CN106366060A - Pharmaceutical-grade sodium dehydroacetate purification method - Google Patents
Pharmaceutical-grade sodium dehydroacetate purification method Download PDFInfo
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- CN106366060A CN106366060A CN201610743474.4A CN201610743474A CN106366060A CN 106366060 A CN106366060 A CN 106366060A CN 201610743474 A CN201610743474 A CN 201610743474A CN 106366060 A CN106366060 A CN 106366060A
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- acid sodium
- dehydroactic acid
- crude product
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- purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
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Abstract
The invention discloses a pharmaceutical-grade sodium dehydroacetate purification method in the technical field of chemical purification. The pharmaceutical-grade sodium dehydroacetate purification method mainly comprises the processes of raw material selection, steam stripping, cooling, filtration, dehydration and drying and comprises the process steps that S1, a prepared sodium dehydroacetate crude product is extracted; S2, saturated steam is input into the sodium dehydroacetate crude product for steam stripping; S3, the v mixed steam is led to condensed water; S4, impurities in raw materials are filtered out through a filtering screen plate; S5, the filtered sodium dehydroacetate crude product is put in a centrifugal machine; S6, the sodium dehydroacetate crude product is delivered to a drying device, low-temperature cooling and separation are adopted, the purification precision is high, the purification method is easy to control and suitable for ensuring of the pharmaceutical-grade sodium dehydroacetate purity and large-scale production and usage, and the device and cost investment is reduced.
Description
Technical field
The present invention relates to technical field of chemical purification, specially a kind of pharmaceutical grade dehydroactic acid sodium method of purification.
Background technology
Dehydroactic acid sodium is white or near-white crystalline powder, nontoxic, odorless.Readily soluble what water, glycerol, propylene glycol, micro-
It is dissolved in ethanol and acetone.Its aqueous solution does not change at 120 DEG C, in 120 DEG C of heating still keep within 2 hours stable be in neutral or
Alkalescence.Fast light, heat-resist, can be used as preservative, anticorrosive insecticide, food additive.
Present commercial production is typically purified to product using distillation under pressure point method, but due to dehydroactic acid sodium
Freezing point is higher, easily blocks pipeline in process of production, in order to overcome this difficult, some employing organic solvent recrystallization
Method is purified, but can bring organic solute impurity into in dehydroactic acid sodium product, and the use being extremely difficult to pharmaceutical grade will
Ask, for this reason, we have invented a kind of pharmaceutical grade dehydroactic acid sodium method of purification coming into operation to solve the above problems.
Content of the invention
It is an object of the invention to provide a kind of pharmaceutical grade dehydroactic acid sodium method of purification, to solve in above-mentioned background technology
Pipeline and the problem of pollution dehydroactic acid sodium product can be blocked in the conventional dehydrogenation sodium acetate purification process proposing.
For achieving the above object, the present invention provides a kind of following technical scheme: pharmaceutical grade dehydroactic acid sodium method of purification, main
Material choice to be included, stripping, cooling, filtration, dehydration, drying process, described pharmaceutical grade dehydroactic acid sodium method of purification, its work
Skill step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is between 75%-78%, standby；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 0 DEG C
12 DEG C, cool time is 15 35min；
S4: filter: its internal impurity is filtered by the raw material after cooling down in step s4 by filtering sieve plate；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 5000 8000r/min, and dewatering time is 30 50min；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 2 4.5h, and baking temperature is 75 DEG C 95 DEG C.
Preferably, in described step s1, using vibrosieve, primary filter, wherein sieves are carried out to dehydroactic acid sodium crude product
Pore size filter 100 120 mesh, continuous working period 12 18min.
Preferably, in described step s3, between 100 DEG C 115 DEG C, stripping time is 20 to stripping temperature control
40min.
Preferably, in described step s4, condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.5 1.2mpa.
Preferably, in described step s5, sieves intralaminar part is provided with three layer filtration net, and the pore size filter of three layer filtration net
Reduce successively in 0.2 times.
Preferably, in described step s7, dried dehydroactic acid sodium aqueous powder is 5.5 8.5wt%.
Preferably, the white powder of sterling dehydroactic acid sodium that described step s7 draws after being dried, its purity is 97
99.2%.
Compared with prior art, the invention has the beneficial effects as follows: dehydroactic acid sodium distils when 109 DEG C, in saturated vapor
In the presence of, the partial pressure of dehydroactic acid sodium reduces, and therefore the sublimation point of dehydroactic acid sodium reduces, and is easier to rise in saturated vapor
China, and its sublimation point of heteropolymer impurity such as the dimerization in dehydroactic acid sodium, trimerization, fusing point are higher, will not be with saturated vapor
It is carried over, using sub-cooled and separation, purify high precision it is easy to control its purification to be applied to the dehydroactic acid sodium essence of pharmaceutical grade
Degree, reduces equipment and cost investment, suitable use of large-scale production.
Brief description
Fig. 1 is present invention process flow chart.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
Embodiment one
A kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, does
Drying process, described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is between 75%-78%, standby, carries out primary filter using vibrosieve to dehydroactic acid sodium crude product, wherein filters
Sieve pore size filter 100 120 mesh, continuous working period 12 18min；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped, and between 100 DEG C 115 DEG C, stripping time is 20 40min to stripping temperature control；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 0 DEG C
12 DEG C, cool time is 15 35min, and condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.5 1.2mpa；
S4: filter: its internal impurity is filtered by filtering sieve plate by the raw material after cooling down in step s4, filters in sieve plate
Portion is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 5000 8000r/min, and dewatering time is 30 50min, dried dehydroactic acid sodium powder
Last moisture is 5.5 8.5wt%, the white powder of sterling dehydroactic acid sodium, and its purity is 97 99.2%；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 2 4.5h, and baking temperature is 75 DEG C 95 DEG C.
Embodiment two
A kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, does
Drying process, described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is 75%, standby, using vibrosieve, dehydroactic acid sodium crude product is carried out with primary filter, wherein sieves pore size filter
100 mesh, continuous working period 12min；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped, and between 100 DEG C, stripping time is 20min to stripping temperature control；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 0 DEG C, cold
But the time is 15min, and condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.5mpa；
S4: filter: its internal impurity is filtered by filtering sieve plate by the raw material after cooling down in step s4, filters in sieve plate
Portion is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 5000r/min, and dewatering time is 30min, and dried dehydroactic acid sodium aqueous powder is
5.5wt%, the white powder of sterling dehydroactic acid sodium, its purity is 97%；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 2h, and baking temperature is 75 DEG C.
Embodiment three
A kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, does
Drying process, described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is 76%, standby, using vibrosieve, dehydroactic acid sodium crude product is carried out with primary filter, wherein sieves pore size filter
105 mesh, continuous working period 14min；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped, and between 105 DEG C, stripping time is 28min to stripping temperature control；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 4 DEG C, cold
But the time is 20min, and condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.7mpa；
S4: filter: its internal impurity is filtered by filtering sieve plate by the raw material after cooling down in step s4, filters in sieve plate
Portion is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 6000r/min, and dewatering time is 35min, and dried dehydroactic acid sodium aqueous powder is
6wt%, the white powder of sterling dehydroactic acid sodium, its purity is 97.9%；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 3h, and baking temperature is 80 DEG C.
Example IV
A kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, does
Drying process, described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is 78%, standby, using vibrosieve, dehydroactic acid sodium crude product is carried out with primary filter, wherein sieves pore size filter
120 mesh, continuous working period 18min；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped, and between 115 DEG C, stripping time is 40min to stripping temperature control；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 12 DEG C,
Cool time is 35min, and condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 1.2mpa；
S4: filter: its internal impurity is filtered by filtering sieve plate by the raw material after cooling down in step s4, filters in sieve plate
Portion is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 8000r/min, and dewatering time is 50min, and dried dehydroactic acid sodium aqueous powder is
8.5wt%, the white powder of sterling dehydroactic acid sodium, its purity is 98.2%；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 4.5h, and baking temperature is 95 DEG C.
Described in comprehensive above example, a kind of optimal enforcement of pharmaceutical grade dehydroactic acid sodium method of purification that the present invention provides
Example is: a kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, back tender
Sequence, described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, tentatively filtered its internal impurity so as to
Crude product purity is 77%, standby, using vibrosieve, dehydroactic acid sodium crude product is carried out with primary filter, wherein sieves pore size filter
110 mesh, continuous working period 16min；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturation
Steam steams, and is stripped, and between 110 DEG C, stripping time is 35min to stripping temperature control；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 8 DEG C, cold
But the time is 25min, and condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.9mpa；
S4: filter: its internal impurity is filtered by filtering sieve plate by the raw material after cooling down in step s4, filters in sieve plate
Portion is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is taken off using centrifugal force
Water, wherein, centrifuge speed is 7000r/min, and dewatering time is 45min, and dried dehydroactic acid sodium aqueous powder is
7.5wt%, the white powder of sterling dehydroactic acid sodium, its purity is 99.2%；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying
Time is 3.5h, and baking temperature is 85 DEG C.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and can carry out multiple changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (7)
1. a kind of pharmaceutical grade dehydroactic acid sodium method of purification, mainly includes material choice, stripping, cooling, filtration, dehydration, is dried
Operation it is characterised in that: described pharmaceutical grade dehydroactic acid sodium method of purification, its processing step is:
S1: material choice: the dehydroactic acid sodium prepared crude product is extracted, is tentatively filtered its internal impurity so as to crude product
Purity is between 75%-78%, standby；
S2: stripping: saturated vapor is inputted inside dehydroactic acid sodium crude product by pipeline, dehydroactic acid sodium crude product is with saturated vapor
Steam, stripped；
S3: cooling: the dehydroactic acid sodium mixed vapour in step s3 is passed through in condensed water, condensate temperature is 0 DEG C 12 DEG C,
Cool time is 15 35min；
S4: filter: its internal impurity is filtered by the raw material after cooling down in step s4 by filtering sieve plate；
S5: dehydration: the dehydroactic acid sodium crude product after filtering in step s5 is put in centrifuge, is dehydrated using centrifugal force,
Wherein, centrifuge speed is 5000 8000r/min, and dewatering time is 30 50min；
S6: be dried: the dehydroactic acid sodium crude product after the completion of being dehydrated in step s6 is conveyed in drying equipment, controls drying time
For 2 4.5h, baking temperature is 75 DEG C 95 DEG C.
2. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s1
In, using vibrosieve, dehydroactic acid sodium crude product is carried out with primary filter, wherein sieves pore size filter 100 120 mesh, continue work
Make time 12 18min.
3. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s3
In, between 100 DEG C 115 DEG C, stripping time is 20 40min to stripping temperature control.
4. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s4
In, condensed water is stored in double-layer stainless steel drainer, its pressure-bearing 0.5 1.2mpa.
5. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s5
In, sieves intralaminar part is provided with three layer filtration net, and the pore size filter of three layer filtration net reduces successively in 0.2 times.
6. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s7
In, dried dehydroactic acid sodium aqueous powder is 5.5 8.5wt%.
7. a kind of pharmaceutical grade dehydroactic acid sodium method of purification according to claim 1 it is characterised in that: described step s7 do
The white powder of sterling dehydroactic acid sodium drawing after dry, its purity is 97 99.2%.
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| CN201610743474.4A CN106366060A (en) | 2016-08-26 | 2016-08-26 | Pharmaceutical-grade sodium dehydroacetate purification method |
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| CN201610743474.4A CN106366060A (en) | 2016-08-26 | 2016-08-26 | Pharmaceutical-grade sodium dehydroacetate purification method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475550A (en) * | 2009-01-13 | 2009-07-08 | 南通奥凯生物技术开发有限公司 | Preparation of high purity sodium dehydroacetate |
| CN102219770A (en) * | 2011-04-27 | 2011-10-19 | 南通奥凯生物技术开发有限公司 | Method for manufacturing high purity sodium dehydroacetate through membrane filtration |
| CN105384714A (en) * | 2015-12-18 | 2016-03-09 | 南京工业大学 | Decolorization and purification technology for sodium dehydroacetate |
-
2016
- 2016-08-26 CN CN201610743474.4A patent/CN106366060A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475550A (en) * | 2009-01-13 | 2009-07-08 | 南通奥凯生物技术开发有限公司 | Preparation of high purity sodium dehydroacetate |
| CN102219770A (en) * | 2011-04-27 | 2011-10-19 | 南通奥凯生物技术开发有限公司 | Method for manufacturing high purity sodium dehydroacetate through membrane filtration |
| CN105384714A (en) * | 2015-12-18 | 2016-03-09 | 南京工业大学 | Decolorization and purification technology for sodium dehydroacetate |
Non-Patent Citations (3)
| Title |
|---|
| M. ISHIDATE JR ET AL.: ""Primary mutagenicity screening of food additives currently used in Japan"", 《FD CHEM. TOXIC.》 * |
| 李星: ""脱氢乙酸合成条件的优化及提纯方法的改进"", 《中国优秀博硕士学位论文全文数据库 (硕士) 工程科技Ⅰ辑》 * |
| 郝利平: "《食品添加剂》", 31 July 2013, 中国农业出版社 * |
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