 2024-04-25 | 安徽金禾实业股份有限公司 | Method for preparing sucralose crude product by using sucralose-6-acetate crystallization mother liquor |
| WO2024082157A1 (en) * | 2022-10-19 | 2024-04-25 | 安徽金禾实业股份有限公司 | Method for preparing crude sucralose using improved alcohol-water alkaline hydrolysis system |
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| CN111574572A (en) * | 2020-05-22 | 2020-08-25 | 安徽金禾实业股份有限公司 | Continuous preparation and supplement method of organic tin catalyst in sucralose production |
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| CN113150047A (en) * | 2021-04-26 | 2021-07-23 | 南通市常海食品添加剂有限公司 | Method for separating and extracting sucralose-6-acetate |
| CN113214330A (en) * | 2021-05-13 | 2021-08-06 | 安徽金禾化学材料研究所有限公司 | Purification and chlorination process of sucrose-6-ethyl ester |
| WO2024082158A1 (en) * | 2022-10-19 | 2024-04-25 | 安徽金禾实业股份有限公司 | Method for preparing sucralose crude product by using sucralose-6-acetate crystallization mother liquor |
| WO2024082157A1 (en) * | 2022-10-19 | 2024-04-25 | 安徽金禾实业股份有限公司 | Method for preparing crude sucralose using improved alcohol-water alkaline hydrolysis system |
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