CN110204581A - A kind of improved separation trichloro-cane-6-ethyl ester method - Google Patents
A kind of improved separation trichloro-cane-6-ethyl ester method Download PDFInfo
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Abstract
The present invention relates to a kind of methods of improved separation trichloro-cane-6-ethyl ester, and technical solution is: each series extraction has only used primary new ethyl acetate, except A is serial.If the amount for the ethyl acetate used in B series is 0.5 to 1 times of B0.Ethyl acetate economy ratio is exactly 0.5 to 1 in so B series, and so on.The beneficial effects of the present invention are: solving the problems, such as that ethyl acetate dosage is excessive, evaporation-concentration step is avoided, reduces energy consumption.By it is described move in circles apply extraction after ethyl acetate phase method, significantly reduce ethyl acetate dosage, ethyl acetate economy is than being reduced to≤1 from the 3.2 of conventional method.The first ethyl acetate phase of each serial experiment, B1, C1, D1 etc., trichloro-cane-6-ethyl ester content is very high, direct decrease temperature crystalline, and suction filtration obtains trichloro-cane-6-ethyl ester solid, eliminates concentration step, reduces energy consumption and ethyl acetate loss.
Description
Technical field
The present invention relates to a kind of method for separating trichloro-cane-6-ethyl ester, in particular to a kind of improved separation trichlorine sugarcanes
Sugar -6- ethyl ester method.
Background technique
Sucralose (No. CAS: 56038-13-2) is a kind of novel sweetener, has high (about the 600 of sucrose of sugariness
Times), it is highly soluble in water, the advantages that heat is low, and human body hardly picks up, market prospects are boundless.Industrial synthesis three at present
The method of chlorine sucrose are as follows: using sucrose as raw material, sucrose-6-ethyl ester is made through esterification in sucrose, then to sucrose-6-ethyl ester into
Row chlorination obtains trichloro-cane-6-ethyl ester, finally carries out de- ester to trichloro-cane-6-ethyl ester and obtains Sucralose.
In sucrose trichloride production process, the chlorated liquid that wherein chloridization process generates adds ammonium hydroxide tune pH, adds by cooling
Hydrochloric acid neutralizes, and concentration and recovery trichloroethanes and DMF solvent are dissolved in water to obtain liquid to be extracted, the 1 ton of white granulated sugar that feeds intake about obtains 7m
3 liquid to be extracted, trichloro-cane-6-ethyl ester content are about 70 to 90g/L.As shown in Figure 1.
Liquid and ethyl acetate to be extracted enter extraction tower simultaneously, and trichloro-cane-6-ethyl ester enters ethyl acetate from water phase
Phase, finally from overhead extraction, referred to as extraction light liquid.Tower bottom extraction extraction heavy-fluid, trichloro-cane-6-ethyl ester content < 5g/L.
As shown in Figure 2.
According to the liquid to be extracted of knowhow extraction 1m3, the ethyl acetate of 3.2m3 need to be used.Obtained extraction light liquid
For volume also in 3.2m3, -6 ethyl ester content of Sucralose is about 27g/L or so.
Light liquid is extracted by active carbon decoloring, into concentration kettle, vacuum distillation removes ethyl acetate, is then added originally
Water, decrease temperature crystalline, filters pressing obtain trichloro-cane-6-ethyl ester primary crystal product.As shown in Figure 1.
This production method has two:
First, ethyl acetate dosage is bigger than normal, and enabling the ratio of the volume for extracting ethyl acetate used and liquid to be extracted product is " acetic acid
Ethyl ester economy ratio ", then the value of ethyl acetate economy ratio is 3.2 in above-mentioned technique
Second, solvent loss, steam, power consumption is bigger than normal, cumbersome
Main cause is that ethyl acetate dosage is big, extraction light liquid volume it is big, trichloro-cane-6-ethyl ester content is relatively low, need using
Vacuum pump, reaction kettle, the equipment such as condenser carry out vacuum distillation and remove ethyl acetate.This process loss ethyl acetate, steam,
Electric power.
Third, crystallization process are easy to appear unstable situation
Liquid to be extracted is due to containing the impurity compositions such as certain superchlorination substance, pigment, caramel, once these substance too high levels
Then hinder crystallization process of the trichloro-cane-6-ethyl ester in aqueous phase system.
Chinese patent literature Publication No. CN108299522A, patent name are a kind of " extraction of trichloro-cane-6-ethyl ester
Method ", the patent the following steps are included: a. dense dry liquid that obtains chlorination reaction 1:1.5 adds by volume with dimethyl carbonate
Enter into extraction kettle, sufficiently circulation is sent into layering slot and stands 1.5 hours；B. an organic phase of layering decoloration kettle is sent into take off
Color, destainer, which is sent into, is concentrated under reduced pressure kettle, recycles extractant dimethyl carbonate DMC, is then crystallized, filters pressing, obtained to concentrate
Obtain trichloro-cane-6-ethyl ester crude product；C. by a water phase after layering, 1:1.5 is added to extraction by volume with dimethyl carbonate
Kettle carries out reextraction, is then fed into layering slot standing and is layered for 1.5 hours；D. by the secondary water phase of layering be sent into tower reactor into
Molten dimethyl carbonate in water is recycled in row air-distillation.The present invention selects extractant DMC extraction efficiency high, reduces volatilization
Consumption, while the price of DMC is about the half of ethyl acetate price, has greatly saved the energy, is reduced costs, and effect is increased
Benefit.Although mentioning the operation of " secondary ester is mutually applied to extraction kettle " in the patent document, ethyl acetate is reduced to a certain extent
Dosage, but still cannot thoroughly solve the problems, such as.
Summary of the invention
The purpose of the present invention is to drawbacks described above of the existing technology, provide a kind of improved separation trichlorine sugarcane
Sugar -6- ethyl ester method, by move in circles above apply extraction after ethyl acetate phase method, significantly reduce acetic acid second
Ester dosage, ethyl acetate economy is than being reduced to≤1 from the 3.2 of conventional method.
The improved separation trichloro-cane-6-ethyl ester method of one kind that the present invention mentions, technical solution is: including following step
It is rapid:
One, single batch of liquid to be extracted of the 1st series extraction, referred to as A series, specific practice are as follows:
It takes liquid A0 to be extracted to mix with ethyl acetate, shakes stratification, an isolated ethyl ester phase A1 i.e. light liquid, water phase
An A1 ' i.e. heavy-fluid, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0, i.e. the economy of ethyl acetate
Than being between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A1 ', stratification, isolated ethyl ester phase A2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of A2 ', wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A2 ', stratification is shaken, isolated ethyl ester phase A3 i.e. light liquid three times, water phase
A3 ' i.e. heavy-fluid three times, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A3 ', stratification, isolated ethyl ester phase A4 i.e. four light liquids, water phase are shaken
A4 ' i.e. four time heavy-fluid, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
Detect water phase A4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row A5, A6, obtain water phase A5 ' and water phase A6 ', and the trichloro-cane-6-ethyl ester in water phase A6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and A0 are 1, i.e., when ethyl acetate economy ratio is equal to 1, Sucralose -6- second in water phase A4 '
Ester content is less than 5g/L；When the volume ratio of ethyl acetate and A0 are 0.5, i.e., when ethyl acetate economy ratio is equal to 0.5, then water phase
Trichloro-cane-6-ethyl ester content is less than 5g/L in A6 '；
Ethyl ester phase A1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid As, mother liquor As '；
Two, single batch of liquid to be extracted of the 2nd series extraction, referred to as B series, specific practice are as follows:
It takes liquid B0 to be extracted to mix with ethyl ester phase A2, shakes stratification, an isolated ethyl ester phase B1 i.e. light liquid, water phase
A B1 ' i.e. heavy-fluid, wherein extract liquor B0 volume is equal with extract liquor A0；
To ethyl ester phase A3 mixing is added in aqueous phase B 1 ', stratification, isolated ethyl ester phase B2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of B2 '；
To ethyl ester phase A4 mixing is added in aqueous phase B 2 ', stratification is shaken, isolated ethyl ester phase B3 i.e. light liquid three times, water phase
B3 ' i.e. heavy-fluid three times；
To ethyl acetate is added in aqueous phase B 3 ', stratification is shaken, isolated ethyl ester phase B4 i.e. four light liquids, aqueous phase B 4 ' is i.e.
Four heavy-fluids, wherein the volume ratio of ethyl acetate and extract liquor B0 are between 0.5 to 1.0；
Detect aqueous phase B 4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row B5, B6, obtain aqueous phase B 5 ' and aqueous phase B 6 ', and the trichloro-cane-6-ethyl ester in aqueous phase B 6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and extract liquor B0 are that 1 when, that is, ethyl acetate economy ratio is equal to 1, then trichlorine sugarcane in aqueous phase B 4 '
Sugar -6- ethyl ester content is less than 5g/L；When the volume ratio of ethyl acetate and extract liquor B0 are 0.5, i.e. ethyl acetate economy ratio etc.
When 0.5, then trichloro-cane-6-ethyl ester content is less than 5g/L in aqueous phase B 6 '；
Ethyl ester phase B1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid Bs, mother liquor Bs '；
Three, single batch of liquid to be extracted of the 3rd series extraction, referred to as C series, specific practice are as follows:
It takes liquid C0 to be extracted to mix with ethyl ester phase B2, shakes stratification, an isolated ethyl ester phase C1 i.e. light liquid, water phase
A C1 ' i.e. heavy-fluid, wherein extract liquor C0 volume is equal with extract liquor A0；
To ethyl ester phase B3 mixing is added in water phase C1 ', stratification, isolated ethyl ester phase C2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of C2 '；
To ethyl ester phase B4 mixing is added in water phase C2 ', stratification is shaken, isolated ethyl ester phase C3 i.e. light liquid three times, water phase
C3 ' i.e. heavy-fluid three times；
To ethyl acetate is added in water phase C3 ', stratification is shaken, isolated ethyl ester phase C4 i.e. four light liquids, water phase C4 ' is i.e.
Four heavy-fluids, wherein the volume ratio of ethyl acetate and extract liquor C0 are between 0.5 to 1.0；
Detect water phase C4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row C5, C6, obtain water phase C5 ' and water phase C6 ', and the trichloro-cane-6-ethyl ester in water phase C6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and extract liquor C0 be 1 i.e. ethyl acetate economy ratio is equal to 1 when, then trichlorine sugarcane in water phase C4 '
Sugar -6- ethyl ester content is less than 5g/L；When the volume ratio of ethyl acetate and extract liquor C0 is that 0.5 i.e. ethyl acetate economy ratio is equal to
When 0.5, then trichloro-cane-6-ethyl ester content is less than 5g/L in water phase C6 '；
Ethyl ester phase C1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid Cs, mother solution C s '；
It loops back and forth like this, it is subsequent to have D series, E series.
Preferably, during extracting single series extraction, extraction times are 4 to 6 times, trichlorine sugarcane in last time water phase
The content of sugar -6- ethyl ester is less than 5g/L, the volume ratio of ethyl acetate or ethyl acetate phase and liquid to be extracted be 0.5 to 1 it
Between, i.e., ethyl acetate economy ratio is between 0.5 to 1.
Preferably, decoloration and concentration step are omitted, by the first ethyl ester phase decrease temperature crystalline of each series, suction filtration obtains trichlorine
Sucrose-6-ethyl ester primary crystal.
The beneficial effects of the present invention are: each series extraction of the invention has only used primary new ethyl acetate, A series is removed
Outside, if the amount for the ethyl acetate used in B series is 0.5 to 1 times of B0, ethyl acetate economy ratio is exactly in B series
0.5 to 1, and so on；
In addition, significantly reducing acetic acid second by the method for applying ethyl acetate phase after extraction to move in circles described above
Ester dosage, ethyl acetate economy is than being reduced to≤1 from the 3.2 of conventional method；
Furthermore the first ethyl acetate phase of each series, B1, C1, D1 etc., trichloro-cane-6-ethyl ester content is very high, directly
Decrease temperature crystalline, suction filtration obtain trichloro-cane-6-ethyl ester solid, eliminate decoloration concentration step, reduce energy consumption and acetic acid second
Ester loss.
Detailed description of the invention
Fig. 1 chlorated liquid is to trichloro-cane-6-ethyl ester primary crystal flow chart；
Fig. 2 trichloro-cane-6-ethyl ester extraction procedure figure；
A1 crystallization figure in Fig. 3 embodiment 1；
Relational graph between trichloro-cane-6-ethyl ester content and ethyl ester phase order in the extraction serial experiment of Fig. 4 embodiment 1；
A1 crystallization figure in Fig. 5 embodiment 2；
Relational graph between trichloro-cane-6-ethyl ester content and ethyl ester phase order in the extraction serial experiment of Fig. 6 embodiment 2.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1: the improved separation trichloro-cane-6-ethyl ester method of one kind that the present invention mentions, with ethyl acetate economy
For being equal to 1, following procedure is specifically included:
One, single batch of liquid to be extracted of the 1st series extraction, referred to as A series, specific practice are as follows:
Liquid 4L to be extracted is taken, is rocked uniformly, sampling analysis trichloro-cane-6-ethyl ester content is 75.8g/L, real for extraction series
Test use.
Take wherein 500.02g be denoted as extract liquor A0, be placed in 2000mL pears type separatory funnel, the shake of 500g ethyl acetate be added
Rear stratification is swung, upper layer ethyl ester phase 539.17g is separated, is denoted as ethyl ester phase A1, separates lower layer water phase 457.98g, is denoted as water phase
A1 ' analyzes and contains trichloro-cane-6-ethyl ester 42.37g/L in ethyl ester phase A1, contains trichloro-cane-6-ethyl ester in water phase A1 '
22.27g/L。
Water phase A1 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 500g ethyl acetate is added, separates
Upper layer ethyl ester phase 507.27g is denoted as ethyl ester phase A2, and separates lower layer water phase 440.70g, is denoted as water phase A2 ', analyzes ethyl ester phase A2
In contain trichloro-cane-6-ethyl ester 10.75g/L, trichloro-cane-6-ethyl ester 9.61g/L is contained in water phase A2 '.
Water phase A2 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 500g ethyl acetate is added, separates
Upper layer ethyl ester phase 490.95g is denoted as ethyl ester phase A3, and separates lower layer water phase 440.65g, is denoted as water phase A3 ', analyzes ethyl ester phase A3
In contain trichloro-cane-6-ethyl ester 4.21g/L, trichloro-cane-6-ethyl ester 3.97g/L is contained in water phase A3 '.
Water phase A3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 500g ethyl acetate is added, separates
Upper layer ethyl ester phase 486.01g is denoted as ethyl ester phase A4, and separates lower layer water phase 446.43g, is denoted as water phase A4 ', analyzes ethyl ester phase A4
In contain trichloro-cane-6-ethyl ester 1.63g/L, trichloro-cane-6-ethyl ester 1.85g/L is contained in water phase A4 '.
Ethyl ester phase A1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 8 hours, obtains trichlorine sugarcane as shown in figure 3, filtering
Sugar -6- ethyl ester crystalline solid As 48.43g, purity 58.21%, its trichloro-cane-6-ethyl ester content of mother liquor As ' 455.06g
11.21g/L。
Two, single batch of liquid to be extracted of the 2nd series extraction, referred to as B series, specific practice are as follows:
It takes liquid 500.05g to be extracted to be denoted as extract liquor B0, is placed in 2000mL pears type separatory funnel, after ethyl ester phase A2 concussion is added
Stratification separates upper layer ethyl ester phase 532.10g, is denoted as ethyl ester phase B1, and separates lower layer water phase 457.28g, is denoted as aqueous phase B 1 ',
It analyzes and contains trichloro-cane-6-ethyl ester 51.21g/L in ethyl ester phase B1, contain trichloro-cane-6-ethyl ester 25.72g/ in aqueous phase B 1 '
L。
Aqueous phase B 1 ' is placed in 2000mL pears type separatory funnel, stratification after ethyl ester phase A3 concussion is added, separates upper layer
Ethyl ester phase 481.90g is denoted as ethyl ester phase B2, and separates lower layer water phase 458.38g, is denoted as aqueous phase B 2 ', analyzes in B2 and contains trichlorine
Contain trichloro-cane-6-ethyl ester 11.28g/L in sucrose-6-ethyl ester 16.14g/L, B2 '.
Aqueous phase B 2 ' is placed in 2000mL pears type separatory funnel, stratification after A4 concussion is added, separates upper layer ethyl ester phase
468.87g is denoted as ethyl ester phase B3, and separates lower layer water phase 461.47g, is denoted as aqueous phase B 3 ', analyzes in ethyl ester phase B3 and contains trichlorine
Contain trichloro-cane-6-ethyl ester 5.57g/L in sucrose-6-ethyl ester 6.77g/L, B3 '.
Aqueous phase B 3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 500g ethyl acetate is added, separates
Upper layer ethyl ester phase 511.52g is denoted as ethyl ester phase B4, and separates lower layer water phase 443.14g, is denoted as aqueous phase B 4 ', analyzes and contains in B4
Trichloro-cane-6-ethyl ester 2.67g/L contains trichloro-cane-6-ethyl ester 2.35g/L in aqueous phase B 4 '.
Ethyl ester phase B1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester knot
Brilliant solid Bs 50.40g, purity 65.84%, its trichloro-cane-6-ethyl ester content of mother liquor Bs ' 422.67g 16.10g/L.
It repeats above step and carries out C series, D serial experiment, and experimental data is aggregated into 1 table 2 of table
1 embodiment 1 of table extracts serial experiment data summary table
2 embodiment 1 of table crystallizes serial experimental data summary sheet
Order is mutually obtained as ordinate to extract ethyl ester, using the content of trichloro-cane-6-ethyl ester as ordinate, is drawn as shown in Figure 4.
2 ethyl acetate economy ratio of embodiment is equal to 0.5
One, single batch of liquid to be extracted of the 1st series extraction, referred to as A series, specific practice are as follows:
Liquid 4L to be extracted is taken, is rocked uniformly, sampling analysis trichloro-cane-6-ethyl ester content is 76.24g/L, real for extraction series
Test use.
Take wherein 500.06g be denoted as extract liquor A0, be placed in 2000mL pears type separatory funnel, the shake of 250g ethyl acetate be added
Rear stratification is swung, upper layer ethyl ester phase 279.58g is separated, is denoted as ethyl ester phase A1, separates lower layer water phase 466.82g, is denoted as water phase
A1 ' analyzes and contains trichloro-cane-6-ethyl ester 78.59g/L in ethyl ester phase A1, contains trichloro-cane-6-ethyl ester in water phase A1 '
25.51g/L。
Water phase A1 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 251.28g is denoted as ethyl ester phase A2, and separates lower layer water phase 455.17g, is denoted as water phase A2 ', analyzes and contains in A2
Contain trichloro-cane-6-ethyl ester 12.23g/L in trichloro-cane-6-ethyl ester 22.38g/L, water phase A2 '.
Water phase A2 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 246.06g is denoted as ethyl ester phase A3, and separates lower layer water phase 450.23g, is denoted as water phase A3 ', analyzes and contains in A3
Contain trichloro-cane-6-ethyl ester 5.67g/L in trichloro-cane-6-ethyl ester 10.19g/L, water phase A3 '.
Water phase A3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 245.14g is denoted as ethyl ester phase A4, and separates lower layer water phase 446.31g, is denoted as water phase A4 ', analyzes and contains in A4
Contain trichloro-cane-6-ethyl ester 2.69g/L in trichloro-cane-6-ethyl ester 4.78g/L, water phase A4 '.
Ethyl ester phase A1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 8 hours, obtains trichlorine sugarcane as shown in figure 5, filtering
Sugar -6- ethyl ester crystalline solid As 48.43g, purity 58.21%, its trichloro-cane-6-ethyl ester content of mother liquor As ' 455.06g
11.21g/L。
Two, single batch of liquid to be extracted of the 2nd series extraction, referred to as B series, specific practice are as follows:
It takes liquid 500.11g to be extracted to be denoted as B0, is placed in 2000mL pears type separatory funnel, stratification after A2 concussion is added, point
Upper layer ethyl ester phase 281.15g out is denoted as ethyl ester phase B1, and separates lower layer water phase 462.13g, is denoted as aqueous phase B 1 ', analyzes and contains in B1
There is trichloro-cane-6-ethyl ester 95.30g/L, contains trichloro-cane-6-ethyl ester 30.12g/L in B1 '.
Aqueous phase B 1 ' is placed in 2000mL pears type separatory funnel, stratification after ethyl ester phase A3 concussion is added, separates upper layer
Ethyl ester phase 246.33g is denoted as ethyl ester phase B2, and separates lower layer water phase 449.64g, is denoted as aqueous phase B 2 ', analyzes in B2 and contains trichlorine
Contain trichloro-cane-6-ethyl ester 17.42g/L in sucrose-6-ethyl ester 32.58g/L, B2 '.
Aqueous phase B 2 ' is placed in 2000mL pears type separatory funnel, stratification after ethyl ester phase A4 concussion is added, separates upper layer
Ethyl ester phase 240.77g is denoted as ethyl ester phase B3, and separates lower layer water phase 441.12g, is denoted as aqueous phase B 3 ', analyzes and contains in ethyl ester phase B3
There is trichloro-cane-6-ethyl ester 17.26g/L, contains trichloro-cane-6-ethyl ester 9.95g/L in B3 '.
Aqueous phase B 3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 244.46g is denoted as ethyl ester phase B4, and separates lower layer water phase 439.80g, is denoted as aqueous phase B 4 ', analyzes ethyl ester phase B4
In contain trichloro-cane-6-ethyl ester 7.92g/L, trichloro-cane-6-ethyl ester 1.93g/L is contained in aqueous phase B 4 '.
Ethyl ester phase B1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester knot
Brilliant solid Bs 50.40g, purity 65.84%, its trichloro-cane-6-ethyl ester content of mother liquor Bs ' 422.67g 16.10g/L.
Three, single batch of liquid to be extracted of the 3rd series extraction, referred to as C series, specific practice are as follows:
It takes liquid 500.49g to be extracted to be denoted as extract liquor C0, is placed in 2000mL pears type separatory funnel, after ethyl ester phase B2 concussion is added
Stratification separates upper layer ethyl ester phase 276.83g, is denoted as ethyl ester phase C1, and separates lower layer water phase 460.56g, is denoted as water phase C1 ',
It analyzes and contains trichloro-cane-6-ethyl ester 105.14g/L in ethyl ester phase C1, contain trichloro-cane-6-ethyl ester in aqueous phase B 1 '
31.27g/L。
Water phase C1 ' is placed in 2000mL pears type separatory funnel, stratification after B3 concussion is added, separates upper layer ethyl ester phase
241.90g is denoted as ethyl ester phase C2, and separates lower layer water phase 447.41g, is denoted as water phase C2 ', analyzes in ethyl ester phase C2 and contains trichlorine
Contain trichloro-cane-6-ethyl ester 19.54g/L in sucrose-6-ethyl ester 39.20g/L, water phase C2 '.
Water phase C2 ' is placed in 2000mL pears type separatory funnel, stratification after ethyl ester phase B4 concussion is added, separates upper layer
Ethyl ester phase 241.06g is denoted as ethyl ester phase C3, and separates lower layer water phase 437.14g, is denoted as water phase C3 ', analyzes and contains in ethyl ester phase C3
There is trichloro-cane-6-ethyl ester 19.90g/L, contains trichloro-cane-6-ethyl ester 12.04g/L in water phase C3 '.
Water phase C3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 245.98g is denoted as ethyl ester phase C4, and separates lower layer water phase 434.26g, is denoted as water phase C4 ', analyzes ethyl ester phase C4
In contain trichloro-cane-6-ethyl ester 9.35g/L, trichloro-cane-6-ethyl ester 5.80g/L is contained in water phase C4 '.
Water phase C4 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 244.45g is denoted as ethyl ester phase C5, and separates lower layer water phase 431.33g, is denoted as water phase C5 ', analyzes ethyl ester phase C5
In contain trichloro-cane-6-ethyl ester 4.55g/L, trichloro-cane-6-ethyl ester 2.71g/L is contained in water phase C5 '.
C1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystalline solid
Cs 50.40g, purity 65.84%, its trichloro-cane-6-ethyl ester content of mother solution C s ' 422.67g 16.10g/L.
Four, single batch of liquid to be extracted of the 4th series extraction, referred to as D series, specific practice are as follows:
It takes liquid 500.06g to be extracted to be denoted as D0, is placed in 2000mL pears type separatory funnel, stratification after C2 concussion is added, point
Upper layer ethyl ester phase 272.00g out is denoted as D1, and separates lower layer water phase 462.36g, is denoted as water phase D1 ', analyzes in D1 and contains trichlorine
Contain trichloro-cane-6-ethyl ester 33.82g/L in sucrose-6-ethyl ester 108.92g/L, B1 '.
Water phase D1 ' is placed in 2000mL pears type separatory funnel, stratification after C3 concussion is added, separates upper layer ethyl ester phase
242.42g is denoted as D2, and separates lower layer water phase 448.15g, is denoted as water phase D2 ', analyzes in D2 and contains trichloro-cane-6-ethyl ester
41.25g/L, D2 ' in contain trichloro-cane-6-ethyl ester 20.86g/L.
Water phase D2 ' is placed in 2000mL pears type separatory funnel, stratification after C4 concussion is added, separates upper layer ethyl ester phase
242.33g is denoted as D3, and separates lower layer water phase 440.09g, is denoted as water phase D3 ', analyzes in D3 and contains trichloro-cane-6-ethyl ester
23.07g/L, D3 ' in contain trichloro-cane-6-ethyl ester 13.56g/L.
Water phase D3 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 240.12g is denoted as D4, and separates lower layer water phase 433.03g, is denoted as water phase D4 ', analyzes and contains trichlorine sugarcane in D4
Contain trichloro-cane-6-ethyl ester 8.07g/L in sugar -6- ethyl ester 12.19g/L, water phase D4 '.
Water phase D4 ' is placed in 2000mL pears type separatory funnel, stratification after the concussion of 250g ethyl acetate is added, separates
Upper layer ethyl ester phase 244.33g is denoted as D5, and separates lower layer water phase 431.09g, is denoted as water phase D5 ', analyzes and contains trichlorine sugarcane in D5
Contain trichloro-cane-6-ethyl ester 3.87g/L in sugar -6- ethyl ester 6.34g/L, water phase D5 '.
D1 is placed in 5 DEG C of cold compartment of refrigerator and stands crystallization in 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystalline solid
Ds 50.40g, purity 65.84%, its trichloro-cane-6-ethyl ester content of mother liquor Ds ' 422.67g 16.10g/L.
3 embodiment 2 of table extracts serial experiment data summary table
4 embodiment 2 of table crystallizes serial experimental data summary sheet
Order is mutually obtained as ordinate to extract ethyl ester, using the content of trichloro-cane-6-ethyl ester as ordinate, is drawn as shown in Figure 6.
The above, is only part preferred embodiment of the invention, and anyone skilled in the art may benefit
Equivalent technical solution is modified or is revised as with the technical solution of above-mentioned elaboration.Therefore, technology according to the present invention
Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.
Claims (3)
1. a kind of improved separation trichloro-cane-6-ethyl ester method, it is characterized in that: the following steps are included:
One, single batch of liquid to be extracted of the 1st series extraction, referred to as A series, specific practice are as follows:
It takes liquid A0 to be extracted to mix with ethyl acetate, shakes stratification, an isolated ethyl ester phase A1 i.e. light liquid, water phase
An A1 ' i.e. heavy-fluid, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0, i.e. the economy of ethyl acetate
Than being between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A1 ', stratification, isolated ethyl ester phase A2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of A2 ', wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A2 ', stratification is shaken, isolated ethyl ester phase A3 i.e. light liquid three times, water phase
A3 ' i.e. heavy-fluid three times, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
To ethyl acetate mixing is added in water phase A3 ', stratification, isolated ethyl ester phase A4 i.e. four light liquids, water phase are shaken
A4 ' i.e. four time heavy-fluid, wherein the volume ratio of ethyl acetate and extract liquor A0 are between 0.5 to 1.0；
Detect water phase A4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row A5, A6, obtain water phase A5 ' and water phase A6 ', and the trichloro-cane-6-ethyl ester in water phase A6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and A0 are 1, i.e., when ethyl acetate economy ratio is equal to 1, Sucralose -6- second in water phase A4 '
Ester content is less than 5g/L；When the volume ratio of ethyl acetate and A0 are 0.5, i.e., when ethyl acetate economy ratio is equal to 0.5, then water phase
Trichloro-cane-6-ethyl ester content is less than 5g/L in A6 '；
Ethyl ester phase A1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid As, mother liquor As '；
Two, single batch of liquid to be extracted of the 2nd series extraction, referred to as B series, specific practice are as follows:
It takes liquid B0 to be extracted to mix with ethyl ester phase A2, shakes stratification, an isolated ethyl ester phase B1 i.e. light liquid, water phase
A B1 ' i.e. heavy-fluid, wherein extract liquor B0 volume is equal with extract liquor A0；
To ethyl ester phase A3 mixing is added in aqueous phase B 1 ', stratification, isolated ethyl ester phase B2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of B2 '；
To ethyl ester phase A4 mixing is added in aqueous phase B 2 ', stratification is shaken, isolated ethyl ester phase B3 i.e. light liquid three times, water phase
B3 ' i.e. heavy-fluid three times；
To ethyl acetate is added in aqueous phase B 3 ', stratification is shaken, isolated ethyl ester phase B4 i.e. four light liquids, aqueous phase B 4 ' is i.e.
Four heavy-fluids, wherein the volume ratio of ethyl acetate and extract liquor B0 are between 0.5 to 1.0；
Detect aqueous phase B 4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row B5, B6, obtain aqueous phase B 5 ' and aqueous phase B 6 ', and the trichloro-cane-6-ethyl ester in aqueous phase B 6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and extract liquor B0 are that 1 when, that is, ethyl acetate economy ratio is equal to 1, then trichlorine sugarcane in aqueous phase B 4 '
Sugar -6- ethyl ester content is less than 5g/L；When the volume ratio of ethyl acetate and extract liquor B0 are 0.5, i.e. ethyl acetate economy ratio etc.
When 0.5, then trichloro-cane-6-ethyl ester content is less than 5g/L in aqueous phase B 6 '；
Ethyl ester phase B1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid Bs, mother liquor Bs '；
Three, single batch of liquid to be extracted of the 3rd series extraction, referred to as C series, specific practice are as follows:
It takes liquid C0 to be extracted to mix with ethyl ester phase B2, shakes stratification, an isolated ethyl ester phase C1 i.e. light liquid, water phase
A C1 ' i.e. heavy-fluid, wherein extract liquor C0 volume is equal with extract liquor A0；
To ethyl ester phase B3 mixing is added in water phase C1 ', stratification, isolated ethyl ester phase C2, that is, secondary light liquid, water phase are shaken
The i.e. secondary heavy-fluid of C2 '；
To ethyl ester phase B4 mixing is added in water phase C2 ', stratification is shaken, isolated ethyl ester phase C3 i.e. light liquid three times, water phase
C3 ' i.e. heavy-fluid three times；
To ethyl acetate is added in water phase C3 ', stratification is shaken, isolated ethyl ester phase C4 i.e. four light liquids, water phase C4 ' is i.e.
Four heavy-fluids, wherein the volume ratio of ethyl acetate and extract liquor C0 are between 0.5 to 1.0；
Detect water phase C4 ' in trichloro-cane-6-ethyl ester content be less than 5g/L, if it is greater than 5g/L, then repeat above step into
The experiment of row C5, C6, obtain water phase C5 ' and water phase C6 ', and the trichloro-cane-6-ethyl ester in water phase C6 ' is both less than 5g/L；
When the volume ratio of ethyl acetate and extract liquor C0 be 1 i.e. ethyl acetate economy ratio is equal to 1 when, then trichlorine sugarcane in water phase C4 '
Sugar -6- ethyl ester content is less than 5g/L；When the volume ratio of ethyl acetate and extract liquor C0 is that 0.5 i.e. ethyl acetate economy ratio is equal to
When 0.5, then trichloro-cane-6-ethyl ester content is less than 5g/L in water phase C6 '；
Ethyl ester phase C1 is placed in 5 DEG C or less environment and stands crystallization in 8 to 12 hours, suction filtration obtains trichloro-cane-6-ethyl ester crystallization
Solid Cs, mother solution C s '；
It loops back and forth like this, it is subsequent to have D series, E series.
2. improved separation trichloro-cane-6-ethyl ester method according to claim 1, it is characterized in that: the single series of extraction
In extraction process, extraction times are 4 to 6 times, and the content of trichloro-cane-6-ethyl ester is less than 5g/L, acetic acid in last time water phase
Ethyl ester or ethyl acetate phase and the volume ratio of liquid to be extracted be between 0.5 to 1, i.e., ethyl acetate economy ratio be 0.5 to 1 it
Between.
3. improved separation trichloro-cane-6-ethyl ester method according to claim 1, it is characterized in that: by each series
First ethyl ester phase decrease temperature crystalline, suction filtration obtain trichloro-cane-6-ethyl ester primary crystal.
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| CN112457356A (en) * | 2020-11-30 | 2021-03-09 | 安徽金禾实业股份有限公司 | Method for removing ethyl ester from secondary esterified crude product in sucralose production |
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