CN108689833A - A kind of high-pure lactic acid preparation method of stabilization - Google Patents
A kind of high-pure lactic acid preparation method of stabilization Download PDFInfo
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- CN108689833A CN108689833A CN201810555080.5A CN201810555080A CN108689833A CN 108689833 A CN108689833 A CN 108689833A CN 201810555080 A CN201810555080 A CN 201810555080A CN 108689833 A CN108689833 A CN 108689833A
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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
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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
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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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
- C07C51/50—Use of additives, e.g. for stabilisation
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Abstract
The invention discloses a kind of high-pure lactic acid preparation methods of stabilization, specifically include following steps:(1)It feeds intake:Lactic acid is added in reaction kettle, is stirred evenly, diluent and depolymerizing agent, heating stirring are then added;(2)Vacuum distillation:Collect the step(1)In fraction;(3)It preserves:By the step(2)The fraction of collection imports in the collecting tank for filling purified water, is then discharged in hermetically sealed can, seals room temperature preservation.The technical problem to be solved by the present invention is to lactic acid can occur self-polymerization in purification process, the problem for causing its purity and stability not high, the present invention adds diluent and depolymerizing agent in commercially available lactic acid, carry out vacuum distillation purifying, the high-pure lactic acid distilled out is diluted storage immediately, the high-pure lactic acid stablized.
Description
Technical field
The present invention relates to a kind of lactic acid preparation method more particularly to a kind of high-pure lactic acid preparation methods of stabilization.
Background technology
Lactic acid is widely used in the important organic acid of chemical industry, light industry, food and medicine.In recent years, lactic acid is in medicine and doctor
Application constantly expands in terms of medicine intermediate.It has also been found that the autopolymer of lactic acid and its there is life with the copolymers of other compounds
Object degradability, application value are increasingly that people pay attention to;For chemical industry, the lactic acid of field of light industry, purity also need not be too high;And it uses
In the lactic acid of food and medicine, just there are very high requirement, therefore input great effort research both at home and abroad to its purity and stability
The separation and purification of lactic acid, but so far, the refined purification of lactic acid does not all solve very well, is primarily due to lactic acid and is purifying
Self-polymerization can occur for process, and this polymer can be good at coexisting with lactic acid, and which results in commercially available lactic acid, no
Pipe is that food-grade or pharmaceutical grade all contain 10%-15% lactic acid polymers.
Invention content
The object of the present invention is to provide a kind of high-pure lactic acid preparation methods of stabilization, in order to solve lactic acid in purification process
Self-polymerization can occur, the problem for causing its purity and stability not high.
To achieve the goals above, present invention employs following technical solutions:
The present invention provides a kind of high-pure lactic acid preparation method of stabilization, specifically includes following steps:
(1) it feeds intake:Lactic acid is added in reaction kettle, is stirred evenly, diluent and depolymerizing agent are then added, heating is stirred
It mixes;
(2) it is evaporated under reduced pressure:Collect the fraction in the step (1);
(3) it preserves:The fraction that the step (2) is collected is imported in the collecting tank for filling purified water, is then discharged to close
In sealed cans, room temperature preservation is sealed;
The lactic acid of pharmaceutical grade preserves:The fraction that the step (2) is collected is imported in the collecting tank for filling water for injection, so
After be discharged in hermetically sealed can, seal room temperature preservation, pharmaceutical grade lactic acid requires purity and stability high, and water for injection is selected to replace
Purified water can improve the purity and stability of lactic acid, ensure that drug effect.
Preferably, diluent is high boiling solvent in step (1), and the high boiling solvent is preferably glycerine, poly- second two
Alcohol, one kind in two polyglycerols or mutual mixture.
Preferably, depolymerizing agent is organic amine compound or quaternary ammonium salt in step (1), and the organic amine compound is preferred
For tetrabutylammonium bromide, diisopropylethylamine, N, one kind in N- dimethyl butylamines or mutual mixture.
Preferably, lactic acid is added in reaction kettle by step (1), is stirred evenly, is then added diluent and depolymerizing agent,
It is warming up to 140~150 DEG C.
Preferably, the condition that fraction is collected in step (2) is 110~120 DEG C of temperature, and pressure is -0.2~-0.15Mpa.
Preferably, in step (3) when lactic acid concn reaches 10%~15% in collecting tank, stop collecting.
Preferably, the addition quality of diluent is 2~3 times of lactic acid inventory in step (1).
Preferably, the addition quality of depolymerizing agent is 0.02~0.05 times of lactic acid inventory in step (1).
Advantageous effect of the present invention:The technical problem to be solved by the present invention is to lactic acid can occur self-polymerization in purification process,
The problem for causing its purity and stability not high, the present invention add diluent and depolymerizing agent in commercially available lactic acid, carry out decompression steaming
Purifying is evaporated, the high-pure lactic acid distilled out is diluted storage immediately.Realize following purpose:1, it distills in substrate and increases boiling point
Solvent dilutes and depolymerizing agent is added, and avoids lactic acid in distillation process from polymerizeing rapidly at high temperature, lactic acid is under a high concentration condition
Easily polymerization, it is therefore desirable to add dilution dilution agent, additionally incorporate depolymerizing agent and prevent its polymerization;2, by the lactic acid distilled out immediately with pure
Change water, which is diluted under the concentration of 10%-15%, to be stored, and lactic acid is stablized at this concentration, substantially will not during storage
It polymerize.
Description of the drawings
Fig. 1 is commercially available lactic acid purity chromatogram.
Fig. 2 is the purity chromatogram after commercially available lactic acid purification.
Fig. 3 is the purity chromatogram that diluent is added in commercially available lactic acid.
Fig. 4 is the purity chromatogram that depolymerizing agent is added in commercially available lactic acid.
Fig. 5 is the purity chromatogram that diluent and depolymerizing agent is added in commercially available lactic acid.
Fig. 6 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 5% concentration immediately 1 month
Figure.
Fig. 7 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 5% concentration immediately 2 months
Figure.
Fig. 8 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 5% concentration immediately 3 months
Figure.
Fig. 9 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 10% concentration immediately 1 month
Figure.
Figure 10 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 10% concentration immediately 2 months
Figure.
Figure 11 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 10% concentration immediately 3 months
Figure.
Figure 12 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 15% concentration immediately 1 month
Figure.
Figure 13 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 15% concentration immediately 2 months
Figure.
Figure 14 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 15% concentration immediately 3 months
Figure.
Figure 15 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 20% concentration immediately 1 month
Figure.
Figure 16 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 20% concentration immediately 2 months
Figure.
Figure 17 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 20% concentration immediately 3 months
Figure.
Figure 18 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 25% concentration immediately 1 month
Figure.
Figure 19 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 25% concentration immediately 2 months
Figure.
Figure 20 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 25% concentration immediately 3 months
Figure.
Figure 21 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 30% concentration immediately 1 month
Figure.
Figure 22 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 30% concentration immediately 2 months
Figure.
Figure 23 is the purity chromatography stored under the lactic acid distilled out is diluted with purified water to 30% concentration immediately 3 months
Figure.
Figure 24 is commercially available lactic acid, without dilution agent and depolymerizing agent, only adds diluent, only adds depolymerizing agent and diluent reconciliation
The Contrast on effect purity chromatogram that poly- agent two adds simultaneously.
Specific implementation mode
In order to deepen the understanding of the present invention, present invention work is further retouched in detail below in conjunction with drawings and examples
It states, the present embodiment is only used for explaining the present invention, does not constitute and limits to protection scope of the present invention.
Embodiment 1
(at pharmaceutcal corporation, Ltd, lot number 161204, purity 63.5%, commercially available lactic acid is or not Henan day for the commercially available lactic acid of 50Kg
Pipe is that food-grade or pharmaceutical grade all contain 10%-15% lactic acid polymers, and after storing a period of time, polymer can increase
More, the commercially available lactic acid purity bought in the present embodiment and following embodiment is 63.5%), to do purity chromatogram, obtain chromatography
Fig. 1, table 1 corresponding with chromatogram 1 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.260 | 2009274 | 270110 | 63.517 | 6865 | 1.309 | 0.206 | -- |
| 2 | 9.804 | 937772 | 70515 | 29.645 | 12126 | 1.195 | 0.356 | 19.738 |
| 3 | 12.003 | 216303 | 4883 | 6.838 | 1664 | 1.128 | 1.177 | 2.869 |
| It amounts to | 3163348 | 345508 | 100.000 |
Embodiment 2
The commercially available lactic acid of 50Kg (Henan day is at pharmaceutcal corporation, Ltd, lot number 161204, purity 63.5%), to 50Kg market milks
Acid is refined, and the 2 corresponding table 2 of purity chromatogram of lactic acid is as follows after refining:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.250 | 2302995 | 308394 | 71.222 | 6735 | 1.318 | 0.207 | -- |
| 2 | 4.703 | 1800 | 239 | 0.056 | 9125 | 1.500 | 0.197 | 2.238 |
| 3 | 9.809 | 928758 | 69894 | 28.723 | 12151 | 1.194 | 0.356 | 18.472 |
| It amounts to | 3233552 | 378526 | 100.000 |
Embodiment 3
The commercially available lactic acid of 50Kg (Henan day is at pharmaceutcal corporation, Ltd, lot number 161204, purity 63.5%), it is anti-to be added to 300L
It answers in kettle, stirs evenly, 100Kg glycerine is added, be warming up to 140 DEG C, stir, vacuum distillation collects 110 DEG C, -0.2Mpa's
Fraction imports the fraction of collection in the collecting tank for filling 300Kg purified waters, when lactic acid concn reaches 12% in collecting tank,
Stop collecting, blowing seals room temperature preservation.
The 3 corresponding table 3 of purity chromatogram that diluent is added in lactic acid is as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.211 | 2644396 | 359904 | 79.115 | 6834 | 1.319 | 0.204 | -- |
| 2 | 9.441 | 698089 | 55637 | 20.885 | 12585 | 1.157 | 0.337 | 19.357 |
| It amounts to | 3342485 | 415541 | 100.000 |
Embodiment 4
The commercially available lactic acid of 50Kg (Henan day is at pharmaceutcal corporation, Ltd, lot number 161204, purity 63.5%), it is anti-to be added to 300L
It answers in kettle, stirs evenly, 1.32Kg tetrabutylammonium bromide is added, be warming up to 140 DEG C, stir, vacuum distillation collects 110 DEG C ,-
The fraction of collection is imported in the collecting tank for filling 300Kg purified waters, waits for that lactic acid concn reaches in collecting tank by the fraction of 0.2Mpa
When 12%, stop collecting, blowing seals room temperature preservation.
The 4 corresponding table 4 of purity chromatogram that depolymerizing agent is added in lactic acid is as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.210 | 2798827 | 379728 | 86.686 | 6786 | 1.327 | 0.204 | -- |
| 2 | 4.693 | 1322 | 205 | 0.041 | 9418 | 1.478 | 0.193 | 2.425 |
| 3 | 9.446 | 428529 | 26614 | 13.273 | 10438 | 0.966 | 0.370 | 16.876 |
| It amounts to | 3228679 | 406546 | 100.000 |
Embodiment 5
The commercially available lactic acid of 50Kg (Henan day is at pharmaceutcal corporation, Ltd, lot number 161204, purity 63.5%), it is anti-to be added to 300L
It answers in kettle, stirs evenly, 100Kg glycerine and 1.32Kg tetrabutylammonium bromide is added, be warming up to 140 DEG C, stirring, decompression is steamed
It evaporates, collects 110 DEG C, the fraction of collection is imported in the collecting tank for filling 300Kg purified waters, waits for collecting tank by the fraction of -0.2Mpa
When middle lactic acid concn reaches 12%, stop collecting, blowing seals room temperature preservation.
Diluent is added in lactic acid and the 5 corresponding table 5 of purity chromatogram of depolymerizing agent is as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.246 | 3769165 | 477651 | 98.606 | 6081 | 1.378 | 0.218 | -- |
| 2 | 4.767 | 35149 | 6102 | 0.920 | 13722 | 1.001 | 0.163 | 2.741 |
| 3 | 9.803 | 18151 | 1395 | 0.475 | 12523 | 1.186 | 0.350 | 19.625 |
| It amounts to | 3822466 | 485149 | 100.000 |
Commercially available lactic acid, without dilution agent and the depolymerizing agent bought, only plus diluent, only plus depolymerizing agent and diluent reconciliation
Contrast on effect spectrogram such as Figure 24, Figure 24 that poly- agent two adds simultaneously are followed successively by commercially available lactic acid, without dilution agent reconciliation from top to bottom
Poly- agent, the spectrum curve for adding diluent, depolymerizing agent and diluent and depolymerizing agent two only being added to add simultaneously, bind profile Figure 24,
It is as follows that spectrogram 1-5 and table 1-5 can obtain table 6:
Table 6 plus diluent and depolymerizing agent and the Contrast on effect being not added with
Note:"+", which represents, to be added, and "-" representative is not added with
As can be seen from Table 6, when diluent only adds one of which substance with depolymerizing agent, purity ratio is not added with any type object
Purity is high when matter, and when the two is added simultaneously, purity can reach 98.60%, it will thus be seen that adding diluent in commercially available lactic acid
And depolymerizing agent, vacuum distillation purifying is carried out, the high-pure lactic acid distilled out is diluted to the lactic acid purity that storage obtains immediately
It is very high, it disclosure satisfy that application of the lactic acid in food and medicine.
The lactic acid distilled out is diluted immediately with purified water under the concentration of 5%-30% below and stores different time
The corresponding peak table of purity chromatogram it is as follows:
1, the lactic acid distilled out stores 1 month purity chromatogram 6 under being diluted immediately to 5% concentration with purified water is right
The peak table 7 answered is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.193 | 2953422 | 434805 | 98.076 | 7340 | 1.363 | 0.196 | -- |
| 2 | 9.461 | 57947 | 4790 | 1.924 | 13199 | 1.122 | 0.329 | 20.061 |
| It amounts to | 3011369 | 439595 | 100.000 |
2, the lactic acid distilled out stores 2 months purity chromatogram 7 under being diluted immediately to 5% concentration with purified water is right
The peak table 8 answered is as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.113 | 2785448 | 344051 | 97.301 | 5632 | 1.515 | 0.219 | -- |
| 2 | 4.647 | 10971 | 2019 | 0.383 | 13554 | 1.078 | 0.160 | 2.818 |
| 3 | 9.122 | 66304 | 5176 | 2.316 | 11395 | 1.187 | 0.342 | 17.850 |
| It amounts to | 2862723 | 351246 | 100.000 |
3, the lactic acid distilled out stores 3 months purity chromatogram 8 under being diluted immediately to 5% concentration with purified water is right
The peak table 9 answered is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.134 | 2994108 | 458764 | 96.939 | 7685 | 1.379 | 0.189 | -- |
| 2 | 8.875 | 94534 | 8421 | 3.061 | 13215 | 1.136 | 0.309 | 19.059 |
| It amounts to | 3088642 | 467186 | 100.000 |
4, the lactic acid distilled out stores 1 month purity chromatogram 9 under being diluted immediately to 10% concentration with purified water
Corresponding peak table 10 is as follows:
PDA Ch1 20gnm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.131 | 1631444 | 238707 | 99.053 | 6909 | 1.312 | 0.199 | -- |
| 2 | 8.922 | 15599 | 1325 | 0.947 | 12125 | 1.075 | 0.324 | 18.324 |
| It amounts to | 1647042 | 240032 | 100.000 |
5, the lactic acid distilled out stores 2 months purity chromatograms 10 under being diluted immediately to 10% concentration with purified water
Corresponding peak table 11 is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.192 | 3298328 | 482038 | 98.870 | 7248 | 1.382 | 0.197 | -- |
| 2 | 9.465 | 37685 | 3124 | 1.130 | 13251 | 1.135 | 0.329 | 20.057 |
| It amounts to | 3336014 | 485162 | 100.000 |
6, the lactic acid distilled out stores 3 months purity chromatograms 11 under being diluted immediately to 10% concentration with purified water
Corresponding peak table 12 is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.132 | 1567441 | 229407 | 98.300 | 6952 | 1.310 | 0.198 | -- |
| 2 | 8.905 | 27105 | 2300 | 1.700 | 12120 | 1.142 | 0.324 | 18.296 |
| It amounts to | 1594547 | 231707 | 100.000 |
7, the lactic acid distilled out stores 1 month purity chromatogram 12 under being diluted immediately to 15% concentration with purified water
Corresponding peak table 13 is as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.115 | 2881438 | 350514 | 98.336 | 5493 | 1.531 | 0.222 | -- |
| 2 | 4.643 | 7423 | 980 | 0.253 | 10700 | 2.307 | 0.180 | 2.628 |
| 3 | 9.152 | 41332 | 3204 | 1.411 | 11279 | 1.192 | 0.345 | 17.202 |
| It amounts to | 2930192 | 354697 | 100.000 |
8, the lactic acid distilled out stores 2 months purity chromatograms 13 under being diluted immediately to 15% concentration with purified water
Corresponding peak table 14 is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.131 | 3175954 | 485439 | 98.769 | 7524 | 1.391 | 0.191 | -- |
| 2 | 8.828 | 39587 | 3572 | 1.231 | 13442 | 1.123 | 0.305 | 18.974 |
| It amounts to | 3215542 | 489011 | 100.000 |
9, the lactic acid distilled out stores 3 months purity chromatograms 14 under being diluted immediately to 15% concentration with purified water
Corresponding peak table 15 is as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.141 | 3108911 | 474479 | 97.938 | 7500 | 1.382 | 0.191 | -- |
| 2 | 8.869 | 65455 | 5827 | 2.062 | 13281 | 1.133 | 0.308 | 18.946 |
| It amounts to | 3174366 | 480306 | 100.000 |
10, the lactic acid distilled out stores 1 month purity chromatogram under being diluted immediately to 20% concentration with purified water
15 corresponding peak tables 16 are as follows:
PDA Ch1 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.140 | 1537255 | 225899 | 97.371 | 7110 | 1.310 | 0.196 | -- |
| 2 | 8.905 | 41498 | 3509 | 2.629 | 11997 | 1.121 | 0.325 | 18.272 |
| It amounts to | 1578752 | 229408 | 100.000 |
11, the lactic acid distilled out stores 2 months purity chromatograms under being diluted immediately to 20% concentration with purified water
16 corresponding peak tables 17 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.123 | 3272913 | 451017 | 97.102 | 6684 | 1.392 | 0.202 | -- |
| 2 | 4.639 | 15072 | 2503 | 0.447 | 11418 | 1.064 | 0.174 | 2.748 |
| 3 | 9.236 | 83609 | 6706 | 2.451 | 12520 | 1.192 | 0.330 | 18.249 |
| It amounts to | 3370594 | 460227 | 100.000 |
12, the lactic acid distilled out stores 3 months purity chromatograms under being diluted immediately to 20% concentration with purified water
17 corresponding peak tables 18 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.126 | 3051056 | 422826 | 95.687 | 6748 | 1.383 | 0.201 | -- |
| 2 | 4.639 | 7712 | 1252 | 0.242 | 10824 | 1.091 | 0.178 | 2.706 |
| 3 | 9.250 | 129815 | 10580 | 4.071 | 12583 | 1.192 | 0.330 | 18.145 |
| It amounts to | 3188583 | 434657 | 100.000 |
13, the lactic acid distilled out stores 1 month purity chromatogram under being diluted immediately to 25% concentration with purified water
18 corresponding peak tables 19 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.125 | 2947321 | 408629 | 96.279 | 6755 | 1.379 | 0.201 | -- |
| 2 | 4.640 | 11817 | 1903 | 0.386 | 10728 | 1.065 | 0.179 | 2.711 |
| 3 | 9.254 | 102094 | 8266 | 3.335 | 12583 | 1.192 | 0.330 | 18.123 |
| It amounts to | 3061232 | 418799 | 100.000 |
14, the lactic acid distilled out stores 2 months purity chromatograms under being diluted immediately to 25% concentration with purified water
19 corresponding peak tables 20 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.125 | 2708822 | 375997 | 94.862 | 6771 | 1.370 | 0.201 | -- |
| 2 | 4.635 | 6580 | 1074 | 0.230 | 10759 | 1.084 | 0.179 | 2.686 |
| 3 | 9.234 | 140137 | 11381 | 4.908 | 12514 | 1.196 | 0.330 | 18.075 |
| It amounts to | 2855539 | 388452 | 100.000 |
15, the lactic acid distilled out stores 3 months purity chromatograms under being diluted immediately to 25% concentration with purified water
20 corresponding peak tables 21 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.122 | 3059748 | 422184 | 94.274 | 6705 | 1.387 | 0.201 | -- |
| 2 | 4.639 | 9146 | 1485 | 0.282 | 10856 | 1.062 | 0.178 | 2.727 |
| 3 | 9.289 | 176696 | 14222 | 5.444 | 12462 | 1.199 | 0.333 | 18.199 |
| It amounts to | 3245589 | 437891 | 100.000 |
16, the lactic acid distilled out stores 1 month purity chromatogram under being diluted immediately to 30% concentration with purified water
21 corresponding peak tables 22 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.124 | 3052086 | 421254 | 96.215 | 6699 | 1.383 | 0.202 | -- |
| 2 | 4.637 | 8969 | 1459 | 0.283 | 10941 | 1.087 | 0.177 | 2.705 |
| 3 | 9.236 | 111084 | 9031 | 3.502 | 12528 | 1.192 | 0.330 | 18.128 |
| It amounts to | 3172138 | 431744 | 100.000 |
17, the lactic acid distilled out stores 2 months purity chromatograms under being diluted immediately to 30% concentration with purified water
22 corresponding peak tables 23 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.130 | 2696144 | 374192 | 94.199 | 6806 | 1.373 | 0.200 | -- |
| 2 | 4.641 | 5810 | 948 | 0.203 | 10836 | 1.101 | 0.178 | 2.695 |
| 3 | 9.246 | 160214 | 13031 | 5.598 | 12584 | 1.196 | 0.330 | 18.133 |
| It amounts to | 2862168 | 388171 | 100.000 |
18, the lactic acid distilled out stores 3 months purity chromatograms under being diluted immediately to 30% concentration with purified water
23 corresponding peak tables 24 are as follows:
Detector A 209nm
| Peak number | Retention time | Area | Highly | Area % | Theoretical cam curve | Tailing factor | USP peak width | Separating degree (USP) |
| 1 | 4.122 | 2991473 | 414077 | 93.995 | 6745 | 1.384 | 0.201 | -- |
| 2 | 4.638 | 6590 | 1068 | 0.207 | 10743 | 1.083 | 0.179 | 2.718 |
| 3 | 9.274 | 184520 | 14896 | 5.798 | 12492 | 1.200 | 0.332 | 18.151 |
| It amounts to | 3182583 | 430041 | 100.000 |
It can be obtained such as the following table 25 by peak table 7-24 and spectrogram 6-23:
The stability contrast of the lactic acid of 25 various concentration of table
As seen from the above table, the lactic acid storage of a concentration of 10%-15% is stablized, and will not be gathered substantially during storage
It closes.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of high-pure lactic acid preparation method of stabilization, which is characterized in that specifically include following steps:
(1)It feeds intake:Lactic acid is added in reaction kettle, is stirred evenly, diluent and depolymerizing agent, heating stirring are then added;
(2)Vacuum distillation:Collect the step(1)In fraction;
(3)It preserves:By the step(2)The fraction of collection imports in the collecting tank for filling purified water, is then discharged to hermetically sealed can
In, seal room temperature preservation.
2. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(1)
Middle diluent be high boiling solvent, the high boiling solvent be preferably glycerine, polyethylene glycol, one kind in two polyglycerols or
Mutual mixture.
3. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(1)
Middle depolymerizing agent is organic amine compound or quaternary ammonium salt, and the organic amine compound is preferably tetrabutylammonium bromide, diisopropyl
Base ethamine, N, one kind in N- dimethyl butylamines or mutual mixture.
4. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(1)
Lactic acid is added in reaction kettle, is stirred evenly, diluent and depolymerizing agent are then added, is warming up to 140~150 DEG C.
5. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(2)
The middle condition for collecting fraction is 110~120 DEG C of temperature, and pressure is -0.2~-0.15Mpa.
6. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(3)
In when lactic acid concn reaches 10%~15% in collecting tank, stop collect.
7. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(1)
The addition quality of middle diluent is 2~3 times of lactic acid inventory.
8. a kind of high-pure lactic acid preparation method of stabilization according to claim 1, it is characterised in that:The step(1)
The addition quality of middle depolymerizing agent is 0.02~0.05 times of lactic acid inventory.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0986532A1 (en) * | 1997-06-06 | 2000-03-22 | Brussels Biotech | Method for purifying lactic acid |
| CN1287113A (en) * | 1999-06-28 | 2001-03-14 | 罗姆和哈斯公司 | Process for producing (methyl) propenoic acid |
| CN101495440A (en) * | 2006-08-02 | 2009-07-29 | 株式会社吴羽 | Method for purifying hydroxycarboxylic acid, method for producing cyclic ester, and method for producing polyhydroxycarboxylic acid |
| CN107098808A (en) * | 2017-05-05 | 2017-08-29 | 湖北壮美生物科技有限公司 | The preparation method and process units of a kind of high-purity, high content normal temperature not crystalline lactic acid product |
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2018
- 2018-06-01 CN CN201810555080.5A patent/CN108689833B/en active Active
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|---|---|---|---|---|
| EP0986532A1 (en) * | 1997-06-06 | 2000-03-22 | Brussels Biotech | Method for purifying lactic acid |
| CN1287113A (en) * | 1999-06-28 | 2001-03-14 | 罗姆和哈斯公司 | Process for producing (methyl) propenoic acid |
| CN101495440A (en) * | 2006-08-02 | 2009-07-29 | 株式会社吴羽 | Method for purifying hydroxycarboxylic acid, method for producing cyclic ester, and method for producing polyhydroxycarboxylic acid |
| CN107098808A (en) * | 2017-05-05 | 2017-08-29 | 湖北壮美生物科技有限公司 | The preparation method and process units of a kind of high-purity, high content normal temperature not crystalline lactic acid product |
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