CN110396044A - A kind of extracting method of succinic acid - Google Patents
A kind of extracting method of succinic acid Download PDFInfo
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- CN110396044A CN110396044A CN201910746231.XA CN201910746231A CN110396044A CN 110396044 A CN110396044 A CN 110396044A CN 201910746231 A CN201910746231 A CN 201910746231A CN 110396044 A CN110396044 A CN 110396044A
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Abstract
The invention discloses a kind of extracting methods of succinic acid.Succinic acid fermentation liquor is made by Actinobacillus succinogenes anaerobic fermentation in the present invention, the solid particle and big molecular impurity in succinic acid fermentation liquor are removed by pretreatment again, it adsorbed again by one-part form adsorption column, afford succinic acid eluent, remove depigmentation, protein, carbohydrate, small molecule acid caused by inorganic ion and anaerobic fermentation, and then passes through vacuum concentration, decrease temperature crystalline, filter, be dried to obtain succinic acid, the purity is high of obtained succinic acid product is extracted, extract yield is high.
Description
Technical field
The present invention relates to chemical technology field, in particular to a kind of extracting method of succinic acid.
Background technique
Succinic acid popular name succinic acid, molecular formula C4H6O4, relative molecular mass 118.09, structural formula HOOC-CH2-CH2-
COOH, succinic acid are a kind of common natural organic acids, are widely present in the tissue of various plants and humans and animals, for example,
In the blood and muscle of immature grape, beet and people.Succinic acid is a kind of important Organic Chemicals and intermediate, main
It is used in medical industry in Erythromycin Ethylsuccinate and agricultural production plant growth regulator, fungicide and dye industry is middle-and-high-ranking has
The red production of machine pigment phthalocyanine；In terms of food industry, succinic acid can be used as the flavor of soy sauce, liquid flavoring and refined product
Modifying agent.
Currently, the succinic acid production method with prospects for commercial application mainly has electrolytic synthesis, catalytic hydrogenation method and life
Object fermentation method, wherein the problems such as that there are power consumptions is high for electrolytic synthesis, electrode corrosion；And catalytic hydrogenation method is current industrial application
Widest succinic acid synthetic method, has high income, good selective, but its reaction condition is complicated, and by-product is dirty
Contaminate environment；It is harsh for needing high-temperature high-voltage reaction condition and for the following environmentally protective expanding economy demand in China,
The chemical synthesis process that by-product easily pollutes environment simultaneously will be eliminated in the epoch eventually；And it is mild condition, environmentally friendly, dirty
Contaminating small biofermentation method at last becomes following mainstream.
Summary of the invention
The purpose of the present invention is intended to provide a kind of extracting method of succinic acid, to solve the above technical problems.
To achieve the goals above, the technical solution of the present invention is as follows:
A kind of extracting method of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, 12~16h of stationary culture at 30~40 DEG C,
Wherein, the constituent of the seed culture medium, based on mass concentration, comprising: 20~40g/L of glucose, 5~30g/ of corn pulp
L, 3~10g/L of peptone, 5~10g/L of potassium dihydrogen phosphate, 7~15g/L of sodium dihydrogen phosphate, 5~15g/L of yeast extract, go
Ionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: 20~40g/ of glucose
L, 5~30g/L of corn pulp, 5~15g/L of yeast extract, 1~5g/L of sodium bicarbonate, 0.5~2g/L of magnesium chloride, calcium chloride 0.1
~1g/L, 20~40g/L of basic magnesium carbonate, deionized water；
(3) succinic acid fermentation liquor obtained is pre-processed, removes the solid particle in succinic acid fermentation liquor and big point
Sub- impurity, obtains pretreatment fluid；
(4) resulting pretreatment fluid is passed through in one-part form adsorption column, eluant, eluent progress is passed through into one-part form adsorption column
Elution, obtains succinic acid eluent；
(5) by after the concentration of resulting succinic acid eluent, crystallization, filtering, drying, succinic acid is obtained.
Preferably, in the step (2), the inoculum concentration of the Actinobacillus succinogenes is 5~15%.
Preferably, in the step (2), the condition of the Anaerobic culturel are as follows: cultivation temperature is 35~40 DEG C, incubation time
For 60~72h, stirring rate is 100~400r/min, and carbon dioxide ventilatory capacity is 0.1~0.5L/min.
Preferably, the step (3) specifically includes: being filtered, is obtained to resulting succinic acid fermentation liquor using ultrafiltration membrane
To pretreatment fluid.
Further, the aperture of the ultrafiltration membrane is 10~50nm.
In the step (4), the one-part form adsorption column has been sequentially filled under upper: active carbon, alkali anion tree
Rouge, wherein the active carbon is 0.5~2:1, the activity in the ratio of the height of adsorption column and the height of basic anionic resin
Microfiltration membranes are provided between charcoal and basic anionic resin.
Further, the aperture of the microfiltration membranes is 0.1~0.5 μm.
Preferably, the flow velocity that is passed through of the pretreatment fluid is 1~5m3/h。
Further, the flow velocity that is passed through of the pretreatment fluid is 2~4m3/h。
Preferably, the elution flow rate of the eluant, eluent is 1~5m3/h。
Further, the elution flow rate of the eluant, eluent is 1~2m3/h。
Preferably, the eluant, eluent is inorganic acid solution.
Further, the inorganic acid solution is selected from one of hydrochloric acid solution, nitric acid solution, sulfuric acid solution or a variety of.
Preferably, the concentration of the inorganic acid solution is 1~3mol/L.
Preferably, in the step (5), the concentration, crystallization the step of specifically include:
Succinic acid eluent is concentrated by evaporation at 70~90 DEG C to the 30~40% of original volume, in 10~100r/min
Stirring rate under, be cooled to 5~10 DEG C with 5~20min/ DEG C of rate of temperature fall and crystallized, heat preservation stop 0.5~1h.
Compared with prior art, the beneficial effects of the present invention are:
Succinic acid fermentation liquor is made by Actinobacillus succinogenes anaerobic fermentation in the present invention, then removes fourth two by pretreatment
Solid particle and big molecular impurity in acid fermentation liquid, then pass through the absorption of one-part form adsorption column, afford succinic acid eluent,
Remove depigmentation, protein, carbohydrate, small molecule acid caused by inorganic ion and anaerobic fermentation, so by vacuum concentration,
Decrease temperature crystalline filters, is dried to obtain succinic acid, the purity is high of the succinic acid product extracted, and extract yield is high.
Detailed description of the invention
Fig. 1 is the extraction process line map of succinic acid provided by the invention.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing.It should be noted that for
The explanation of these embodiments is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, disclosed below
The each embodiment of the present invention involved in technical characteristic can be combined with each other as long as they do not conflict with each other.
The extraction process route for the succinic acid that following embodiment provides is as shown in Figure 1.
Embodiment 1
The extracting method for present embodiments providing a kind of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, the stationary culture 14h at 37 DEG C, wherein described
The constituent of seed culture medium, based on mass concentration, comprising: glucose 35g/L, corn pulp 20g/L, peptone 7g/L, phosphorus
Acid dihydride potassium 8g/L, sodium dihydrogen phosphate 12g/L, yeast extract 12g/L, deionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: glucose 30g/L, jade
Rice & peanut milk 25g/L, yeast extract 10g/L, sodium bicarbonate 3g/L, magnesium chloride 1g/L, calcium chloride 0.5g/L, basic magnesium carbonate 30g/
L, deionized water, the inoculum concentration of Actinobacillus succinogenes are 8%, the condition of the Anaerobic culturel are as follows: cultivation temperature is 37 DEG C, training
Supporting the time is 66h, and stirring rate 200r/min, carbon dioxide ventilatory capacity is 0.3L/min；
(3) it uses aperture to be filtered for the ultrafiltration membrane of 30nm to resulting succinic acid fermentation liquor, removes succinic acid fermentation
Solid particle and big molecular impurity in liquid, obtain pretreatment fluid；
(4) prepare one-part form adsorption column to be sequentially filled under upper: active carbon, basic anionic resin, wherein described
Active carbon is 1:1, the active carbon and alkali anion tree in the ratio of the height of adsorption column and the height of basic anionic resin
The microfiltration membranes that aperture is 0.3 μm are provided between rouge；By resulting pretreatment fluid with 3m3The flow velocity of/h is passed through one-part form adsorption column
In, and the intake for controlling pretreatment fluid is the 70% of the saturated extent of adsorption of basic anionic resin, into one-part form adsorption column
With 1.5m3The flow velocity of/h is passed through the nitric acid solution that concentration is 2mol/L and is eluted, and obtains succinic acid eluent；
(5) succinic acid eluent is concentrated by evaporation at 80 DEG C to the 35% of original volume, in the stirring rate of 50r/min
Under, 10 DEG C are cooled to 10min/ DEG C of rate of temperature fall and is crystallized, and after heat preservation stop 1h is filtered, dried, obtain succinic acid
(purity is not less than 99.5%).
Embodiment 2
The extracting method for present embodiments providing a kind of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, the stationary culture 16h at 37 DEG C, wherein described
The constituent of seed culture medium, based on mass concentration, comprising: glucose 30g/L, corn pulp 20g/L, peptone 7g/L, phosphorus
Acid dihydride potassium 6g/L, sodium dihydrogen phosphate 10g/L, yeast extract 10g/L, deionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: glucose 35g/L, jade
Rice & peanut milk 20g/L, yeast extract 12g/L, sodium bicarbonate 3.5g/L, magnesium chloride 1g/L, calcium chloride 0.6g/L, basic magnesium carbonate
25g/L, deionized water, the inoculum concentration of Actinobacillus succinogenes are 10%, the condition of the Anaerobic culturel are as follows: cultivation temperature 37
DEG C, incubation time 60h, stirring rate 200r/min, carbon dioxide ventilatory capacity are 0.25L/min；
(3) it uses aperture to be filtered for the ultrafiltration membrane of 30nm to resulting succinic acid fermentation liquor, removes succinic acid fermentation
Solid particle and big molecular impurity in liquid, obtain pretreatment fluid；
(4) prepare one-part form adsorption column to be sequentially filled under upper: active carbon, basic anionic resin, wherein described
Active carbon is 1:1, the active carbon and alkali anion tree in the ratio of the height of adsorption column and the height of basic anionic resin
The microfiltration membranes that aperture is 0.3 μm are provided between rouge；By resulting pretreatment fluid with 3m3The flow velocity of/h is passed through one-part form adsorption column
In, and the intake for controlling pretreatment fluid is the 70% of the saturated extent of adsorption of basic anionic resin, into one-part form adsorption column
With 1.5m3The flow velocity of/h is passed through the nitric acid solution that concentration is 2mol/L and is eluted, and obtains succinic acid eluent；
(5) succinic acid eluent is concentrated by evaporation at 80 DEG C to the 30% of original volume, in the stirring rate of 70r/min
Under, 10 DEG C are cooled to 8min/ DEG C of rate of temperature fall and is crystallized, and after heat preservation stop 1h is filtered, dried, obtain succinic acid
(purity is not less than 99.5%).
Embodiment 3
The extracting method for present embodiments providing a kind of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, the stationary culture 12h at 37 DEG C, wherein described
The constituent of seed culture medium, based on mass concentration, comprising: glucose 32g/L, corn pulp 25g/L, peptone 6g/L, phosphorus
Acid dihydride potassium 8g/L, sodium dihydrogen phosphate 10g/L, yeast extract 10g/L, deionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: glucose 30g/L, jade
Rice & peanut milk 15g/L, yeast extract 10g/L, sodium bicarbonate 2g/L, magnesium chloride 1g/L, calcium chloride 0.3g/L, basic magnesium carbonate 25g/
L, deionized water, the inoculum concentration of Actinobacillus succinogenes are 5%, the condition of the Anaerobic culturel are as follows: cultivation temperature is 37 DEG C, training
Supporting the time is 65h, and stirring rate 300r/min, carbon dioxide ventilatory capacity is 0.2L/min；
(3) it uses aperture to be filtered for the ultrafiltration membrane of 30nm to resulting succinic acid fermentation liquor, removes succinic acid fermentation
Solid particle and big molecular impurity in liquid, obtain pretreatment fluid；
(4) prepare one-part form adsorption column to be sequentially filled under upper: active carbon, basic anionic resin, wherein described
Active carbon is 1.5:1, the active carbon and alkali anion in the ratio of the height of adsorption column and the height of basic anionic resin
The microfiltration membranes that aperture is 0.3 μm are provided between resin；By resulting pretreatment fluid with 3m3The flow velocity of/h is passed through one-part form absorption
In column, and the intake for controlling pretreatment fluid is the 70% of the saturated extent of adsorption of basic anionic resin, to one-part form adsorption column
In with 2m3The flow velocity of/h is passed through the nitric acid solution that concentration is 2mol/L and is eluted, and obtains succinic acid eluent；
(5) succinic acid eluent is concentrated by evaporation at 85 DEG C to the 35% of original volume, in the stirring rate of 80r/min
Under, 7 DEG C are cooled to 10min/ DEG C of rate of temperature fall and is crystallized, and after heat preservation stop 1h is filtered, dried, obtain succinic acid
(purity is not less than 99.5%).
Embodiment 4
The extracting method for present embodiments providing a kind of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, the stationary culture 14h at 37 DEG C, wherein described
The constituent of seed culture medium, based on mass concentration, comprising: glucose 35g/L, corn pulp 20g/L, peptone 7g/L, phosphorus
Acid dihydride potassium 8g/L, sodium dihydrogen phosphate 12g/L, yeast extract 12g/L, deionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: glucose 30g/L, jade
Rice & peanut milk 25g/L, yeast extract 10g/L, sodium bicarbonate 3g/L, magnesium chloride 1g/L, calcium chloride 0.5g/L, basic magnesium carbonate 30g/
L, deionized water, the inoculum concentration of Actinobacillus succinogenes are 8%, the condition of the Anaerobic culturel are as follows: cultivation temperature is 40 DEG C, training
Supporting the time is 60h, and stirring rate 400r/min, carbon dioxide ventilatory capacity is 0.5L/min；
(3) it uses aperture to be filtered for the ultrafiltration membrane of 40nm to resulting succinic acid fermentation liquor, removes succinic acid fermentation
Solid particle and big molecular impurity in liquid, obtain pretreatment fluid；
(4) prepare one-part form adsorption column to be sequentially filled under upper: active carbon, basic anionic resin, wherein described
Active carbon is 2:1, the active carbon and alkali anion tree in the ratio of the height of adsorption column and the height of basic anionic resin
The microfiltration membranes that aperture is 0.5 μm are provided between rouge；By resulting pretreatment fluid with 3m3The flow velocity of/h is passed through one-part form adsorption column
In, and the intake for controlling pretreatment fluid is the 70% of the saturated extent of adsorption of basic anionic resin, into one-part form adsorption column
With 2m3The flow velocity of/h is passed through the nitric acid solution that concentration is 2mol/L and is eluted, and obtains succinic acid eluent；
(5) succinic acid eluent is concentrated by evaporation at 90 DEG C to the 40% of original volume, in the stirring speed of 100r/min
Under rate, 10 DEG C are cooled to 20min/ DEG C of rate of temperature fall and is crystallized, after heat preservation stop 1h is filtered, dried, obtain fourth two
Acid (purity is not less than 94.1%).
Embodiment 5
The extracting method for present embodiments providing a kind of succinic acid, includes the following steps:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, the stationary culture 14h at 37 DEG C, wherein described
The constituent of seed culture medium, based on mass concentration, comprising: glucose 35g/L, corn pulp 20g/L, peptone 7g/L, phosphorus
Acid dihydride potassium 8g/L, sodium dihydrogen phosphate 12g/L, yeast extract 12g/L, deionized water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, is obtained through Anaerobic culturel
To succinic acid fermentation liquor, wherein the constituent of the fermentation medium, based on mass concentration, comprising: glucose 30g/L, jade
Rice & peanut milk 25g/L, yeast extract 10g/L, sodium bicarbonate 3g/L, magnesium chloride 1g/L, calcium chloride 0.5g/L, basic magnesium carbonate 30g/
L, deionized water, the inoculum concentration of Actinobacillus succinogenes are 8%, the condition of the Anaerobic culturel are as follows: cultivation temperature is 35 DEG C, training
Supporting the time is 60h, and stirring rate 100r/min, carbon dioxide ventilatory capacity is 0.1L/min；
(3) it uses aperture to be filtered for the ultrafiltration membrane of 10nm to resulting succinic acid fermentation liquor, removes succinic acid fermentation
Solid particle and big molecular impurity in liquid, obtain pretreatment fluid；
(4) prepare one-part form adsorption column to be sequentially filled under upper: active carbon, basic anionic resin, wherein described
Active carbon is 0.5:1, the active carbon and alkali anion in the ratio of the height of adsorption column and the height of basic anionic resin
The microfiltration membranes that aperture is 0.1 μm are provided between resin；By resulting pretreatment fluid with 2m3The flow velocity of/h is passed through one-part form absorption
In column, and the intake for controlling pretreatment fluid is the 70% of the saturated extent of adsorption of basic anionic resin, to one-part form adsorption column
In with 1m3The flow velocity of/h is passed through the nitric acid solution that concentration is 2mol/L and is eluted, and obtains succinic acid eluent；
(5) succinic acid eluent is concentrated by evaporation at 80 DEG C to the 30% of original volume, in the stirring rate of 10r/min
Under, 5 DEG C are cooled to 5min/ DEG C of rate of temperature fall and is crystallized, and after heat preservation stop 0.5h is filtered, dried, obtain succinic acid
(purity is not less than 92.1%).
In conjunction with attached drawing, the embodiments of the present invention are described in detail above, but the present invention is not limited to described implementations
Mode.For a person skilled in the art, in the case where not departing from the principle of the invention and spirit, to these embodiments
A variety of change, modification, replacement and modification are carried out, are still fallen in protection scope of the present invention.
Claims (10)
1. a kind of extracting method of succinic acid, which comprises the steps of:
(1) Actinobacillus succinogenes are accessed in liquid seed culture medium, 12~16h of stationary culture at 30~40 DEG C, wherein
The constituent of the seed culture medium, based on mass concentration, comprising: 20~40g/L of glucose, 5~30g/L of corn pulp, egg
White 3~10g/L of peptone, 5~10g/L of potassium dihydrogen phosphate, 7~15g/L of sodium dihydrogen phosphate, 5~15g/L of yeast extract, deionization
Water；
(2) Actinobacillus succinogenes Jing Guo seed culture medium culture are moved into fermentation medium, obtains fourth through Anaerobic culturel
Diacid fermentation liquid, wherein the constituent of the fermentation medium, based on mass concentration, comprising: 20~40g/L of glucose, jade
5~30g/L of Rice & peanut milk, 5~15g/L of yeast extract, 1~5g/L of sodium bicarbonate, 0.5~2g/L of magnesium chloride, calcium chloride 0.1~
1g/L, 20~40g/L of basic magnesium carbonate, deionized water；
(3) succinic acid fermentation liquor obtained is pre-processed, the solid particle and macromolecular in removing succinic acid fermentation liquor are miscellaneous
Matter obtains pretreatment fluid；
(4) resulting pretreatment fluid is passed through in one-part form adsorption column, is passed through eluant, eluent into one-part form adsorption column and is eluted,
Obtain succinic acid eluent；
(5) by after the concentration of resulting succinic acid eluent, crystallization, filtering, drying, succinic acid is obtained.
2. the extracting method of succinic acid according to claim 1, which is characterized in that in the step (2), the succinic acid
The inoculum concentration of Actinobacillus is 5~15%.
3. the extracting method of succinic acid according to claim 1, which is characterized in that in the step (2), the anaerobism training
Feeding condition are as follows: cultivation temperature is 35~40 DEG C, and incubation time is 60~72h, and stirring rate is 100~400r/min, dioxy
Change carbon ventilatory capacity is 0.1~0.5L/min.
4. the extracting method of succinic acid according to claim 1, which is characterized in that the step (3) specifically includes: using
Ultrafiltration membrane is filtered resulting succinic acid fermentation liquor, obtains pretreatment fluid.
5. the extracting method of succinic acid according to claim 1, which is characterized in that in the step (4), the one-part form
Adsorption column has been sequentially filled under upper: active carbon, basic anionic resin, wherein height of the active carbon in adsorption column
Ratio with the height of basic anionic resin is 0.5~2:1, is provided with micro-filtration between the active carbon and basic anionic resin
Film.
6. the extracting method of succinic acid according to claim 1, which is characterized in that the flow velocity that is passed through of the pretreatment fluid is
1~5m3/h。
7. the extracting method of succinic acid according to claim 1, which is characterized in that the elution flow rate of the eluant, eluent is 1
~5m3/h。
8. the extracting method of succinic acid according to claim 1, which is characterized in that the eluant, eluent is inorganic acid solution.
9. the extracting method of succinic acid according to claim 1, which is characterized in that the concentration of the inorganic acid solution is 1
~3mol/L.
10. the extracting method of succinic acid according to claim 1, which is characterized in that in the step (5), the concentration,
The step of crystallization, specifically includes:
Succinic acid eluent is concentrated by evaporation at 70~90 DEG C to the 30~40% of original volume, in stirring for 10~100r/min
It mixes under rate, is cooled to 5~10 DEG C with 5~20min/ DEG C of rate of temperature fall and is crystallized, heat preservation stops 0.5~1h.
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| CN113262769A (en) * | 2021-05-28 | 2021-08-17 | 江南大学 | Polyhydroxy amphoteric resin and application thereof in adsorption separation of succinic acid |
| CN114773152A (en) * | 2022-03-30 | 2022-07-22 | 山东元利科技有限公司 | Preparation method of bio-based butanediol |
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| 孙超: "发酵丁二酸的提取工艺研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113262769A (en) * | 2021-05-28 | 2021-08-17 | 江南大学 | Polyhydroxy amphoteric resin and application thereof in adsorption separation of succinic acid |
| CN114773152A (en) * | 2022-03-30 | 2022-07-22 | 山东元利科技有限公司 | Preparation method of bio-based butanediol |
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