CN109485558A - A kind of method of purification of long-chain biatomic acid - Google Patents
A kind of method of purification of long-chain biatomic acid Download PDFInfo
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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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- 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
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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Abstract
The present invention relates to a kind of method of purification of long-chain biatomic acid, including I, fermentation liquid heating demulsification type will be terminated, fermentation clear liquid is obtained by filtration；II, the pH value for stirring while adjusting fermentation clear liquid to acidity, then pH is adjusted to alkalinity, a small amount of surfactant is then added, stirring a period of time, is filtered to remove solid content；III, active carbon, stirring decoloration, filtering is added；IV, the clear liquid for obtaining step III carry out heating acidification, then through cooling, filtering, dry acquisition long-chain biatomic acid product.The present invention effectively reduces the nitrogen content in bioanalysis long-chain biatomic acid product, can get the dicarboxylic acid product of high-quality by way of acid, alkali and surfactant synergistic effect.
Description
Technical field
The invention belongs to technical field of biochemical industry, more particularly to a kind of method of purification of long-chain biatomic acid, especially
The method of high purity long chain binary acid is obtained from microbial fermentation solution.
Background technique
Long-chain biatomic acid general molecular formula is CnH2n-2O4, wherein n is 10-18, is that microorganism is obtained using the fermentation such as liquid wax
Metabolite.Its fermentation liquid is complicated heterogeneous system, wherein containing unreacted carbon source, microbial cell and fragment, not
The secretion etc. of the culture medium and metabolite and microorganism that utilize especially wherein contains a large amount of protein, pigment and ash
Divide equal impurity, seriously affects the purity and application of product, and bring difficulty to the extraction and purification of the type binary acid.
The method for extracting long-chain biatomic acid at present is generally divided into solvent method and Aqueous phase.Although solvent method can solve above-mentioned
Problem, but big, equipment seriously corroded is invested since solvent method exists, remain solvent and alkane and production security in product
And the problems such as environmental pollution, the use of this method are greatly limited.Although traditional water phase method of purification overcomes solvent method
Defect, but its product purity and yield cannot reach compared with high target.
In long-chain biatomic acid refining methd disclosed in patent CN01142806.6, using long-chain biatomic acid dry powder as raw material, make
With acetone, methanol and ethanol as solvent refining long-chain biatomic acid.Binary acid in method fermentation liquid first is first through activated carbon adsorption
Afterwards, then acidizing crystal, filtering, washing and dry binary acid crystalli-zation cake obtain long-chain biatomic acid dry powder, then using organic molten
Agent is refined.Used alcohols solvent is a kind of cheap common solvent, the purification for long-chain biatomic acid crude product
With certain effect, but esterification can occurs with raw material binary acid in it, generate a small amount of ester byproducts, thus long to finished product
The quality of chain binary acid and the polymerization of product have certain influence.In addition, although the requirement of decoloration can be reached using adsorbent,
But it is still limited to the removal effect of the nitrogen-containing impurities such as protein.
Patent CN103030550A is using being repeatedly acidified, be filtered, washed long-chain biatomic acid crude product, by DCn filter cake Yu Shuizhong,
More than heated under pressure to the fusing point of DCn, cools down after keeping the temperature a period of time, long-chain biatomic acid crystal, the list of product is obtained by filtration
Sour purity is up to 98.5% or more.But for the impurity such as albumen water-soluble in fermentation liquid only with filtering and repeatedly be acidified it is diluted
Means, removal effect is limited, and system, which is heated to high temperature also, before crystallization can promote the oxidation and denaturation of pigment, albumen etc., with
The reduction of temperature can be adsorbed in crystal product, have a certain impact to the color and nitrogen content of product.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of methods of purification of long-chain biatomic acid.The present invention by acid,
The mode of alkali and surfactant synergistic effect, effectively reduces the nitrogen content in bioanalysis long-chain biatomic acid product, can get
The dicarboxylic acid product of high-quality.
The method of purification of long-chain biatomic acid of the present invention, including the following contents:
I, fermentation liquid heating demulsification type will be terminated, fermentation clear liquid is obtained by filtration；
II, the pH value for stirring while adjusting fermentation clear liquid to acidity, then pH is adjusted to alkalinity, a small amount of surface-active is then added
Agent, is filtered to remove solid content at stirring a period of time；
III, active carbon, stirring decoloration, filtering is added；
IV, the clear liquid for obtaining step III carry out heating acidification, then refine production through cooling, filtering, the dry long-chain biatomic acid that obtains
Product.
In the method for the present invention, termination fermentation liquid described in step I is microorganism generation obtained from liquid wax or alkane fermentation
Thank to product, wherein the long-chain biatomic acid general molecular formula contained is CnH2n-2O4, wherein n is 10~18, and long-chain biatomic acid is single one
Kind or hybrid long chain dicarboxylic acid.
In the method for the present invention, the heating demulsification type mode of step I uses heating demulsification type mode commonly used in the art, such as exists
It is demulsified at 70~100 DEG C, stands to room temperature, divide and remove the remaining alkane in upper layer, refilter removing thallus.Further preferably such as lower section
Fermentation liquid will be terminated and be heated to 85~100 DEG C, 1~2h is stood, then separate unreacted alkane likes:；It is cooled to 60~75 again
DEG C, it is filtered to remove the impurity such as thallus and obtains fermentation clear liquid.
In the method for the present invention, step I can be using conventional methods and the equipment such as centrifugation or filtering.
In the method for the present invention, slowly to acidity, the acid of addition can be the pH value of acid adding adjusting fermentation clear liquid simultaneously for stirring
At least one of inorganic acid of any concentration, such as hydrochloric acid, sulfuric acid, nitric acid, preferably sulfuric acid；Adjust fermentation clear liquid pH value be
3.0~5.5, preferably 4.0~5.0.
In the method for the present invention, it is adjusted to after acidity slowly plus alkali adjusts pH to alkalinity, the alkali of addition can be any concentration
At least one of inorganic base, such as sodium hydroxide, potassium hydroxide, calcium hydroxide, preferably sodium hydroxide；Adjusting pH value is 8.0
~11, preferably 8.0~9.5.After continuing 10~60min of stirring after acid adding to specified pH value, then plus alkali adjust pH, add alkali to specified
After continuing 10~60min of stirring after pH value, surfactant is added.
In the method for the present invention, surfactant described in step II is that ionic surfactant or non-ionic surface are living
Property agent, dodecyl sodium sulfate, lauryl sodium sulfate or non-ionic surfactant in preferred ion type surfactant
At least one of fatty alcohol polyoxyethylene ether in agent, more preferable isomerous tridecanol polyoxyethylene ether.The addition of surfactant
Amount carries out after continuing 1~4h of stirring after addition surfactant for 1~100g, preferably 5~20g are added in every liter of fermentation clear liquid
Filtering.
Further, after adding acid for adjusting pH value to acidity, a certain amount of urea, guanidine hydrochloride, guanidinium isothiocyanate etc. is added
At least one of, it is preferably added to guanidinium isothiocyanate.Urea, guanidine hydrochloride additional amount be added 0.5 in every liter of fermentation clear liquid~
50g, preferably 3~15g.Alkali is added to adjust pH to alkalinity again after stirring 10~60min after addition.
In the method for the present invention, filtering described in step II can be filtered point using the methods of ultrafiltration, nanofiltration or micro-filtration
From, remove solid content after obtain clear liquid.
In the method for the present invention, the amounts of activated carbon that step III is added accounts for the 0.3%~1.5% of supernatant volume, and bleaching time 20~
120min, preferably 30~60min.
In the method for the present invention, heating temperature described in step IV is 80~95 DEG C, and acidification pH value is 2.0~4.0, acidization
In be stirred.Acidification acid used can be the H of any concentration2SO4、HNO3, HCl or H3PO4At least one of Deng.
In the method for the present invention, until cooling temperature generally makes long-chain biatomic acid sufficient crystallising, generally 10~30 DEG C.It is dry
Dry temperature is 105~110 DEG C, and drying time is 4~6h.
The method of the present invention can obtain the single long-chain biatomic acid product of high-purity, it is also possible to obtain hybrid long chain dicarboxylic acid
Product.
Compared with prior art, the invention has the following advantages that
(1) the inventors discovered that, heat though long-chain biatomic acid termination fermentation liquid passes through, due to bioanalysis long-chain biatomic acid
Contain a large amount of thallus in fermentation liquid, is heated during conventional pretreatment plus the method main function of alkali is emulsification and somatic cells
It is broken, to reach recycling alkane and improve the target of yield.With broken, a large amount of albumen, nucleic acid in thallus of cell wall
Equal water-soluble biologicals molecule is discharged into fermentation liquid, it is difficult to be removed with means such as subsequent filtering, absorption, a large amount of impurity are in water phase
Middle presence is the major reason for causing product quality especially nitrogen content not up to standard.The present invention will be demulsified first, three phase separation
The pH value of fermentation clear liquid afterwards is adjusted to acidity, then plus alkali be adjusted to alkalinity, surfactant is added under alkaline condition, strengthens
To the denaturation of the biomolecule such as albumen, nucleic acid, sedimentation effect in fermentation clear liquid, to significantly improve the removal rate of nitrogen.
(2) fermentation clear liquid is adjusted to acidity by the present invention, and urea, guanidine hydrochloride, guanidinium isothiocyanate are added in acid condition
Equal reagents, then plus alkali adjusts pH to alkalinity, and surfactant is added under alkaline condition, facilitate further enhanced deformation,
Sedimentation effect further improves the removal rate of nitrogen.
(3) the method for the present invention simple process is easily achieved, while having environmental-friendly, and product yield is high, quality well equal spies
Point.
Specific embodiment
The method of the present invention and effect are described in detail below by embodiment, but protection scope of the present invention is not limited to
Following embodiments.In the present invention, wt% is mass fraction.
Total acid purity is titrated using standard solution of sodium hydroxide, using phenolphthalein as indicator.Specifically: claim 0.5g sample
(being accurate to 0.0002g) is placed in 250mL conical flask, and 30mL ethanol solution is added, and after sample all dissolution, adds 2 drop phenolphthalein
Indicator drops to blush with Standard Volumetric Solutions for Sodium Hydroxide, keeps 30s colour-fast.By X(%)=C × V × 0.115 ×
100%/m is calculated, in which: X- binary acid mass percentage, %；C- Standard Volumetric Solutions for Sodium Hydroxide actual concentrations, mol/L；
V- titrates consumed Standard Volumetric Solutions for Sodium Hydroxide volume, mL；0.115- and 1.00mL Standard Volumetric Solutions for Sodium Hydroxide [c
(NaOH)=1.000mol/L] comparable binary acid quality in grams；M- sample mass, g.
Mono-acid purity is detected using gas chromatography, reference standard method GB5413.27-2010 infant food and dairy products
Middle fatty acid determination.
Total nitrogen uses chemoluminescence method, nitrogen content in reference standard NB/SH/T 0704-2010 petroleum and oil product
Measure boat sample introduction chemoluminescence method.
Embodiment 1
Using positive 12 carbon alkane as substrate, Candida tropicalis fermenting and producing dodecanedicarboxylic acid is utilized.Ten when fermentation ends
Two carbon dicarboxylic acid concentration are 150g/L, pH 7.0.Fermentation liquid 1000ml is taken, is heated to 90 DEG C, is stood to room temperature, is divided and go to upper layer
Remaining alkane, is filtered to remove thallus, obtains fermentation clear liquid.The sulfuric acid of 6mol/L is slowly added in stirring into fermentation clear liquid simultaneously
PH to 5.0 is adjusted, continues to stir 30min, the sodium hydroxide solution of 10mol/L is then added into fermentation clear liquid under stiring,
PH to 8.0 is adjusted, continues to stir 30min, then 5g lauryl sodium sulfate is added into clear liquid, continues to stir 60min.Use film
Aperture is 10-2μm membrane filtration, remove precipitating.5g active carbon is added into filtered clear liquid, stirring decoloration 20min is used
Membrane aperture is 10-2μm membrane filtration, remove solid content.Clear liquid pH to 3.0, heating are adjusted with the sulfuric acid of 6mol/L under stiring
System carries out heating acidification to 85 DEG C.System temperature is slowly dropped to room temperature, until making long-chain biatomic acid sufficient crystallising.It filters
Long-chain biatomic acid filter cake, by filter cake 105 DEG C of dry 6h to get arrive product.Product quality is shown in Table 1.
Embodiment 2
Using tridecane hydrocarbon as substrate, Candida tropicalis fermenting and producing tridecanyldicarboxylic acid is utilized.Ten when fermentation ends
Three carbon dicarboxylic acid concentration are 145g/L, pH 7.2.Fermentation liquid 1000ml is taken, is heated to 95 DEG C, is stood to room temperature, is divided and go to upper layer
Remaining alkane, is filtered to remove thallus, obtains fermentation clear liquid.The nitric acid of 8mol/L is slowly added in stirring into fermentation clear liquid simultaneously
PH to 4.0 is adjusted, continues to stir 20min, the potassium hydroxide solution of 10mol/L is then added into fermentation clear liquid under stiring,
PH to 9.0 is adjusted, continues to stir 20min, then 15g isomerous tridecanol polyoxyethylene ether is added into clear liquid, continues to stir 3h.With
Membrane aperture is 10-2μm membrane filtration, remove precipitating.10g active carbon is added into filtered clear liquid, stirs decoloration 60min,
It is 10 with membrane aperture-2μm membrane filtration, remove solid content.Under agitation with the sulfuric acid of 6mol/L adjust clear liquid pH to
2.0, heating systems carry out heating acidification to 85 DEG C.System temperature is slowly dropped to room temperature, makes long-chain biatomic acid sufficient crystallising
Only.Filter to obtain long-chain biatomic acid filter cake, by filter cake 110 DEG C of dry 4h to get arrive product.Product quality is shown in Table 1.
Embodiment 3
Using n-tetradecane hydrocarbon as substrate, Candida tropicalis fermenting and producing tetradecane diacid is utilized.Ten when fermentation ends
Four-carbon dicarboxylic acid concentration is 135g/L, pH 7.4.Fermentation liquid 1000ml is taken, is heated to 95 DEG C, is stood to room temperature, is divided and go to upper layer
Remaining alkane, is filtered to remove thallus, obtains fermentation clear liquid.The hydrochloric acid of 4mol/L is slowly added in stirring into fermentation clear liquid simultaneously
PH to 4.5 is adjusted, continues to stir 40min, the sodium hydroxide solution of 6mol/L is then added into fermentation clear liquid under stiring, adjust
PH to 9.5 is saved, continues to stir 40min, then 20g dodecyl sodium sulfate is added into clear liquid, continues to stir 2h.It is with membrane aperture
10-2μm membrane filtration, remove precipitating.3g active carbon is added into filtered clear liquid, stirring decoloration 40min uses membrane aperture
It is 10-2μm membrane filtration, remove solid content.Clear liquid pH to 4.0, calandria are adjusted with the sulfuric acid of 6mol/L under agitation
It is to carry out heating acidification to 95 DEG C.System temperature is slowly dropped to room temperature, until making long-chain biatomic acid sufficient crystallising.Filter long
Chain binary acid filter cake, by filter cake 105 DEG C of dry 5h to get arrive product.Product quality is shown in Table 1.
Embodiment 4
Treatment process and operating condition are the same as embodiment 1.Difference is for fermentation liquid to be heated to 90 DEG C, stands 1h, then separate not
The alkane of reaction；It is cooled to 70 DEG C again, is filtered to remove the impurity such as thallus and obtains fermentation clear liquid.Product quality is shown in Table 1.
Embodiment 5
Treatment process and operating condition are the same as embodiment 1.Difference is the pH of fermentation clear liquid being adjusted to 5.5.Product quality is shown in Table
1。
Embodiment 6
Treatment process and operating condition are the same as embodiment 1.Difference is the pH of fermentation clear liquid being adjusted to 3.0.Product quality is shown in Table
1。
Embodiment 7
Treatment process and operating condition are the same as embodiment 1.Difference be to be adjusted to after acidity plus alkali to be adjusted to pH be 11.Product quality
It is shown in Table 1.
Embodiment 8
Treatment process and operating condition are the same as embodiment 1.Difference is that the surfactant being added is isomerous tridecanol polyoxyethylene
Ether.Product quality is shown in Table 1.
Embodiment 9
Treatment process and operating condition are the same as embodiment 1.Difference is that the additional amount of surfactant is 100g.Product quality is shown in Table
1。
Embodiment 10
Treatment process and operating condition are the same as embodiment 1.Difference is after adding acid for adjusting pH value to acidity, in every liter of fermentation clear liquid
15g urea is added, stirs 30min after addition.Product quality is shown in Table 1.
Embodiment 11
Treatment process and operating condition are the same as embodiment 1.Difference is after adding acid for adjusting pH value to acidity, in every liter of fermentation clear liquid
10g guanidine hydrochloride is added, stirs 30min after addition.Product quality is shown in Table 1.
Embodiment 12
Treatment process and operating condition are the same as embodiment 1.Difference is after adding acid for adjusting pH value to acidity, in every liter of fermentation clear liquid
The guanidinium isothiocyanate 7mL of 4mol/L is added, stirs 30min after addition.Product quality is shown in Table 1.
Embodiment 13
Treatment process and operating condition are the same as embodiment 1.Difference is after adding acid for adjusting pH value to acidity, in every liter of fermentation clear liquid
The guanidinium isothiocyanate 8mL of 6mol/L is added, stirs 30min after addition.Product quality is shown in Table 1.
Embodiment 14
Treatment process and operating condition are the same as embodiment 1.Difference is after adding acid for adjusting pH value to acidity, in every liter of fermentation clear liquid
The guanidinium isothiocyanate 1mL of 8mol/L is added, stirs 30min after addition.Product quality is shown in Table 1.
Embodiment 15
Treatment process and operating condition are the same as embodiment 1.Difference is after adding alkali to adjust pH value to alkalinity, in every liter of fermentation clear liquid
The guanidinium isothiocyanate 1mL of 8mol/L is added, stirs 30min after addition.Product quality is shown in Table 1.
Comparative example 1
Treatment process and operating condition are the same as embodiment 1.Difference is not to be adjusted to alkalinity after adding acid for adjusting pH value, directly plus table
Face activating agent.Product quality is shown in Table 1.
Comparative example 2
Treatment process and operating condition are the same as embodiment 1.Difference is not adjust acidity, is directly adjusted to after alkalinity plus surface-active
Agent.Product quality is shown in Table 1.
Comparative example 3
Treatment process and operating condition are the same as embodiment 1.Difference is that surfactant is not added.Product quality is shown in Table 1.
Comparative example 4
Treatment process and operating condition are the same as embodiment 1.Difference is to exchange the sequence for adjusting soda acid.Product quality is shown in Table 1.
Comparative example 5
Treatment process and operating condition are the same as embodiment 1.Difference is to be purified using CN01142806.6 the method.Product
Quality is shown in Table 1.
Comparative example 6
Treatment process and operating condition are the same as embodiment 1.Difference is to be purified using CN103030550A the method.Product
Quality is shown in Table 1.
1 long-chain biatomic acid product quality of table
Compare with comparative example through the foregoing embodiment it is found that the method for the present invention is cooperateed with by acid, alkali with the sequence of surfactant
Effect, effectively reduces nitrogen content while guaranteeing product purity, can get the dicarboxylic acid product of high-quality.Especially adding
After acid for adjusting pH value to acidity, a certain amount of urea, guanidine hydrochloride, guanidinium isothiocyanate etc. is added, product matter can be advanced optimized
Amount.Compared with prior art, nitrogen content significantly reduces.
Claims (13)
1. a kind of method of purification of long-chain biatomic acid, it is characterised in that including the following contents:
I, fermentation liquid heating demulsification type will be terminated, fermentation clear liquid is obtained by filtration；
II, the pH value for stirring while adjusting fermentation clear liquid to acidity, then pH is adjusted to alkalinity, a small amount of surface-active is then added
Agent, is filtered to remove solid content at stirring a period of time；
III, active carbon, stirring decoloration, filtering is added；
IV, the clear liquid for obtaining step III carry out heating acidification, then refine production through cooling, filtering, the dry long-chain biatomic acid that obtains
Product.
2. according to the method described in claim 1, it is characterized by: termination fermentation liquid described in step I is that microorganism utilizes liquid wax
Or metabolite obtained from alkane fermentation, wherein the long-chain biatomic acid general molecular formula contained is CnH2n-2O4, wherein n be 10~
18。
3. according to the method described in claim 1, it is characterized by: the heating demulsification type of step I is demulsified at 70~100 DEG C,
It stands to room temperature, divides and remove the remaining alkane in upper layer, refilter removing thallus.
4. according to the method described in claim 1, it is characterized by: the heating demulsification type of step I is will to terminate fermentation liquid to be heated to
85~100 DEG C, 1~2h is stood, unreacted alkane is then separated；It is cooled to 60~75 DEG C again, is filtered to remove the impurity such as thallus
Obtain fermentation clear liquid.
5. according to the method described in claim 1, it is characterized by: step II is stirred simultaneously, slowly acid adding adjusts fermentation clear liquid
PH value to acidity, the acid of addition is inorganic acid, and the pH value for adjusting fermentation clear liquid is 3.0~5.5, preferably 4.0~5.0.
6. according to the method described in claim 1, it is characterized by: step II is adjusted to after acidity slowly plus alkali adjusts pH to alkali
Property, the alkali of addition is inorganic base, and adjusting pH value is 8.0~11, preferably 8.0~9.5.
7. according to the method described in claim 1, it is characterized by: surfactant described in step II is that ionic surface is living
Property agent or nonionic surface active agent, the additional amount of surfactant is that 1~100g is added in every liter of fermentation clear liquid.
8. method according to claim 1 or claim 7, it is characterised in that: surfactant described in step II is dodecyl
At least one of sodium sulfonate, lauryl sodium sulfate or fatty alcohol polyoxyethylene ether, additional amount are to be added 5 in every liter of fermentation clear liquid
~20g.
9. according to the method described in claim 1, it is characterized by: being added a certain amount of after adding acid for adjusting pH value to acidity
At least one of urea, guanidine hydrochloride, guanidinium isothiocyanate add alkali to adjust pH to alkalinity again after stirring 10~60min after addition.
10. according to the method described in claim 9, it is characterized by: the additional amount of urea, guanidine hydrochloride, guanidinium isothiocyanate is every
It rises and 0.5~50g, preferably 3~15g is added in fermentation clear liquid.
11. according to the method described in claim 1, it is characterized by: the amounts of activated carbon that step III is added accounts for supernatant volume
0.3%~1.5%, 20~120min of bleaching time.
12. according to the method described in claim 1, it is characterized by: heating temperature described in step IV be 80~95 DEG C, be acidified pH
Value is 2.0~4.0；Acidification acid used is the H of any concentration2SO4、HNO3, HCl or H3PO4At least one of.
13. according to the method described in claim 1, it is characterized by: the cooling temperature of step IV is to keep long-chain biatomic acid abundant
Until crystallization；Drying temperature is 105~110 DEG C, and drying time is 4~6h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112299985A (en) * | 2019-07-31 | 2021-02-02 | 中国石油化工股份有限公司 | Method for refining long-chain dicarboxylic acid in fermentation liquor by using water phase |
| CN114426476A (en) * | 2020-10-10 | 2022-05-03 | 中国石油化工股份有限公司 | Refining method and device for long-chain dibasic acid |
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| CN104591999A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司 | Long chain organic acid purifying method |
| CN105712871B (en) * | 2014-12-01 | 2018-10-12 | 中国石油化工股份有限公司 | A method of purifying long-chain biatomic acid |
| CN106554273B (en) * | 2015-09-30 | 2020-02-14 | 中国石油化工股份有限公司 | Method for purifying long-chain dicarboxylic acid in fermentation liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112299985A (en) * | 2019-07-31 | 2021-02-02 | 中国石油化工股份有限公司 | Method for refining long-chain dicarboxylic acid in fermentation liquor by using water phase |
| CN112299985B (en) * | 2019-07-31 | 2023-05-30 | 中国石油化工股份有限公司 | Method for refining long-chain dicarboxylic acid in fermentation liquor by using aqueous phase |
| CN114426476A (en) * | 2020-10-10 | 2022-05-03 | 中国石油化工股份有限公司 | Refining method and device for long-chain dibasic acid |
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