CN104910006A - Method for extracting lactic acid in Nisin fermentation waste liquid by using weakly basic anion exchange resin - Google Patents

Method for extracting lactic acid in Nisin fermentation waste liquid by using weakly basic anion exchange resin Download PDF

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Publication number
CN104910006A
CN104910006A CN201510191256.XA CN201510191256A CN104910006A CN 104910006 A CN104910006 A CN 104910006A CN 201510191256 A CN201510191256 A CN 201510191256A CN 104910006 A CN104910006 A CN 104910006A
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Prior art keywords
lactic acid
exchange resin
weak base
nisin
base anion
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CN201510191256.XA
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刘英梅
苏移山
李珍爱
朱云峰
张林军
宗工理
马双双
赵文刚
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SHANDONG FREDA BIOTECHNOLOGY CO Ltd
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SHANDONG FREDA BIOTECHNOLOGY CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/47Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention provides a method for extracting lactic acid in a Nisin fermentation waste liquid by using weakly basic anion exchange resin, and belongs to the field of biochemical engineering. The method comprises the following steps: decoloring the Nisin fermentation waste liquid, deproteinizing, processing weakly basic anion exchange resin, carrying out content determination, adsorbing lactic acid by using the weakly basic anion exchange resin, desorbing, recovering, and concentrating. The method has the advantages of few operating steps, small impurity content, simplicity, feasibility, repeated use of the resin, low cost, and high efficiency, and the lactic acid extraction rate is about 70%; and the method allows lactic acid to be produced and the COD value of wastewater to be reduced, so the method reduces damages of environmental pollution to mankind.

Description

The lactic acid in Nisin fermented waste fluid is extracted with weak base anion-exchange resin
Technical field
The present invention relates to a kind of method that weak base anion-exchange resin extracts the lactic acid in Nisin fermented waste fluid, belong to biological chemical field.
Background technology
Lactic acid, as one of three large organic acids, is widely used in the industrial circles such as food, chemical industry, medicine, makeup.Produce containing a large amount of lactic acid in the waste liquid of saltouing of nisin, not only difficult, and contaminate environment.By the lactic acid extraction in nisin waste liquid out, not only can protection of the environment, reduce difficulty and the expense of company's sewage disposal, and can turn waste into wealth, the lactic acid extracted is used for industrial production, increases economic efficiency.From fermented liquid, extract lactic acid mainly contain ion exchange adsorption, electroosmose process and organic solvent extractionprocess.Wherein electroosmose process needs corresponding electric osmose analyzer, and cost and technical difficulty are all higher.Organic solvent extractionprocess easily produces the residual of organic solvent, works the mischief to human body.General ion exchange resin just removes the impurity in lactic acid fermentation liquid, and this method directly can adsorb lactic acid on ion exchange column, can obtain lactic acid after wash-out.Operation steps is few, and foreign matter content is few, simple, reusable, and cost is lower.
Summary of the invention
Seeing for overcoming prior art Problems existing, the invention discloses a kind of method that weak base anion-exchange resin extracts the lactic acid in Nisin fermented waste fluid.
Technical scheme of the present invention is:
Extract the lactic acid in Nisin fermented waste fluid with weak base anion-exchange resin, it is characterized in that, comprise the following steps:
The decolouring of Nisin fermented waste fluid, deproteinated, the process of weak base anion-exchange resin, assay, weak base anion-exchange resin absorption lactic acid, resolves, reclaims, concentrated.
Further, described weak base anion-exchange resin is weak base anion-exchange resin 315.
Further, described Nisin fermented waste fluid decolouring, Deproteinated step are:
Use the gac of 1 ~ 1.5%, the MgSO4 of 0.4% joins Nisin and saltouts in waste liquid, then waste liquid of being saltoutd by this Nisin is positioned in 80 DEG C of water-baths, and 200r/min stirs 1h, vacuum filtration, removing gac.
Further, the process of described weak base anion-exchange resin is:
A. alcohol immersion 24h, NaOH is b.4% washed to neutrality after soaking 1h, and Hcl c.5% soaks 1h after washing to neutral, and d. with after the NaOH immersion 1h of 4%, is washed to neutrality again;
Further, described assay is:
The lactic acid concn of Nisin fermented waste fluid after the decolouring of National Standard Method mensuration, deproteinated, waste liquid when lactic acid concn is 90-100g/L is sample liquid.
Further, comprise the following steps:
1. Nisin fermented waste fluid decolouring, deproteinated:
With the gac of 1 ~ 1.5%, the MgSO of 0.4% 4join in Nisin fermented waste fluid, then be positioned in 80 DEG C of water-baths, 200r/min stirs 1h, vacuum filtration, removing gac;
2. the process of weak base anion-exchange resin: a. alcohol immersion 24h, NaOH is b.4% washed to neutrality after soaking 1h, and Hcl c.5% soaks 1h after washing to neutral, and d. with after the NaOH immersion 1h of 4%, is washed to neutrality again;
3. assay: National Standard Method measure decolouring, after deproteinated waste liquid lactic acid concn after, waste liquid when lactic acid concn is 90-100g/L is sample liquid, by step 2. in handle well resin dress post, above-mentioned sample liquid and resin weight in wet base are with the ratio loading of 100ml/100g;
4. weak base anion-exchange resin 315 adsorbs lactic acid:
Adsorption time: 3 ~ 20h,
5. resolve, reclaim: first get pillar express developed with 2 times of cylinder ponding, with remove not with the raffinate of resin-bonded, then to analyse with the speed hydrolysis of 2 ~ 2.5BV/h, recovery lactic acid.This technological operation is simple, and cost is low.
6. concentrate: the method that lactic acid desorbed solution concentrates is: 60 ~ 75 DEG C vacuumize concentrated.
Further, step 4. described in adsorption time be 12-20h.
The invention has the beneficial effects as follows:
The present invention uses weak base anion-exchange resin to extract the lactic acid of saltouing in filtered liquid in nisin production process, first the process of decolouring and Deproteinization is passed through, then lactic acid is adsorbed with weak base anion-exchange resin 315, and with deionized water wash-out, (general ion exchange resin just removes the impurity in lactic acid fermentation liquid, and this method directly can adsorb lactic acid on ion exchange column, after wash-out, lactic acid can be obtained.Operation steps is few, and foreign matter content is few, simple, reusable, and cost is lower).Method is simple, and step is few, and operation is simple, efficient, cost is low, and lactic acid extraction rate is about 70%; Not only can produce lactic acid (extracting the lactic acid in nisin fermented waste fluid), turn waste into wealth, and reduce the COD value of waste water, reduce environmental pollution, reduce environmental pollution to the injury of the mankind.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples, embodiment should not regard as limiting the scope of the present invention.
Embodiment 1
(1) get Nisin fermented waste fluid 10L, add 100g gac, 40g MgSO 4, agitator is adjusted to 200r/min, 80 DEG C of heating in water bath 1h, decolouring, deproteinated.
(2) National Standard Method measures the lactic acid concn (lactic acid concn is about 100g/L) of the rear waste liquid of decolouring, is sample liquid.
(3) by after the resin dress post handled well, according to the ratio loading of sample liquid (lactic acid concn is about 100g/L) and resin weight in wet base 100ml/100g.
(4) adsorb about 4h, first get pillar express developed with 2 cylinder ponding, with remove not with the raffinate of resin-bonded.Analyse with the speed hydrolysis of 2.5BV/h, lactic acid can by high efficiente callback again.
(5) 65 DEG C vacuumize concentrated, obtain finished product lactic acid.
(6) COD of difference wastewater measurement stoste and processed waste water.Result: stoste waste water COD is 19000mg/L, processed waste water COD be 10000mg/L, COD clearance is 49%.
Embodiment 2
(1) get Nisin fermented waste fluid 20L, add 200g gac, 80g MgSO 4, agitator is adjusted to 200r/min, 80 DEG C of heating in water bath 1h, decolouring, deproteinated.
(2) National Standard Method measures the lactic acid concn (lactic acid concn is about 100g/L) of the rear waste liquid of decolouring, is sample liquid.
(3) by after the resin dress post handled well, according to the ratio loading of sample liquid (lactic acid concn is about 100g/L) and resin weight in wet base 100ml/100g.
(4) adsorb about 5h, first get pillar express developed with 2 cylinder ponding, with remove not with the raffinate of resin-bonded.Analyse with the speed hydrolysis of 2BV/h, lactic acid can by high efficiente callback again.
(5) 65 DEG C vacuumize concentrated, obtain finished product lactic acid.
(6) COD of difference wastewater measurement stoste and processed waste water.Result: stoste waste water COD is 19000mg/L, processed waste water COD be 10000mg/L, COD clearance is 49%.
Embodiment 3
(1) get Nisin fermented waste fluid 10L, add 100g gac, 40g MgSO 4, agitator is adjusted to 200r/min, 80 DEG C of heating in water bath 1h, decolouring, deproteinated.
(2) National Standard Method measures the lactic acid concn (lactic acid concn is about 100g/L) of the rear waste liquid of decolouring, is sample liquid.
(3) by after the resin dress post handled well, according to the ratio loading of sample liquid (lactic acid concn is about 100g/L) and resin weight in wet base 100ml/100g.
(4) adsorb about 3h, first get pillar express developed with 2 cylinder ponding, with remove not with the raffinate of resin-bonded.Analyse with the speed hydrolysis of 2.5BV/h, lactic acid can by high efficiente callback again.
(5) 65 DEG C vacuumize concentrated, obtain finished product lactic acid.
(6) COD of difference wastewater measurement stoste and processed waste water.Result: stoste waste water COD is 19000mg/L, processed waste water COD be 10000mg/L, COD clearance is 49%.
Embodiment 4
(1) get Nisin fermented waste fluid 20L, add 200g gac, 80g MgSO 4, agitator is adjusted to 200r/min, 80 DEG C of heating in water bath 1h, decolouring, deproteinated.
(2) National Standard Method measures the lactic acid concn (lactic acid concn is about 100g/L) of the rear waste liquid of decolouring, is sample liquid.
(3) by after the resin dress post handled well, according to the ratio loading of sample liquid (lactic acid concn is about 100g/L) and resin weight in wet base 100ml/100g.
(4) adsorb about 20h, first get pillar express developed with 2 cylinder ponding, with remove not with the raffinate of resin-bonded.Analyse with the speed hydrolysis of 2BV/h, lactic acid can by high efficiente callback again.
(5) 65 DEG C vacuumize concentrated, obtain finished product lactic acid.
(6) COD of difference wastewater measurement stoste and processed waste water.Result: stoste waste water COD is 19000mg/L, processed waste water COD be 10000mg/L, COD clearance is 49%.

Claims (7)

1. extract the lactic acid in Nisin fermented waste fluid with weak base anion-exchange resin, it is characterized in that, comprise the following steps:
The decolouring of Nisin fermented waste fluid, deproteinated, the process of weak base anion-exchange resin, assay, weak base anion-exchange resin absorption lactic acid, resolves, reclaims, concentrated.
2. weak base anion-exchange resin according to claim 1 extracts the lactic acid in Nisin fermented waste fluid, and it is characterized in that, described weak base anion-exchange resin is weak base anion-exchange resin 315.
3. weak base anion-exchange resin according to claim 1 extracts the lactic acid in Nisin fermented waste fluid, it is characterized in that, described Nisin fermented waste fluid decolouring, Deproteinated step are:
Use the gac of 1 ~ 1.5%, the MgSO of 0.4% 4join Nisin to saltout in waste liquid, then waste liquid of being saltoutd by this Nisin is positioned in 80 DEG C of water-baths, 200r/min stirs 1h, vacuum filtration, removing gac.
4. weak base anion-exchange resin according to claim 1 extracts the lactic acid in Nisin fermented waste fluid, it is characterized in that, the process of described weak base anion-exchange resin is: a. alcohol immersion 24h, b.4% after NaOH soaks 1h, be washed to neutrality, c.5% Hcl soaks 1h after washing to neutral, and d. with after the NaOH immersion 1h of 4%, is washed to neutrality again.
5. weak base anion-exchange resin according to claim 1 extracts the lactic acid in Nisin fermented waste fluid, and it is characterized in that, described assay is:
The lactic acid concn of Nisin fermented waste fluid after the decolouring of National Standard Method mensuration, deproteinated, waste liquid when lactic acid concn is 90-100g/L is sample liquid.
6., according to the arbitrary described lactic acid extracted with weak base anion-exchange resin in Nisin fermented waste fluid of claim 1-5, it is characterized in that, comprise the following steps:
1. Nisin fermented waste fluid decolouring, deproteinated:
With the gac of 1 ~ 1.5%, the MgSO of 0.4% 4join in Nisin fermented waste fluid, then be positioned in 80 DEG C of water-baths, 200r/min stirs 1h, vacuum filtration, removing gac;
2. the process of weak base anion-exchange resin: a. alcohol immersion 24h, NaOH is b.4% washed to neutrality after soaking 1h, and Hcl c.5% soaks 1h after washing to neutral, and d. with after the NaOH immersion 1h of 4%, is washed to neutrality again;
3. assay: National Standard Method measure decolouring, after deproteinated waste liquid lactic acid concn after, waste liquid when lactic acid concn is 90-100g/L is sample liquid, by step 2. in handle well resin dress post, above-mentioned sample liquid and resin weight in wet base are with the ratio loading of 100ml/100g;
4. weak base anion-exchange resin 315 adsorbs lactic acid:
Adsorption time: 3 ~ 20h,
5. resolve, reclaim: first get pillar express developed with 2 times of cylinder ponding, with remove not with the raffinate of resin-bonded, then to analyse with the speed hydrolysis of 2 ~ 2.5BV/h, recovery lactic acid;
6. concentrate: the method that lactic acid desorbed solution concentrates is: 60 ~ 75 DEG C vacuumize concentrated.
7. weak base anion-exchange resin according to claim 6 extracts the lactic acid in Nisin fermented waste fluid, it is characterized in that, step 4. described in adsorption time be 12-20h.
CN201510191256.XA 2015-04-21 2015-04-21 Method for extracting lactic acid in Nisin fermentation waste liquid by using weakly basic anion exchange resin Pending CN104910006A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113880710A (en) * 2021-10-22 2022-01-04 万华化学集团股份有限公司 Lactic acid purification method
CN113912488A (en) * 2021-11-17 2022-01-11 浙江新银象生物工程有限公司 Method for extracting lactic acid from nisin extraction mother liquor
CN114478231A (en) * 2020-10-27 2022-05-13 河北圣雪大成制药有限责任公司 Method for recovering lactic acid from nisin waste liquid
CN114702379A (en) * 2021-09-08 2022-07-05 欧尚元(天津)有限公司 Purification method of red lactic acid

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007040458A1 (en) * 2005-10-06 2007-04-12 Hyflux Ip Resources Pte Ltd Process for recovery and purification of lactic acid
CN101234962A (en) * 2008-03-04 2008-08-06 江苏道森生物化学有限公司 Technique for separating and purifying L-lactic acid
CN101638362A (en) * 2008-08-01 2010-02-03 曾伟民 Method for comprehensively using nisin fermentation waste solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007040458A1 (en) * 2005-10-06 2007-04-12 Hyflux Ip Resources Pte Ltd Process for recovery and purification of lactic acid
CN101234962A (en) * 2008-03-04 2008-08-06 江苏道森生物化学有限公司 Technique for separating and purifying L-lactic acid
CN101638362A (en) * 2008-08-01 2010-02-03 曾伟民 Method for comprehensively using nisin fermentation waste solution

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* Cited by examiner, † Cited by third party
Title
葛亚中等: "Nisin的发酵生产条件和纯化研究", 《中国食品添加剂》, no. 05, 15 October 2003 (2003-10-15) *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114478231A (en) * 2020-10-27 2022-05-13 河北圣雪大成制药有限责任公司 Method for recovering lactic acid from nisin waste liquid
CN114702379A (en) * 2021-09-08 2022-07-05 欧尚元(天津)有限公司 Purification method of red lactic acid
CN114702379B (en) * 2021-09-08 2022-09-20 欧尚元(天津)有限公司 Purification method of red lactic acid
CN113880710A (en) * 2021-10-22 2022-01-04 万华化学集团股份有限公司 Lactic acid purification method
CN113880710B (en) * 2021-10-22 2023-10-20 万华化学集团股份有限公司 Purification method of lactic acid
CN113912488A (en) * 2021-11-17 2022-01-11 浙江新银象生物工程有限公司 Method for extracting lactic acid from nisin extraction mother liquor

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Application publication date: 20150916