CN106946695A - The method for purifying sorbic acid - Google Patents
The method for purifying sorbic acid Download PDFInfo
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- CN106946695A CN106946695A CN201710175935.7A CN201710175935A CN106946695A CN 106946695 A CN106946695 A CN 106946695A CN 201710175935 A CN201710175935 A CN 201710175935A CN 106946695 A CN106946695 A CN 106946695A
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- sorbic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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Abstract
The invention discloses the production technology for the sorbic acid that high-purity is prepared using fusion-crystallization, it comprises the following steps：First chilled brine is passed through in melting crystallizer external jacket bottom, chilled brine is in uniformly film evaporation device in crystallizer outer wall, then thick sorbic acid solutions are put into melting crystallizer, sorbic acid solutions are under crystallizer inwall falling liquid film stream, progressively cool down and crystallize, uniform crystal layer is progressively grown on heat-transfer surface, the concentration of crystal layer is higher than the concentration of mixture solution, and impurity is progressively enriched in mixture solution；Then hot water temperature is adjusted to crystal layer progress part melt operation by heat exchanger, melts the low-melting impurities part being mingled with crystal layer and exclude, further to purify crystal.Method of the present invention technique is simple, compact equipment, using falling liquid film form, energy is reduced, while reducing cost and equipment investment；The product purity produced using the melting crystallizer is high.
Description
Technical field
The present invention relates to the method that the method for purification of sorbic acid, especially melting crystallizer purify sorbic acid.
Background technology
Sorbic acid and its sylvite can suppress fungus growth, come to be used as food preservative for a long time, especially in low ph value, can make
Antisepsis is played for non-dissociated acid.Sorbic acid has the unexistent feature of other preservatives, that is, has very strong anti-corrosion selectivity,
It can suppress the growth to human hazard bacterium, and then harmless to the bacterium for being beneficial to people, and for example it can suppress fill cheese moulds life
Growth that is long but having no effect on the bacterium for helping cheese curing.Therefore sorbic acid is largely used as cheese, cake in the food industry
With the preservative of other cakes.It is mainly used in cheese, pickless, dries fruit, fruit juice, fruit sugar syrups, beverage, preserved fruit, face
Bag, candy etc. it is mould proof.It is also used for the fresh-keeping of flesh of fish product.It is also applied in terms of cosmetics, medicine, feed.At present both at home and abroad
The equipment of large-scale production sorbic acid is general enamel reaction still, the process of its maturation process approximately as：Take ketenes
With crotonaldehyde in the presence of catalyst, occur condensation reaction, then the process acquisition finished product such as hydrolyze, dry, packing, yet with
The sorbic acid outward appearance that the technique productions go out is very secondary, and impurity is more, irritant smell.Therefore the technique of existing this sorbic acid and set
Have to be modified.
The content of the invention
The technical problem to be solved in the present invention is to provide the method that melting crystallizer purifies sorbic acid, it has good put down
Row reaction selectivity and security, reduce cost and equipment investment；It is environmentally friendly, less energy consumption, and sorbic acid product purity
High, stay in grade.
In order to solve the above technical problems, the technical solution adopted by the present invention is：The method for purifying sorbic acid, its innovative point exists
In：Sorbic acid is purified using melting crystallizer, concretely comprised the following steps：
(1) crystallize：Chilled brine is passed through in melting crystallizer external jacket bottom, chilled brine is uniformly in melting crystallizer
Outer wall is in film evaporation device, thick sorbic acid solutions is put into melting crystallizer, thick sorbic acid solutions are in melting crystallizer inwall
Falling liquid film is flowed down, and is progressively cooled down and is crystallized, and uniform crystal layer is progressively grown on heat-transfer surface, the concentration of crystal layer is higher than melting
The concentration of solution in crystallizer, impurity is progressively enriched in solution；
(2) sweating, fusing：Chilled brine is passed through after 12~30minmin, stops feed, then adjusts heat by heat exchanger
Coolant-temperature gage carries out part fusing to crystal layer, melts the low-melting impurities being mingled with crystal layer and excludes, further purifies crystal.
The present invention realizes material separation and purification using melting crystallizer using the difference of freezing point between separate substance,
Mass transfer is controlled by the transmission for adjusting energy, so as to reach the effect for the purity for improving crystalline rate and crystal product；Improve
Parallel reaction selectivity；The system of unsafe factor such as can set off an explosion for the recrystallization using solvent, burn, and pass through melting
Crystallizer control input, maintains the optium concentration of crystallization, and low-temperature operation can improve security of system；In crystallizer upper airway
Appropriate compressed air is passed through, solution is formed the rising of slug flow bubble in crystallizer, causes the turbulence of melt, mass transfer enhancement
And heat transfer property.
Further, the crystallisation step is specially：First chilled brine, temperature are passed through in melting crystallizer external jacket bottom
For -10 DEG C~-2 DEG C, chilled brine is in uniformly film evaporation device in melting crystallizer outer wall, then puts into thick sorbic acid solutions
Into melting crystallizer, while by melting crystallizer wireway with 4~7m3/ min speed is passed through into thick sorbic acid solutions
Compressed air, is allowed to form the rising of slug flow bubble in crystallizer, causes the turbulence of melt, mass transfer enhancement and heat transfer property,
Sorbic acid solutions are progressively cooled down and crystallized under melting crystallizer inwall falling liquid film stream, are progressively grown on heat-transfer surface uniform
Crystal layer, concentration of the concentration higher than solution in melting crystallizer of crystal layer, impurity is progressively enriched in solution.
Further, the sweating, fusing step are specially：Control chilled brine is passed through after time 12-30min, is stopped
Feed, switching warm water tank carries out part fusing to crystal layer, and water temperature is 88~92 DEG C, and warm water is passed through the time for 15~40min；So
Switching hot-water cylinder water temperature, which is 90~94 DEG C, afterwards makes the low-melting impurities being mingled with crystal layer melt exclusion, further purifies crystal,
Hot water is passed through the time for 25~35min.
Further, the chilled brine is calcium chloride solution or sodium chloride solution.
Further, the melting crystallizer is the falling film melt crystallization device of vertical array tubular heat exchanger type.
Compared with prior art, the advantage of the invention is that：The technique letter of sorbic acid is purified by above-mentioned melting crystallizer
Single, it has good parallel reaction selectivity and security, using falling liquid film form and low-temperature operation, the energy of specific yield product
Amount consumption is greatly lowered, and has preferable economy, while the technical process crystal is in heating surface formation crystal layer, without
It is suspended in liquid, this avoid the blocking of equipment and pipeline, reduces the generation of fault in production, reduces cost and set
Standby investment；Almost do not have in production process " three wastes ", it is environmentally friendly, compared with the recrystallization using solvent, it is not necessary to dry
With desolvation, energy consumption is only the 10%~30% of rectifying, and the sorbic acid product purity produced using the melting crystallizer
High, stay in grade, increase operation series can be such that purity infinitely improves, and can make in product impurity content from percentage composition to ppm
Content, so as to overcome deficiency of the prior art.
Embodiment
Technical scheme is elaborated with reference to specific embodiment.
Embodiment 1
Melting crystallizer purifies the technique of sorbic acid, comprises the following steps：
(1) crystallize：- 8 DEG C of calcium chloride solution first is passed through in melting crystallizer external jacket bottom, calcium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the sorbic acid solutions being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer wireway is crossed using compressor with 4m3The compressed air that/min speed is passed through into sorbic acid solutions, is allowed to
Slug flow bubble is formed in crystallizer to rise, and causes the turbulence of melt, mass transfer enhancement and heat transfer property, sorbic acid solutions are in knot
Brilliant device inwall falling liquid film is flowed down, and is progressively cooled down and is crystallized, uniform crystal layer, the concentration of crystal layer are progressively grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is progressively enriched in solution；
(2) sweating, fusing：Control calcium chloride solution is passed through after time 30min, stops feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 88 DEG C, and warm water is passed through the time for 15min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with is excluded, and further purifies crystal, and hot-water cylinder water temperature is 88 DEG C, and hot water is passed through the time for 28min,
The purity for obtaining sorbic acid is 99.91%.
Embodiment 2
Melting crystallizer purifies the technique of sorbic acid, comprises the following steps：
(1) crystallize：- 6 DEG C of sodium chloride solution first is passed through in melting crystallizer external jacket bottom, sodium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the sorbic acid solutions being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer wireway is crossed using compressor with 5m3The compressed air that/min speed is passed through into sorbic acid solutions, is allowed to
Slug flow bubble is formed in crystallizer to rise, and causes the turbulence of melt, mass transfer enhancement and heat transfer property, sorbic acid solutions are in knot
Brilliant device inwall falling liquid film is flowed down, and is progressively cooled down and is crystallized, uniform crystal layer, the concentration of crystal layer are progressively grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is progressively enriched in solution；
(2) sweating, fusing：Control sodium chloride solution is passed through after time 15min, stops feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 90 DEG C, and warm water is passed through the time for 30min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with is excluded, and further purifies crystal, and hot-water cylinder water temperature is 92 DEG C, and hot water is passed through the time for 30min,
The purity for obtaining sorbic acid is 99.92%.
Embodiment 3
Melting crystallizer purifies the technique of sorbic acid, comprises the following steps：
(1) crystallize：- 2 DEG C of calcium chloride solution first is passed through in melting crystallizer external jacket bottom, calcium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the sorbic acid solutions being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer wireway is crossed using compressor with 7m3The compressed air that/min speed is passed through into sorbic acid solutions, is allowed to
Slug flow bubble is formed in crystallizer to rise, and causes the turbulence of melt, mass transfer enhancement and heat transfer property, sorbic acid solutions are in knot
Brilliant device inwall falling liquid film is flowed down, and is progressively cooled down and is crystallized, uniform crystal layer, the concentration of crystal layer are progressively grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is progressively enriched in solution；
(2) sweating, fusing：Control calcium chloride solution is passed through after time 33min, stops feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 92 DEG C, and warm water is passed through the time for 40min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with is excluded, and further purifies crystal, and hot-water cylinder water temperature is 94 DEG C, and hot water is passed through the time for 32min,
The purity for obtaining sorbic acid is 99.91%.
After the falling film melt crystallization device similar to vertical array tubular heat exchanger, the crystallization process of sorbic acid becomes more
It is easily controlled, impurity is few, the purity of finished product is higher, typically can reach more than 99.8%, outward appearance is whiter and bright, crystal is good.Pass through
There is no or greatly reduce the presence of impurity in the improvement of the technique, sorbic acid finished product, effectively raise its antiseptic property,
The consumption of preservative in food is reduced, food security is effectively raised.
Comparative example 1
(1) sorbic acid solutions being condensed are got in crystallization kettle, it is cold to lead to cooling water (20~25 DEG C) toward crystallization kettle chuck
When but to 50~60 DEG C, then pre-cooling cycle valve is closed, stop cooling, add 1kg sorbic acid calomel mercurous chloride crystal seed；
(2) cooling water is about opened after 40min, continues to cool, cooling is stopped to 38~42 DEG C, cross and freezing is opened after 20min
(5~7 DEG C) of water continues to cool, and stops chilled water when 18~20 DEG C, prepares blowing, and centrifugal dehydration obtains the purity of sorbic acid
For 99.82%.
It is pointed out that the technical concept and feature of above-mentioned preferred embodiment only to illustrate the invention, its object is to
Person skilled in the art can understand present disclosure and implement according to this, the protection of the present invention can not be limited with this
Scope.Any equivalent change or modification in accordance with the spirit of the invention, should all be included within the scope of the present invention.
Claims (5)
1. purify the method for sorbic acid, it is characterised in that：Sorbic acid is purified using melting crystallizer, concretely comprised the following steps：
(1) crystallisation step：Chilled brine is passed through in melting crystallizer external jacket bottom, chilled brine is uniformly in melting crystallizer
Outer wall is in film evaporation device, thick sorbic acid solutions is put into melting crystallizer, thick sorbic acid solutions are in melting crystallizer inwall
Falling liquid film is flowed down, and is progressively cooled down and is crystallized, and uniform crystal layer is progressively grown on heat-transfer surface, the concentration of crystal layer is higher than melting
The concentration of solution in crystallizer, impurity is progressively enriched in solution；
(2) sweating, fusing：Chilled brine is passed through after 12~30min, is stopped feed, is then adjusted hot water temperature by heat exchanger
Part fusing is carried out to crystal layer, the low-melting impurities being mingled with crystal layer is melted and excludes, further purify crystal.
2. the method for sorbic acid is purified according to claim 1, it is characterised in that：The crystallisation step is specially：First molten
Melt crystallizer external jacket bottom and be passed through chilled brine, temperature is -10 DEG C~-2 DEG C, and chilled brine is uniformly outside melting crystallizer
Wall is in film evaporation device, is then put into thick sorbic acid solutions in melting crystallizer, while by melting crystallizer wireway with 4
~7m3/ min speed is passed through compressed air into thick sorbic acid solutions, is allowed to form the rising of slug flow bubble in crystallizer,
The turbulence of melt, mass transfer enhancement and heat transfer property are caused, sorbic acid solutions are progressively cooled down under melting crystallizer inwall falling liquid film stream
And crystallize, progressively grow uniform crystal layer on heat-transfer surface, the concentration of crystal layer higher than in melting crystallizer solution it is dense
Degree, impurity is progressively enriched in solution.
3. the method for sorbic acid is purified according to claim 1, it is characterised in that：The sweating, fusing are specially：Control is cold
Freeze salt solution to be passed through after 12~30min of time, stop feed, switching warm water tank carries out part fusing, warm water tank water temperature to crystal layer
For 88~92 DEG C, warm water is passed through the time for 15~40min；Then switching hot-water cylinder melts the low-melting impurities being mingled with crystal layer
Change and exclude, further purify crystal, hot-water cylinder water temperature is 90~94 DEG C, and hot water is passed through the time for 25~35min.
4. the method for purification sorbic acid according to claim 1 or claim 2, it is characterised in that：The chilled brine is that calcium chloride is molten
Liquid or sodium chloride solution.
5. the method for purification sorbic acid according to claim 1 or claim 2, it is characterised in that：The melting crystallizer is vertical row
The falling film melt crystallization device of heat exchange of heat pipe formula.
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| CN201710175935.7A CN106946695A (en) | 2017-03-23 | 2017-03-23 | The method for purifying sorbic acid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694105A (en) * | 2014-01-13 | 2014-04-02 | 南通奥凯生物技术开发有限公司 | Method for purifying sorbic acid |
| CN105198727A (en) * | 2015-09-08 | 2015-12-30 | 张勇 | Method of purifying sorbic acid |
| CN105949050A (en) * | 2016-07-13 | 2016-09-21 | 南通中兴多元复合钢管有限公司 | Method for purifying sorbic acid |
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2017
- 2017-03-23 CN CN201710175935.7A patent/CN106946695A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694105A (en) * | 2014-01-13 | 2014-04-02 | 南通奥凯生物技术开发有限公司 | Method for purifying sorbic acid |
| CN105198727A (en) * | 2015-09-08 | 2015-12-30 | 张勇 | Method of purifying sorbic acid |
| CN105949050A (en) * | 2016-07-13 | 2016-09-21 | 南通中兴多元复合钢管有限公司 | Method for purifying sorbic acid |
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