CN102050723B - Method for producing sodium lactate - Google Patents
Method for producing sodium lactate Download PDFInfo
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- CN102050723B CN102050723B CN 200910188147 CN200910188147A CN102050723B CN 102050723 B CN102050723 B CN 102050723B CN 200910188147 CN200910188147 CN 200910188147 CN 200910188147 A CN200910188147 A CN 200910188147A CN 102050723 B CN102050723 B CN 102050723B
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- hydroxypropionate
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Abstract
The invention relates to a method for preparing refining sodium lactate, in particular to a method for extracting and preparing refining sodium lactate from fermentation liquor of calcium lactate. In the method, the calcium lactate is converted into the sodium lactate by utilizing a double salt precipitation reaction, wherein calcium carbonate or calcium hydroxide is formed simultaneously as a byproduct; and the refining sodium lactate is obtained by combining the technology of resin purifying, membrane filtration and electroosmosis. The lactate-containing calcium carbonate or calcium hydroxide serving as the byproduct is recycled as a neutralizing agent, so waste residues are not discharged, the extraction yield of the sodium lactate can be increased, and the production cost of the sodium lactate also can be reduced.
Description
Technical field
The present invention relates to a kind of method of method for preparing fine purification of lactic acid sodium, the particularly extraction from calcium lactate fermentation solution and fine purification of lactic acid sodium.
Background technology
Sodium.alpha.-hydroxypropionate (Sodium Lactate) molecular formula C
3H
5NaO
3, molecular weight 112.06, colourless or almost colourless transparent liquid can fuse with water, ethanol, glycerine.Sodium.alpha.-hydroxypropionate is industrial of many uses, is applied to fresh-keeping, moisturizing, flavouring and the pharmaceutical raw material of food.
The traditional technology process of industrial production Sodium.alpha.-hydroxypropionate is: first with sulfuric acid, calcium lactate is carried out acidolysis, then filter, decolouring and ion-exchange, obtain lactic acid.Lactic acid and sodium carbonate or sodium hydroxide are carried out neutralization reaction, namely obtain Sodium.alpha.-hydroxypropionate.The method production cost is high, the cycle long, byproduct calcium sulfate can not effectively utilize, thereby cause environmental pollution.The traditional technology of producing Sodium.alpha.-hydroxypropionate exists significantly not enough, therefore is badly in need of developing a kind of new production technique, to reduce the production cost of Sodium.alpha.-hydroxypropionate, improves the quality of Sodium.alpha.-hydroxypropionate product, thus the heavy demand of satisfying the market to Sodium.alpha.-hydroxypropionate better.Byproduct of reaction is utilized effectively, avoids causing environmental pollution.
it is raw material that CN99116651.5 adopts edible lactic acid or fine purification of lactic acid, be three steps with ester salt legal system extracting lactic acid sodium basic technology, the first step, with edible lactic acid or fine purification of lactic acid and alcohol compound methyl alcohol, any mixing in ethanol and butanols, esterification occurs under certain temperature and pressure condition generate the lactic acid ester reactant, second step, under the certain temperature condition, make lactic acid ester and sodium carbonate or sodium hydroxide carry out the saponification reaction of equimolar ratio, produce elementary Sodium.alpha.-hydroxypropionate, the 3rd step, elementary Sodium.alpha.-hydroxypropionate is through absorption, decolouring, after exchange purifies, regulate its pH value and content and namely obtain the finished product Sodium.alpha.-hydroxypropionate.Use edible lactic acid or fine purification of lactic acid and alcohols because of this invention and carry out esterification, and need to reclaim pure reagent, have complex process, the demanding shortcoming of starting material.
CN200610009657.X relates to the frequently pole-reversing electroosmosis method of extraction and concentration Sodium.alpha.-hydroxypropionate from garbage fermentation liquid, a kind of extraction and concentration method and device thereof of Sodium.alpha.-hydroxypropionate have been proposed, purpose be for solve from garbage fermentation liquid extract and the traditional electrical dialysis method of concentrating sodium lactate in exist film to pollute problem.The fermented liquid of this invention is the Sodium.alpha.-hydroxypropionate fermented liquid, and this carries out the front sodium lactate solution of electrodialysis process from the present invention and comes source procedure fully different.And before entering electrodialyzer in this invention, the Sodium.alpha.-hydroxypropionate fermented liquid does not pass through purifying treatment, will certainly produce the film of electrodialyzer to pollute, and causes electrodialyzer current efficiency low, has increased production cost.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of fine purification of lactic acid sodium particularly directly extracts the also method of fine purification of lactic acid sodium from calcium lactate fermentation solution, there is no the calcium sulfate waste residues discharging, and the by-product reusable edible.
The present invention extracts the method for Sodium.alpha.-hydroxypropionate from contain calcium lactate fermentation solution, comprise the following steps:
(1) contain calcium lactate fermentation solution and be heated to 60～100 ℃, and to regulate pH value be 7～12, filtration obtains calcium lactate filtrate;
(2) concentrated lactic acid calcium solution to lactate content is 200～500g/L, adds sodium carbonate and/or sodium hydroxide, 40～100 ℃ of reactions 0.5～4 hour, makes the calcium ion precipitation fully, filters calcium carbonate or calcium hydroxide, obtains sodium lactate solution;
(3) add the gac of 0.3wt%～3wt% in the sodium lactate solution, 60～100 ℃ of decolourings 15～60 minutes, filter and obtain Sodium.alpha.-hydroxypropionate filtrate;
(4) the Sodium.alpha.-hydroxypropionate filtrate that is obtained by step (3) removes the impurity such as polyvalent metal ion through plastic resin treatment; Sodium lactate solution after resin purifies is optionally processed through membrane filtration;
(5) sodium lactate solution of rough purification through electrodialysis process, makes Sodium.alpha.-hydroxypropionate effectively be separated with impurity, obtains pure sodium lactate solution;
(6) pure sodium lactate solution is 40%～80% qualified product through the concentrated massfraction that obtains.
Preferred Heating temperature is 80～90 ℃ in step of the present invention (1), and preferred pH value is 8.0～10.0, more preferably 9.0～9.5;
After calcium lactate solution concentrates in step of the present invention (2), the preferred 300～400g/L of lactate content;
The mol ratio of reaction raw materials lactate and sodium ion is 1: 0.95～1: 1.50 in step of the present invention (2), preferred 1: 0.99～1: 1.15;
Precipitation reaction temperature is preferred 80～90 ℃ in step of the present invention (2), 1～2 hour preferred reaction time.
The gac that preferably adds 0.7wt%～1.5wt% in step of the present invention (3), preferred 70～80 ℃ of bleaching temperature, preferred 25～40 minutes of bleaching time.
Sodium lactate solution after in step of the present invention (4), resin purifies can carry out membrane filtration to be processed, and described membrane filtration comprises one or more in micro-filtration, ultrafiltration and nanofiltration; Perhaps process without micro-filtration, ultrafiltration and nanofiltration, make with extra care and directly advance electrodialysis.
In step of the present invention (5), in order to obtain the pharmaceutical grade Sodium.alpha.-hydroxypropionate, can select the two-stage electrodialysis process.
Neutralizing agent during the calcium carbonate that contains lactate that obtains in step of the present invention (2) or calcium hydroxide can be used as lactic fermentation process.
The pure sodium lactate solution that obtains in step of the present invention (5) can selectivity add pure lactic acid or sodium carbonate or sodium hydroxide, to regulate pH value 6.5～7.5.
Compared with prior art, the inventive method has following advantage:
The present invention utilizes the double salt precipitation reaction, makes calcium lactate be converted into Sodium.alpha.-hydroxypropionate, while by-product calcium carbonate or calcium hydroxide, and binding resin purification, membrane filtration and electrodialytic technique obtain fine purification of lactic acid sodium.By product calcium carbonate or the calcium hydroxide that will contain lactate continue recycle as neutralizing agent, namely without the calcium sulfate waste residues discharging, can increase again the Sodium.alpha.-hydroxypropionate extract yield and reduce production costs.
Embodiment
The present invention directly extracts from calcium lactate fermentation solution and the concrete steps of fine purification of lactic acid sodium comprise:
To contain calcium lactate fermentation solution and be heated to 60～100 ℃, and regulate pH value 7～12, and filter and obtain calcium lactate filtrate; This filtrate is concentrated into lactate content 200～500g/L, the mol ratio that adds lactate and sodium ion is at 1: 0.990～1: 1.150 sodium carbonate or sodium hydroxide, 40～100 ℃ of reactions 0.5～4 hour, make the calcium ion precipitation fully, filter calcium carbonate or calcium hydroxide, obtain sodium lactate solution.
The gac that adds 0.3wt%～3wt% in the sodium lactate solution 60～100 ℃ of decolourings 15～60 minutes, filters and obtains Sodium.alpha.-hydroxypropionate filtrate; This streams is first through plastic resin treatment or optionally through micro-filtration, ultrafiltration and nanofiltration processing, then select one-level or secondary electrodialysis to purify according to Sodium.alpha.-hydroxypropionate Application Areas (food grade or pharmaceutical grade), the concentrated massfraction that obtains is 40%～80% commodity Sodium.alpha.-hydroxypropionate at last.
Below in conjunction with specific embodiment, method of the present invention is described further.
Embodiment 1
Get the calcium lactate fermentation solution that the 1000mL lactate concentration is 180g/L, regulating the pH value is 9.0, be heated to after 90 ℃ of stirrings static 30 minutes, filtration obtains clarifying calcium lactate filtrate 980ml, concentrated this filtrate is to lactate concentration 300g/L, add sodium carbonate 115g, 80 ℃ of stirring reactions 1 hour, filter calcium carbonate and obtain Sodium.alpha.-hydroxypropionate filtrate.
Sodium.alpha.-hydroxypropionate filtrate is heated to 80 ℃, adds the 3.8g gac to stir decolouring 30 minutes, filter and obtain colourless Sodium.alpha.-hydroxypropionate filtrate.The filtrate of decolouring removes the impurity such as polyvalent metal ion, albumen through resin and ultra-filtration membrane, then purifies through electrodialysis, obtains 50% qualified Sodium.alpha.-hydroxypropionate product after concentrating with the newborn acid for adjusting pH value to 6.5 that meets the GB2023-2003 standard～7.5 are last.
Embodiment 2
Get the calcium lactate fermentation solution that the 1000mL lactate concentration is 180g/L, regulating the pH value is 9.5, be heated to after 80 ℃ of stirrings static 30 minutes, filtration obtains clarifying calcium lactate filtrate 980ml, concentrated this filtrate is to lactate concentration 300g/L, add sodium carbonate 115g, 90 ℃ of stirring reactions 1.5 hours, filter calcium carbonate and obtain Sodium.alpha.-hydroxypropionate filtrate.
Sodium.alpha.-hydroxypropionate filtrate is heated to 70 ℃, adds the 3.8g gac to stir decolouring 30 minutes, filter and obtain flaxen Sodium.alpha.-hydroxypropionate filtrate.The filtrate of decolouring removes the impurity such as polyvalent metal ion, albumen through resin, then purifies through electrodialysis, obtains 70% qualified Sodium.alpha.-hydroxypropionate product after concentrating with the newborn acid for adjusting pH value to 6.5 that meets the GB2023-2003 standard～7.5 are last.
Embodiment 3
Get the calcium lactate fermentation solution that the 1000mL lactate concentration is 180g/L, regulating the pH value is 9.0, be heated to after 80 ℃ of stirrings static 30 minutes, filtration obtains clarifying calcium lactate filtrate 980ml, concentrated this filtrate is to lactate concentration 300g/L, add sodium hydroxide 90.5g, 85 ℃ of stirring reactions 2 hours, filter calcium hydroxide and obtain Sodium.alpha.-hydroxypropionate filtrate.
Sodium.alpha.-hydroxypropionate filtrate is heated to 70 ℃, adds the 4.5g gac to stir decolouring 30 minutes, filter and obtain colourless Sodium.alpha.-hydroxypropionate filtrate.Decolouring filtrate removes the impurity such as polyvalent metal ion, albumen through resin and ultra-filtration membrane, sodium lactate solution after purifying through electrodialysis, with the newborn acid for adjusting pH value to 6.5 that meets the GB2023-2003 standard～7.5, obtain 60% qualified Sodium.alpha.-hydroxypropionate product after concentrating at last.
The product property of each embodiment sees Table 1.
Table 1 embodiment product property
| Project | Colourity APHA | Molysite, calcium salt, heavy metal, arsenic salt | Vitriol, muriate | Methyl alcohol | The volatile fat hydrochlorate | Product yield (w%) |
| Example 1 | ≤30 | Qualified | Qualified | Qualified | Without acid smell | 93.2 |
| Example 2 | ≤30 | Qualified | Qualified | Qualified | Without acid smell | 93.7 |
| Example 3 | ≤30 | Qualified | Qualified | Qualified | Without acid smell | 92.6 |
Claims (11)
1. the preparation method of a fine purification of lactic acid sodium comprises the following steps:
(1) contain calcium lactate fermentation solution and be heated to 60～100 ℃, and to regulate pH value be 7～12, filtration obtains calcium lactate filtrate;
(2) concentrated lactic acid calcium solution to lactate content is 200～500g/L, adds sodium carbonate and/or sodium hydroxide, 40～100 ℃ of reactions 0.5～4 hour, makes the calcium ion precipitation fully, filters calcium carbonate or calcium hydroxide, obtains sodium lactate solution;
(3) add the gac of 0.3wt%～3wt% in the sodium lactate solution, 60～100 ℃ of decolourings 15～60 minutes, filter and obtain Sodium.alpha.-hydroxypropionate filtrate;
(4) the Sodium.alpha.-hydroxypropionate filtrate that is obtained by step (3) removes polyvalent metal ion impurity through plastic resin treatment; Sodium lactate solution after resin purifies is optionally processed through membrane filtration;
(5) sodium lactate solution of rough purification through electrodialysis process, makes Sodium.alpha.-hydroxypropionate effectively be separated with impurity, obtains pure sodium lactate solution;
(6) pure sodium lactate solution is through concentrated 40%～80% the qualified product that obtain.
2. according to preparation method claimed in claim 1, it is characterized in that, the Heating temperature described in step (1) is 80～90 ℃, and the pH value is 8.0～10.0.
3. according to the described preparation method of claim 1 or 2, it is characterized in that, regulating the pH value in step (1) is 9.0～9.5.
4. according to preparation method claimed in claim 1, it is characterized in that, in step (2), that calcium lactate solution is concentrated after to lactate content be 300～400g/L.
5. according to preparation method claimed in claim 1, it is characterized in that, the mol ratio that the add-on of the middle sodium carbonate of step (2) or sodium hydroxide satisfies lactate and sodium ion is 1: 0.95～1: 1.50.
6. according to the described preparation method of claim 1 or 5, it is characterized in that, the mol ratio that the add-on of the middle sodium carbonate of step (2) or sodium hydroxide satisfies lactate and sodium ion is 1: 0.99～1: 1.15.
7. according to preparation method claimed in claim 1, it is characterized in that, in step (2), the temperature of precipitin reaction is 80～90 ℃, and the reaction times is 1～2 hour.
8. according to preparation method claimed in claim 1, it is characterized in that, in step (3), the add-on of gac accounts for the 0.7wt%～1.5wt% of sodium lactate solution, and bleaching temperature is 70～80 ℃, and bleaching time is 25～40 minutes.
9. according to preparation method claimed in claim 1, it is characterized in that, select the secondary electrodialysis process in step (5), to obtain the pharmaceutical grade Sodium.alpha.-hydroxypropionate.
10. according to preparation method claimed in claim 1, it is characterized in that, the pure sodium lactate solution that obtains in the step (5) adds pure lactic acid, sodium carbonate or sodium hydroxide, and regulating the pH value is 6.5～7.5.
11. according to preparation method claimed in claim 1, it is characterized in that, described membrane filtration is processed one or more that comprise in micro-filtration, ultrafiltration and nanofiltration.
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| CN 200910188147 CN102050723B (en) | 2009-10-27 | 2009-10-27 | Method for producing sodium lactate |
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| CN 200910188147 CN102050723B (en) | 2009-10-27 | 2009-10-27 | Method for producing sodium lactate |
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| CN102050723B true CN102050723B (en) | 2013-06-19 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102838476B (en) * | 2012-08-07 | 2014-11-05 | 蚌埠丰原涂山制药有限公司 | Preparation method for 60-65% sodium lactate solution |
| CN110372497A (en) * | 2019-08-30 | 2019-10-25 | 临沂艾德森生物科技有限公司 | A kind of method that crude lactic acid salting liquid prepares high purity powdered form lactate |
| CN112812004B (en) * | 2020-12-25 | 2023-09-29 | 蚌埠丰原涂山制药有限公司 | Industrial preparation method of sodium lactate solution |
| CN113292415B (en) * | 2021-05-28 | 2022-12-06 | 河北圣雪大成制药有限责任公司 | Method for recovering sodium lactate from nisin fermentation broth |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4885247A (en) * | 1988-04-19 | 1989-12-05 | Michigan Biotechnology Institute | Recovery and purification of lactate salts from whole fermentation broth by electrodialysis |
| CN101018756A (en) * | 2004-06-17 | 2007-08-15 | 普拉克生化公司 | Process for the preparation of lactic acid or lactate from a magnesium lactate comprising medium |
| CN101265179A (en) * | 2008-04-18 | 2008-09-17 | 南京工业大学 | A kind of purification process of lactate |
-
2009
- 2009-10-27 CN CN 200910188147 patent/CN102050723B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4885247A (en) * | 1988-04-19 | 1989-12-05 | Michigan Biotechnology Institute | Recovery and purification of lactate salts from whole fermentation broth by electrodialysis |
| CN101018756A (en) * | 2004-06-17 | 2007-08-15 | 普拉克生化公司 | Process for the preparation of lactic acid or lactate from a magnesium lactate comprising medium |
| CN101265179A (en) * | 2008-04-18 | 2008-09-17 | 南京工业大学 | A kind of purification process of lactate |
Non-Patent Citations (2)
| Title |
|---|
| 乳酸钠的生产与应用探讨;郭廷等;《第十一届中国国际食品添加剂和配料展览会学术论文集》;20070301;第322-323页 * |
| 郭廷等.乳酸钠的生产与应用探讨.《第十一届中国国际食品添加剂和配料展览会学术论文集》.2007,第322-323页. |
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