CN110372485A - A kind of recycling ice solution processing method suitable for alpha, beta-lonone production process - Google Patents
A kind of recycling ice solution processing method suitable for alpha, beta-lonone production process Download PDFInfo
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- CN110372485A CN110372485A CN201910656375.6A CN201910656375A CN110372485A CN 110372485 A CN110372485 A CN 110372485A CN 201910656375 A CN201910656375 A CN 201910656375A CN 110372485 A CN110372485 A CN 110372485A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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Abstract
The present invention relates to a kind of recycling ice solution processing methods suitable for alpha, beta-lonone production process, this method specifically: the extraction of ice solution is carried out to the alpha, beta-lonone mixed liquor after cyclization using ice water liquid, separate the organic phase and water phase of the alpha, beta-lonone containing high concentration, recovery section water phase and to supplement ice water liquid constant to the water for being used for the extraction of ice solution, repeats the above ice solution to the alpha, beta-lonone mixed liquor of ice solution non-after cyclization and operates.Compared with prior art, the present invention drastically reduces the use of ice water liquid, increase the content of sulfuric acid in ice solution liquid, reach the concentration of production chemical fertilizer calcium superphosphate sulfuric acid, also slightly increase the yield of product, both it had saved the energy and the time is used in production, and in turn avoided the problem of environmental pollution of acid pickle.
Description
Technical field
The present invention relates to chemical fields, more particularly, to a kind of recycling ice solution suitable for alpha, beta-lonone production process
Processing method.
Background technique
Prepare after alpha, beta-lonone cyclization at present ice solution liquid in ice solution preocess have it is several:
1. 15% or so salt is added hypothermic saline, in water, temperature is cooled on -10 DEG C of left sides by reacting kettle jacketing
It is right.
2. water is cooled to 0 DEG C by reacting kettle jacketing, adds the broken of water one third or so by ice water mixed liquor
Ice.
Alpha, beta-lonone can generate a large amount of low acid concentration waste water (sulfuric acid concentration about 20%), ring in cyclization ice solution preocess
To use a large amount of alkali and other industrial chemicals, cost very high in guarantor's processing；Consumption is big again in the refrigerating process of ice solution liquid preparation
The energy of amount.
Patent CN106278853A discloses macro work technology and continuously synthesizes alpha, beta-lonone applied to pseudo ionone
Method.This method comprises: by the diluted pseudoionone of solvent and the concentrated sulfuric acid continually by one integrate micro- reaction with it is micro-
It exchanges heat in the microreactor 1 of one, is reacted and exchanged heat in microreactor channel and generate alpha, beta-lonone product；Contain
The microemulsion of alpha, beta-lonone product passes through one and integrates micro- reaction with micro- heat exchange in the microreactor 2 of one, micro- anti-at this
It answers in device and dilutes microemulsion to enter the ice water of concentrated sulfuric acid certain volume ratio in microreactor 1 compared to microemulsion, quenching reaction,
The mixture containing alpha, beta-lonone product is obtained, the extraction and separation mixture obtains alpha, beta-lonone product.This method is only adopted
It is diluted with an ice water, cannot achieve the discharge of low concentration acid, and product yield is not high.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems and it is a kind of suitable for alpha, beta-lonone production process to provide
Recycling ice solution processing method, drastically reduces the use of ice water, increases the content of sulfuric acid in ice solution liquid, reaches productionization
The concentration of fertile calcium superphosphate sulfuric acid, also slightly increases the yield of product, has both saved the energy and production time, in turn avoid
The problem of environmental pollution of acid pickle.
The purpose of the present invention is achieved through the following technical solutions:
A kind of recycling ice solution processing method suitable for alpha, beta-lonone production process, this method specifically: use ice
Aqueous carries out the extraction of ice solution to the alpha, beta-lonone mixed liquor after cyclization, separates the organic phase and water of the alpha, beta-lonone containing high concentration
Phase, recovery section water phase and supplement ice water liquid to be used for ice solution extraction water it is constant, to β-violet of ice solution non-after cyclization
Ketone mixed liquor repeats the above ice solution extraction and separation operation.
Preferably, the method specifically includes the following steps:
(a) water for accounting for ice solution autoclave body product 20-60% is added in ice solution kettle, is cooled to -5~5 DEG C, sequentially adding volume is
The trash ice and volume of water 1/4-1/2 is the petroleum ether of water 2-8%, obtains the ice water liquid for ice solution；
(b) volume is added in the ice water liquid for using step (a) to prepare as β-violet after ice water liquid 1/3-1/5 cyclization
Ketone mixed liquor is stirred ice solution, forms organic phase and water phase and separates；
(c) petroleum ether that volume is water 2-8% is added in the water phase that step (b) obtains to be extracted, will extract
To the organic phase of the alpha, beta-lonone containing high concentration merge with the organic phase that step (b) obtains, recycling 60-90% volume content
Water phase extracted into ice solution kettle, and supplement water or trash ice to be used for ice solution extraction water it is constant, repeat above step.
Preferably, the water being added in step (a) is the 40% of ice solution autoclave body product, is easy to be stirred, can make β-violet
Ketone mixed liquor comes into full contact with ice water liquid, and ice solution is more thorough.
Preferably, water is added in ice solution kettle in step (a), is cooled to 0 DEG C, ice and water can coexist at a temperature of this, can make
Ice water liquid plays better ice Xie Zuoyong.
Preferably, in step (a), trash ice additional amount is the 1/3 of water, and excessive trash ice can make liquid flowing uneven,
Very few trash ice can make ice solution effect not significant.
Preferably, in step (a) and step (c), petroleum ether additional amount is the 5% of water, and petroleum ether appropriate can promote
Into the progress of ice solution, and the significant effect of petroleum ether extraction alpha, beta-lonone.
Preferably, in step (b), the alpha, beta-lonone mixeding liquid volume after cyclization is the 1/4 of ice water liquid, the volume ratio
Under, the ice solution effect of alpha, beta-lonone is best.
Preferably, in step (c), petroleum ether repeats to extract twice, and repeatedly extraction is conducive to improve alpha, beta-lonone
Yield.
Preferably, in step (c), the amount for recycling water phase accounts for the 70% of water phase volume extracted, by experiment, in the body
Under long-pending recycle-water phasor, guarantee the purity of alpha, beta-lonone, and after multi-reflow, the yield of product is considerable.
In ice solution preocess, the concentrated sulfuric acid is diluted, and releases big calorimetric, and alpha, beta-lonone is in higher temperature and larger acidity
When can generate can not α against distortion, therefore to keep low temperature.The too small meeting of ice water additive amount is so that temperature is too high when ice solution, ice water addition
Amount too it is big not only can waste of energy, excessively dilute acid solution processing cost is too high.
Compared with prior art, the invention has the following advantages: carrying out the ice solution of alpha, beta-lonone using ice water liquid,
And recovery section water phase is reused, and the use of ice water is drastically reduced, and is increased the content of sulfuric acid in ice solution liquid, is reached
To the concentration of production chemical fertilizer calcium superphosphate sulfuric acid, the yield of product is also slightly increased, the environment in turn avoiding acid pickle is dirty
Dye problem, is conducive to eliminate the discharge of low concentration acid using the extraction that petroleum ether carries out water phase later, and energy saving and production is used
Time.
Specific embodiment
The present invention is described in detail combined with specific embodiments below, but should be in no way restrictive.
In following embodiment, raw material or processing technique unless otherwise instructed, then show be this field conventional city
Sell raw produce or routine techniques.
Embodiment 1
A kind of recycling ice solution processing method suitable for alpha, beta-lonone production process, specifically includes the following steps:
(a) water for accounting for ice solution autoclave body product 40% is added in ice solution kettle, is cooled to 0 DEG C or so, addition accounts for ice water amount three and divides
One of left and right trash ice, add 5% or so petroleum ether of water, obtain the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/4 is added in ice water liquid is stirred ice
Solution forms organic phase and water phase and separates；
(c) it is added in the water phase that step (b) obtains and is same as above 5% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 40% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 60%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 5% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 40% acid pickle.It repeats according to this below.
Obtained alpha, beta-lonone meter purity, yield, waste sulfuric acid concentration, ice solution electricity consumption and it is cooled to -10 DEG C
Time, see Table 1 for details.
Embodiment 2
A kind of recycling ice solution processing method suitable for alpha, beta-lonone production process, specifically includes the following steps:
(a) water for accounting for ice solution autoclave body product 40% is added in ice solution kettle, is cooled to 0 DEG C or so, addition accounts for ice water amount three and divides
One of left and right trash ice, add 5% or so petroleum ether of water, obtain the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/4 is added in ice water liquid stirs ice solution, shape
At organic phase and water phase and separate；
(c) it is added in the water phase that step (b) obtains and is same as above 5% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 30% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 70%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 5% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 30% acid pickle.It repeats according to this below.
Obtained alpha, beta-lonone meter purity, yield, waste sulfuric acid concentration, ice solution electricity consumption and it is cooled to -10 DEG C
Time, see Table 1 for details.
Embodiment 3
(a) water for accounting for ice solution autoclave body product 40% is added in ice solution kettle, is cooled to 0 DEG C or so, addition accounts for ice water amount three and divides
One of left and right trash ice, add 5% or so petroleum ether of water, obtain the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/4 is added in ice water liquid stirs ice solution, shape
At organic phase and water phase and separate；
(c) it is added in the water phase that step (b) obtains and is same as above 5% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 20% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 80%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 5% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 20% acid pickle.It repeats according to this below.
Obtained alpha, beta-lonone meter purity, yield, waste sulfuric acid concentration, ice solution electricity consumption and it is cooled to -10 DEG C
Time, see Table 1 for details.
Embodiment 4
(a) water for accounting for ice solution autoclave body product 40% is added in ice solution kettle, is cooled to 0 DEG C or so, addition accounts for ice water amount three and divides
One of left and right trash ice, add 5% or so petroleum ether of water, obtain the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/4 is added in ice water liquid stirs ice solution, shape
At organic phase and water phase and separate；
(c) it is added in the water phase that step (b) obtains and is same as above 5% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 10% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 90%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 5% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 10% acid pickle.It repeats according to this below.
Obtained alpha, beta-lonone meter purity, yield, waste sulfuric acid concentration, ice solution electricity consumption and it is cooled to -10 DEG C
Time, see Table 1 for details.
Embodiment 5
(a) water for accounting for ice solution autoclave body product 20% is added in ice solution kettle, is cooled to 5 DEG C or so, it is left that addition accounts for ice water amount 1/2
Right trash ice, adds 8% or so petroleum ether of water, obtains the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/3 is added in ice water liquid stirs ice solution, shape
At organic phase and water phase and separate；
(c) it is added in the water phase that step (b) obtains and is same as above 8% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 10% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 90%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 8% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 10% acid pickle.It repeats according to this below.
Embodiment 6
(a) water for accounting for ice solution autoclave body product 60% is added in ice solution kettle, is cooled to -5 DEG C or so, addition accounts for ice water amount 1/4
The trash ice of left and right, adds 2% or so petroleum ether of water, obtains the ice water liquid for ice solution；
(b) the alpha, beta-lonone mixed liquor after the cyclization that volume is ice water liquid 1/5 is added in ice water liquid stirs ice solution, shape
At organic phase and water phase and separate；
(c) it is added in the water phase that step (b) obtains and is same as above 2% petroleum ether extraction twice, will be obtained by extraction containing highly concentrated
The organic phase of degree alpha, beta-lonone merges with the organic phase that step (b) obtains, and remaining water phase is drawn back after removing 40% acid pickle
Supplement water or rubble ice, weight are equivalent to removal into ice solution kettle, and in ice solution kettle for ice solution kettle, the i.e. water phase of recycling 60%
The weight of acid pickle, mixed liquor stirs ice solution after cyclization is added, and collects organic phase by liquid separation, is added in water phase and is same as above 5% stone
Oily ether is extracted twice, and merges organic phase；Remaining water phase draws back ice solution kettle after removing 40% acid pickle.It repeats according to this below.
Comparative example 1
The water for accounting for ice solution autoclave body product 40% is added in ice solution kettle, is cooled to 0 DEG C or so, addition accounts for ice water amount one third
The trash ice of left and right, adds 5% or so petroleum ether of water.Mixed liquor stirs ice solution after cyclization is added, and is collected by liquid separation organic
Phase is added in water phase and is same as above 5% petroleum ether extraction twice, merges organic phase.Water phase is acid pickle, all removes processing.
The purity of obtained alpha, beta-lonone, yield, waste sulfuric acid concentration, ice solution electricity consumption and it is cooled to -10 DEG C
Time, see Table 1 for details.
The purity of 1 embodiment 1-4 of table and the alpha, beta-lonone of comparative example 1, yield, waste sulfuric acid concentration, ice solution electricity consumption
With the passage of calendar time for being cooled to -10 DEG C
Wherein, waste sulfuric acid concentration after applying 10 times in terms of；Ice solution electricity consumption is compared with the electricity consumption of comparative example 1 for 1；
Being cooled to -10 DEG C of time is compared with used time of comparative example 1 amount for 1, is compared with 25 DEG C of temperature.
Alpha, beta-lonone lowest purity as vitamin A raw material must reach 94%, and sulfur waste acid concentration will reach
60%, otherwise phosphate fertilizer plant cannot use, it is also contemplated that the alpha, beta-lonone cyclization time matches with cooling time in embodiment 3, because
The operating condition and proportion of this embodiment 3 are best.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (9)
1. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process, which is characterized in that this method is specific
Are as follows: the extraction of ice solution is carried out to the alpha, beta-lonone mixed liquor after cyclization using ice water liquid, separation alpha, beta-lonone containing high concentration
Organic phase and water phase, recovery section water phase and supplement ice water liquid to be used for ice solution extraction water it is constant, to ice solution non-after cyclization
Alpha, beta-lonone mixed liquor repeat the operation of above ice solution.
2. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 1,
Be characterized in that, the method specifically includes the following steps:
(a) water for accounting for ice solution autoclave body product 20-60% is added in ice solution kettle, is cooled to -5~5 DEG C, sequentially adding volume is water
Trash ice and volume be water 2-8% petroleum ether, obtain the ice water liquid for ice solution；
(b) in the ice water liquid for taking part steps (a) to prepare, and β-purple sieve after the cyclization that volume is ice water liquid 1/3-1/5 is added
Blue ketone mixed liquor is stirred ice solution, forms organic phase and water phase and separates；
(c) petroleum ether that volume is water 2-8% is added in the water phase that step (b) obtains to be extracted, by what is be obtained by extraction
The organic phase of the alpha, beta-lonone containing high concentration merges with the organic phase that step (b) obtains, and the 60-90% for the water phase being obtained by extraction is then
Be back into ice solution kettle, and supplement water or trash ice to be used for ice solution extraction water it is constant, repeat above step.
3. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, the water being added in step (a) is the 40% of ice solution autoclave body product.
4. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, water is added in ice solution kettle in step (a), is cooled to 0 DEG C.
5. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, in step (a), trash ice additional amount is the 1/3 of water.
6. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, in step (a) and step (c), petroleum ether additional amount is the 5% of water.
7. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, in step (b), the alpha, beta-lonone mixeding liquid volume after cyclization is the 1/4 of ice water liquid.
8. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2,
It is characterized in that, in step (c), petroleum ether repeats to extract twice.
9. a kind of recycling ice solution processing method suitable for alpha, beta-lonone production process according to claim 2, step
Suddenly in (c), the amount for recycling water phase accounts for the 70% of water phase volume extracted.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496006A (en) * | 2016-09-30 | 2017-03-15 | 万华化学集团股份有限公司 | A kind of method for preparing β ionoionone using modified functionalized acidic ionic liquid |
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- 2019-07-19 CN CN201910656375.6A patent/CN110372485A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496006A (en) * | 2016-09-30 | 2017-03-15 | 万华化学集团股份有限公司 | A kind of method for preparing β ionoionone using modified functionalized acidic ionic liquid |
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| 卢季红; 姚毅: "改进β-紫罗兰酮的合成方法", 《贵州化工》 * |
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Application publication date: 20191025 |